CN104609409B - A kind of preparation method of Graphene millimeter sheet - Google Patents
A kind of preparation method of Graphene millimeter sheet Download PDFInfo
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- CN104609409B CN104609409B CN201510033879.4A CN201510033879A CN104609409B CN 104609409 B CN104609409 B CN 104609409B CN 201510033879 A CN201510033879 A CN 201510033879A CN 104609409 B CN104609409 B CN 104609409B
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Abstract
The present invention relates to new material technology field, specifically disclose the preparation method of a kind of Graphene millimeter sheet, comprise the following steps: first graphite oxide is added in deionized water, ultrasonic disperse forms the graphene oxide dispersion of 4wt ‰～500wt ‰, then this graphene oxide dispersion is dripped on the substrate of super hydrophobic surface；Putting into baking oven, regulation oven temperature is 45～85 DEG C, dries；Finally with hydrazine steam, graphene oxide sheet is carried out reduction and obtain Graphene millimeter sheet.The present invention utilizes the characteristic of super hydrophobic surface to synthesize Graphene millimeter sheet, and the method can be by controlling dispersion liquid concentration or droplet size, it is achieved the control of Graphene millimeter sheet size.Simultaneously as the reason that substrate is super-hydrophobic, can be very easy to and complete graphene film is taken off from substrate, it is easy to large-scale production.
Description
Technical field
The present invention relates to new material technology field, particularly relate to the preparation method of a kind of Graphene millimeter sheet.
Background technology
Graphene is more and more paid attention to due to performances such as the power of its excellence, heat, electricity, light, and the current world is each
State is all accelerating the commercialization research of Graphene.In studying business-like process, owing to it is widely used, Graphene
Macroscopic body has been increasingly becoming the focus of research, and such as graphene sponge can be conveniently used for the absorption (Advanced of leakage of oil
Functional Materials, 2012,22,4421-4425), graphene film may be used for transparency conductive electrode
(Scientific Reports, 2013,3, article number:2714 (1-7)) etc..The grapheme material of these macroscopic views is permissible
It is conveniently integrated in existing use system, such that it is able to being applied quickly.For some application such as Industry Waste
The adsorption treatment of gas, it is desirable to material to have a highest specific surface area, these scantlings can not the most greatly can not be too simultaneously
Little, too conference reduces specific surface area, the least not aspect that operates, it is also possible to can cause the waste of material and environment
Polluting, up to the present optimal size in millimeter rank, but, the most should not find about grade graphene film
Report.
It addition, in prior art, the flake graphite alkene shape flexibility of preparation is the highest, mostly by substrate shape
Looks or the restriction of template pattern, and peel off after having prepared relatively difficult from substrate, operate relatively complicated.
Summary of the invention
Technical problem: the present invention is in order to overcome the deficiency of above-mentioned technical problem, it is provided that a kind of Graphene millimeter sheet
Preparation method, Graphene prepared by the method is millimeter chip architecture, and very easy and complete and substrate desquamation.
Technical scheme: the preparation method of a kind of Graphene millimeter sheet of the present invention comprises the following steps:
First adding in deionized water by graphite oxide, ultrasonic disperse forms the graphite oxide of 4wt ‰～500wt ‰
Alkene dispersion liquid, then drips this graphene oxide dispersion on the substrate of super hydrophobic surface；Put into baking oven, regulation
Oven temperature is 45～85 DEG C, dries；Finally with hydrazine steam, graphene oxide sheet is carried out reduction and obtain stone
Ink alkene millimeter sheet.
The substrate of described super hydrophobic surface includes: Folium Nelumbinis, politef, seven fluorinated monomers, Fluorine containing olefine
And processed by low-surface energy substance glass, silicon chip, sheet metal, in plastics any one.
Described low-surface energy substance is containing fluoropropyl caged silsesquioxane or dimethicone.
Beneficial effect: the present invention utilizes the characteristic of super hydrophobic surface to synthesize Graphene millimeter sheet, and the method can be led to
Cross control dispersion liquid concentration or droplet size, it is achieved the control of Graphene millimeter sheet size.Simultaneously as substrate is super thin
The reason of water, can be very easy to and complete being taken off from substrate by graphene film, it is easy to large-scale production.At this
During individual, utilize the multiformity of super hydrophobic surface and motility can obtain the Graphene millimeter of different-shape and size
Sheet, convenient and swift, energy consumption product that is extremely low and that obtain easily is peeled off from substrate, simple to operation.
Accompanying drawing explanation
The present invention is further detailed explanation with detailed description of the invention below in conjunction with the accompanying drawings.
Fig. 1 is the digital photograph of the Graphene millimeter sheet of embodiment 1 preparation；
Fig. 2 is the scanning electron microscope (SEM) photograph of the Graphene millimeter sheet of embodiment 1 preparation.
Detailed description of the invention
Embodiment 1
The preparation method of Graphene millimeter sheet of the present invention, comprises the following steps:
The first step, first adds in deionized water by graphite oxide, and ultrasonic disperse forms the graphene oxide of 4wt ‰
Dispersion liquid, drops in lotus leaf surface by this dispersion liquid dropper, and described Folium Nelumbinis is in advance with deionized water and ethanol purge；
Second step, has the Folium Nelumbinis of graphene oxide to put into baking oven by dripping, and regulation oven temperature is 60 DEG C, dries
Dry；To be dried complete, take off from Folium Nelumbinis；
3rd step, by dried product, puts in the container filling hydrazine hydrate, and good seal, is heated to 95 DEG C
And maintain 24h, utilize hydrazine steam that it is reduced, i.e. can get Graphene millimeter sheet.Gained sample such as Fig. 1
Shown in, Fig. 2 is the scanning electron microscopic picture of gained sample, from Fig. 1 and Fig. 2 can it is clear to see that Graphene milli
There is substantial amounts of fold on rice sheet surface, and the fold on its surface can stop between graphene sheet layer and is superimposed with each other, thus
Make it have higher specific surface area, it is simple to expand the range of application of Graphene.
Embodiment 2
The first step, first adds in deionized water by graphite oxide, and ultrasonic disperse forms the graphite oxide of 100wt ‰
Alkene dispersion liquid, drops in lotus leaf surface by this dispersion liquid dropper, and described Folium Nelumbinis is clear with deionized water and ethanol in advance
Wash；
Second step, has the Folium Nelumbinis of graphene oxide to put into baking oven by dripping, and regulation oven temperature is 60 DEG C, dries
Dry；To be dried complete, take off from Folium Nelumbinis；
3rd step, by dried product, puts in the container filling hydrazine hydrate, and good seal, is heated to 95 DEG C
And maintain 24h, utilize hydrazine steam that it is reduced, i.e. can get Graphene millimeter sheet.The similar figure of gained sample
1, but the volume of sheet substantially increases.
Embodiment 3
The first step, first adds in deionized water by graphite oxide, and ultrasonic disperse forms the graphite oxide of 300wt ‰
Alkene dispersion liquid, drops in ptfe surface by this dispersion liquid dropper, described politef spend in advance from
Sub-water and ethanol purge；
Second step, has the politef of graphene oxide to put into baking oven by dripping, and regulation oven temperature is 45 DEG C,
Dry；To be dried complete, take off from politef；
3rd step, by dried product, puts in the container filling hydrazine hydrate, and good seal, is heated to 95 DEG C
And maintain 24h, utilize hydrazine steam that it is reduced, i.e. can get Graphene millimeter sheet.The similar figure of gained sample
1, but the volume of sheet substantially increases.
Embodiment 4
The first step, first adds in deionized water by graphite oxide, and ultrasonic disperse forms the graphite oxide of 500wt ‰
Alkene dispersion liquid, drops in substrate surface by this dispersion liquid dropper, and described substrate is clear with deionized water and ethanol in advance
Wash；The glass that described substrate is modified by the caged silsesquioxane containing fluoropropyl (fluoroPOSS)；
Second step, has the substrate of graphene oxide to put into baking oven by dripping, and regulation oven temperature is 85 DEG C, dries
Dry；To be dried complete, take off from substrate；
3rd step, by dried product, puts in the container filling hydrazine hydrate, and good seal, is heated to 95 DEG C also
Maintain 24h, utilize hydrazine steam that it is reduced, i.e. can get Graphene millimeter sheet.Gained sample is similar to Fig. 1,
But the volume of sheet substantially increases.
Embodiment 5
The first step, first adds in deionized water by graphite oxide, and ultrasonic disperse forms the graphite oxide of 400wt ‰
Alkene dispersion liquid, drops in substrate surface by this dispersion liquid dropper, and described substrate is clear with deionized water and ethanol in advance
Wash；Described substrate is the silicon chip that dimethicone (polydimethysiloxane) processed；
Second step, has the substrate of graphene oxide to put into baking oven by dripping, and regulation oven temperature is 50 DEG C, dries
Dry；To be dried complete, take off from substrate；
3rd step, by dried product, puts in the container filling hydrazine hydrate, and good seal, is heated to 95 DEG C also
Maintain 24h, utilize hydrazine steam that it is reduced, i.e. can get Graphene millimeter sheet.Gained sample is similar to Fig. 1,
But the volume of sheet substantially increases.
Embodiment 6
The first step, first adds in deionized water by graphite oxide, and ultrasonic disperse forms the graphite oxide of 500wt ‰
Alkene dispersion liquid, drops in substrate surface by this dispersion liquid dropper, and described substrate is clear with deionized water and ethanol in advance
Wash；Described substrate is the copper sheet metal that dimethicone (polydimethysiloxane) processed；
Second step, has the substrate of graphene oxide to put into baking oven by dripping, and regulation oven temperature is 80 DEG C, dries
Dry；To be dried complete, take off from substrate；
3rd step, by dried product, puts in the container filling hydrazine hydrate, and good seal, is heated to 95 DEG C also
Maintain 24h, utilize hydrazine steam that it is reduced, i.e. can get Graphene millimeter sheet.
Embodiment 7
The first step, first adds in deionized water by graphite oxide, and ultrasonic disperse forms the graphite oxide of 500wt ‰
Alkene dispersion liquid, drops in substrate surface by this dispersion liquid dropper, and described substrate is clear with deionized water and ethanol in advance
Wash；The plastics that described substrate is modified by the caged silsesquioxane containing fluoropropyl (fluoroPOSS)；
Second step, has the substrate of graphene oxide to put into baking oven by dripping, and regulation oven temperature is 45 DEG C, dries
Dry；To be dried complete, take off from substrate；
3rd step, by dried product, puts in the container filling hydrazine hydrate, and good seal, is heated to 95 DEG C also
Maintain 24h, utilize hydrazine steam that it is reduced, i.e. can get Graphene millimeter sheet.
Embodiment 8
The first step, first adds in deionized water by graphite oxide, and ultrasonic disperse forms the graphite oxide of 250wt ‰
Alkene dispersion liquid, drops in substrate surface by this dispersion liquid dropper, and described substrate is clear with deionized water and ethanol in advance
Wash；Described substrate is seven fluorinated monomers；
Second step, has the substrate of graphene oxide to put into baking oven by dripping, and regulation oven temperature is 75 DEG C, dries
Dry；To be dried complete, take off from substrate；
3rd step, by dried product, puts in the container filling hydrazine hydrate, and good seal, is heated to 95 DEG C also
Maintain 24h, utilize hydrazine steam that it is reduced, i.e. can get Graphene millimeter sheet.
Embodiment 9
The first step, first adds in deionized water by graphite oxide, and ultrasonic disperse forms the graphite oxide of 50wt ‰
Alkene dispersion liquid, drops on the substrate of super hydrophobic surface by this dispersion liquid dropper, and described substrate uses deionization in advance
Water and ethanol purge；Described substrate is Fluorine containing olefine；
Second step, has the substrate of graphene oxide to put into baking oven by dripping, and regulation oven temperature is 55 DEG C, dries
Dry；To be dried complete, take off from substrate；
3rd step, by dried product, puts in the container filling hydrazine hydrate, and good seal, is heated to 95 DEG C also
Maintain 24h, utilize hydrazine steam that it is reduced, i.e. can get Graphene millimeter sheet.
Embodiment 10
The first step, first adds in deionized water by graphite oxide, and ultrasonic disperse forms the graphite oxide of 500wt ‰
Alkene dispersion liquid, drops in substrate surface by this dispersion liquid dropper, and described substrate is clear with deionized water and ethanol in advance
Wash；Described substrate is the aluminum metal film that dimethicone (polydimethysiloxane) processed；
Second step, has the substrate of graphene oxide to put into baking oven by dripping, and regulation oven temperature is 80 DEG C, dries
Dry；To be dried complete, take off from substrate；
3rd step, by dried product, puts in the container filling hydrazine hydrate, and good seal, is heated to 95 DEG C also
Maintain 24h, utilize hydrazine steam that it is reduced, i.e. can get Graphene millimeter sheet.
Embodiment 11
The first step, first adds in deionized water by graphite oxide, and ultrasonic disperse forms the graphite oxide of 500wt ‰
Alkene dispersion liquid, drops in substrate surface by this dispersion liquid dropper, and described substrate is clear with deionized water and ethanol in advance
Wash；Described substrate is the ferrous metal sheet that dimethicone (polydimethysiloxane) processed；
Second step, has the substrate of graphene oxide to put into baking oven by dripping, and regulation oven temperature is 85 DEG C, dries
Dry；To be dried complete, take off from substrate；
3rd step, by dried product, puts in the container filling hydrazine hydrate, and good seal, is heated to 95 DEG C also
Maintain 24h, utilize hydrazine steam that it is reduced, i.e. can get Graphene millimeter sheet.
The above, be only presently preferred embodiments of the present invention, and the present invention not does any pro forma restriction, every
According to any simple modification in the technical spirit of the present invention, above example made, equivalent variations, each fall within this
Within bright protection domain.
Claims (2)
1. the preparation method of a Graphene millimeter sheet, it is characterised in that this preparation method comprises the following steps:
First adding in deionized water by graphite oxide, ultrasonic disperse forms the oxidation of 4wt ‰～500wt ‰
Graphene dispersing solution, then drips this graphene oxide dispersion on the substrate of super hydrophobic surface；Put into baking
Case, regulation oven temperature is 45～85 DEG C, dries；Finally with hydrazine steam, graphene oxide sheet is entered
Row reduction obtains Graphene millimeter sheet；
The substrate of described super hydrophobic surface includes: Folium Nelumbinis, politef, seven fluorinated monomers, fluorine-containing
In alkene or the glass, silicon chip, sheet metal or the plastics that processed by low-surface energy substance any one.
The preparation method of a kind of Graphene millimeter sheet the most according to claim 1, it is characterised in that
Described low-surface energy substance is containing fluoropropyl caged silsesquioxane or dimethicone.
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| CN105732038A (en) * | 2016-01-15 | 2016-07-06 | 东南大学 | Highly conductive flexible self-supported graphene film and preparation method thereof |
| CN105967172B (en) * | 2016-05-06 | 2018-06-19 | 电子科技大学 | A kind of preparation method of the foldable graphene film of large area |
| CN108946709A (en) * | 2018-07-10 | 2018-12-07 | 东南大学 | A kind of preparation method of the three-dimensional high-densit more fold graphene oxides of high-hydroscopicity |
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| KR101260433B1 (en) * | 2010-04-30 | 2013-05-06 | 연세대학교 산학협력단 | Graphene thin film by electrostatic spraying deposition and manufacturing method thereof |
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