CN104609409A - Preparation method of graphene millimeter sheet - Google Patents
Preparation method of graphene millimeter sheet Download PDFInfo
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- CN104609409A CN104609409A CN201510033879.4A CN201510033879A CN104609409A CN 104609409 A CN104609409 A CN 104609409A CN 201510033879 A CN201510033879 A CN 201510033879A CN 104609409 A CN104609409 A CN 104609409A
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Abstract
The invention relates to the technical field of a novel material, in particular to a preparation method of a graphene millimeter sheet. The preparation method comprises the following steps: firstly, adding graphite oxide into deionized water, carrying out ultrasonic dispersion to form a 0.4-50wt% graphene oxide dispersion and then dropping the graphene oxide dispersion on a substrate of a super-hydrophobic surface; putting the substrate in an oven and adjusting the temperature of the oven to 45-85 DEG C for drying; finally, reducing the graphene oxide sheet by using hydrazine steam to obtain the graphene millimeter sheet. According to the preparation method of the graphene millimeter sheet provided by the invention, the graphene millimeter sheet is synthesized by means of the characteristics of the super-hydrophobic surface. The method can be used for controlling the graphene millimeter sheet by controlling the concentration or drops of the dispersion so as to control the size of the graphene millimeter sheet. Moreover, as the substrate is super-hydrophobic, the graphene millimeter sheet can be easily and integrally taken down from the substrate for large-scaled production.
Description
Technical field
The present invention relates to new material technology field, particularly relate to a kind of preparation method of Graphene millimeter sheet.
Background technology
Graphene is subject to increasing attention due to the performance such as power, heat, electricity, light of its excellence, and the commercialization research of Graphene is all being accelerated in current countries in the world.In the business-like process of research, because it is widely used, graphene macroform becomes the focus of research gradually, such as graphene sponge can easily for absorption (AdvancedFunctional Materials, 2012,22 of leakage of oil, 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 can be integrated in existing use system easily, thus can very fast being applied.For some application as the adsorption treatment of industrial gaseous waste, require that material will have very high specific surface area, simultaneously these scantlings can not too greatly can not be too little, too conference reduces specific surface area, the too little not aspect that operates, also may cause the waste of material and the pollution of environment, and best size should in millimeter rank, but up to the present, also do not find the report about grade graphene film.
In addition, in prior art, the flake graphite alkene shape flexibility of preparation is often not high, is mostly subject to the restriction of substrate pattern or template pattern, and more difficult from overburden ratio substrate after having prepared, and operates comparatively loaded down with trivial details.
Summary of the invention
Technical problem: the present invention is in order to overcome the deficiency of above-mentioned technical problem, and provide a kind of preparation method of Graphene millimeter sheet, Graphene prepared by the method is millimeter chip architecture, and be very easy to 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 add in deionized water by graphite oxide, ultrasonic disperse forms the graphene oxide dispersion of 4wt ‰ ~ 500wt ‰, then drips on the substrate of super hydrophobic surface by this graphene oxide dispersion; Put into baking oven, regulate oven temperature to be 45 ~ 85 DEG C, dry; Finally with hydrazine steam, reduction is carried out to graphene oxide sheet and obtain Graphene millimeter sheet.
The substrate of described super hydrophobic surface comprises: lotus leaf, tetrafluoroethylene, seven fluorinated monomers, Fluorine containing olefine and with in the glass of low-surface energy substance process, silicon chip, tinsel, plastics any one.
Described low-surface energy substance is for containing fluoropropyl caged silsesquioxane or dimethyl silicone oil.
Beneficial effect: the present invention utilizes the characteristic of super hydrophobic surface to synthesize Graphene millimeter sheet, the method by controlling dispersion liquid concentration or droplet size, can realize the control of Graphene millimeter sheet size.Meanwhile, due to the cause that substrate is super-hydrophobic, can be very easy to and complete graphene film is taken off from substrate, be easy to scale operation.In this process, utilize the diversity of super hydrophobic surface and handiness can obtain the Graphene millimeter sheet of different-shape and size, convenient and swift, the extremely low and product obtained of energy consumption is easily peeled off from substrate, simple to operation.
Accompanying drawing explanation
Below in conjunction with the drawings and specific embodiments, the present invention is further detailed explanation.
Fig. 1 is the digital photograph of Graphene millimeter sheet prepared by embodiment 1;
Fig. 2 is the scanning electron microscope (SEM) photograph of Graphene millimeter sheet prepared by embodiment 1.
Embodiment
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 dispersion of 4wt ‰, and this dispersion liquid dropper is dropped in lotus leaf surface, and described lotus leaf uses deionized water and ethanol purge in advance;
Second step, having the lotus leaf of graphene oxide to put into baking oven by dripping, regulating oven temperature to be 60 DEG C, drying; To be dried complete, take off from lotus leaf;
3rd step, by dried product, puts into the container filling hydrazine hydrate, and good seal, be heated to 95 DEG C and maintain 24h, utilizing hydrazine steam to reduce to it, Graphene millimeter sheet can be obtained.Gained sample as shown in Figure 1, Fig. 2 is the scanning electron microscopic picture of gained sample, can clearly find out from Fig. 1 and Fig. 2, there is a large amount of folds on Graphene millimeter sheet surface, 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, be convenient to the range of application expanding Graphene.
Embodiment 2
The first step, first adds in deionized water by graphite oxide, and ultrasonic disperse forms the graphene oxide dispersion of 100wt ‰, and this dispersion liquid dropper is dropped in lotus leaf surface, and described lotus leaf uses deionized water and ethanol purge in advance;
Second step, having the lotus leaf of graphene oxide to put into baking oven by dripping, regulating oven temperature to be 60 DEG C, drying; To be dried complete, take off from lotus leaf;
3rd step, by dried product, puts into the container filling hydrazine hydrate, and good seal, be heated to 95 DEG C and maintain 24h, utilizing hydrazine steam to reduce to it, Graphene millimeter sheet can be obtained.The similar Fig. 1 of gained sample, but the volume of sheet obviously increases.
Embodiment 3
The first step, first adds in deionized water by graphite oxide, and ultrasonic disperse forms the graphene oxide dispersion of 300wt ‰, and this dispersion liquid dropper is dropped in ptfe surface, and described tetrafluoroethylene uses deionized water and ethanol purge in advance;
Second step, having the tetrafluoroethylene of graphene oxide to put into baking oven by dripping, regulating oven temperature to be 45 DEG C, drying; To be dried complete, take off from tetrafluoroethylene;
3rd step, by dried product, puts into the container filling hydrazine hydrate, and good seal, be heated to 95 DEG C and maintain 24h, utilizing hydrazine steam to reduce to it, Graphene millimeter sheet can be obtained.The similar Fig. 1 of gained sample, but the volume of sheet obviously increases.
Embodiment 4
The first step, first adds in deionized water by graphite oxide, and ultrasonic disperse forms the graphene oxide dispersion of 500wt ‰, and this dispersion liquid dropper is dropped in substrate surface, and described substrate uses deionized water and ethanol purge in advance; The glass of described substrate for modifying containing fluoropropyl caged silsesquioxane (fluoroPOSS);
Second step, having the substrate of graphene oxide to put into baking oven by dripping, regulating oven temperature to be 85 DEG C, drying; To be dried complete, take off from substrate;
3rd step, by dried product, puts into the container filling hydrazine hydrate, and good seal, be heated to 95 DEG C and maintain 24h, utilizing hydrazine steam to reduce to it, Graphene millimeter sheet can be obtained.The similar Fig. 1 of gained sample, but the volume of sheet obviously increases.
Embodiment 5
The first step, first adds in deionized water by graphite oxide, and ultrasonic disperse forms the graphene oxide dispersion of 400wt ‰, and this dispersion liquid dropper is dropped in substrate surface, and described substrate uses deionized water and ethanol purge in advance; Described substrate is the silicon chip that dimethyl silicone oil (polydimethysiloxane) processed;
Second step, having the substrate of graphene oxide to put into baking oven by dripping, regulating oven temperature to be 50 DEG C, drying; To be dried complete, take off from substrate;
3rd step, by dried product, puts into the container filling hydrazine hydrate, and good seal, be heated to 95 DEG C and maintain 24h, utilizing hydrazine steam to reduce to it, Graphene millimeter sheet can be obtained.The similar Fig. 1 of gained sample, but the volume of sheet obviously increases.
Embodiment 6
The first step, first adds in deionized water by graphite oxide, and ultrasonic disperse forms the graphene oxide dispersion of 500wt ‰, and this dispersion liquid dropper is dropped in substrate surface, and described substrate uses deionized water and ethanol purge in advance; Described substrate is the copper tinsel that dimethyl silicone oil (polydimethysiloxane) processed;
Second step, having the substrate of graphene oxide to put into baking oven by dripping, regulating oven temperature to be 80 DEG C, drying; To be dried complete, take off from substrate;
3rd step, by dried product, puts into the container filling hydrazine hydrate, and good seal, be heated to 95 DEG C and maintain 24h, utilizing hydrazine steam to reduce to it, Graphene millimeter sheet can be obtained.
Embodiment 7
The first step, first adds in deionized water by graphite oxide, and ultrasonic disperse forms the graphene oxide dispersion of 500wt ‰, and this dispersion liquid dropper is dropped in substrate surface, and described substrate uses deionized water and ethanol purge in advance; The plastics of described substrate for modifying containing fluoropropyl caged silsesquioxane (fluoroPOSS);
Second step, having the substrate of graphene oxide to put into baking oven by dripping, regulating oven temperature to be 45 DEG C, drying; To be dried complete, take off from substrate;
3rd step, by dried product, puts into the container filling hydrazine hydrate, and good seal, be heated to 95 DEG C and maintain 24h, utilizing hydrazine steam to reduce to it, Graphene millimeter sheet can be obtained.
Embodiment 8
The first step, first adds in deionized water by graphite oxide, and ultrasonic disperse forms the graphene oxide dispersion of 250wt ‰, and this dispersion liquid dropper is dropped in substrate surface, and described substrate uses deionized water and ethanol purge in advance; Described substrate is seven fluorinated monomers;
Second step, having the substrate of graphene oxide to put into baking oven by dripping, regulating oven temperature to be 75 DEG C, drying; To be dried complete, take off from substrate;
3rd step, by dried product, puts into the container filling hydrazine hydrate, and good seal, be heated to 95 DEG C and maintain 24h, utilizing hydrazine steam to reduce to it, Graphene millimeter sheet can be obtained.
Embodiment 9
The first step, first adds in deionized water by graphite oxide, and ultrasonic disperse forms the graphene oxide dispersion of 50wt ‰, and drop on the substrate of super hydrophobic surface by this dispersion liquid dropper, described substrate uses deionized water and ethanol purge in advance; Described substrate is Fluorine containing olefine;
Second step, having the substrate of graphene oxide to put into baking oven by dripping, regulating oven temperature to be 55 DEG C, drying; To be dried complete, take off from substrate;
3rd step, by dried product, puts into the container filling hydrazine hydrate, and good seal, be heated to 95 DEG C and maintain 24h, utilizing hydrazine steam to reduce to it, Graphene millimeter sheet can be obtained.
Embodiment 10
The first step, first adds in deionized water by graphite oxide, and ultrasonic disperse forms the graphene oxide dispersion of 500wt ‰, and this dispersion liquid dropper is dropped in substrate surface, and described substrate uses deionized water and ethanol purge in advance; Described substrate is the aluminum metal film that dimethyl silicone oil (polydimethysiloxane) processed;
Second step, having the substrate of graphene oxide to put into baking oven by dripping, regulating oven temperature to be 80 DEG C, drying; To be dried complete, take off from substrate;
3rd step, by dried product, puts into the container filling hydrazine hydrate, and good seal, be heated to 95 DEG C and maintain 24h, utilizing hydrazine steam to reduce to it, Graphene millimeter sheet can be obtained.
Embodiment 11
The first step, first adds in deionized water by graphite oxide, and ultrasonic disperse forms the graphene oxide dispersion of 500wt ‰, and this dispersion liquid dropper is dropped in substrate surface, and described substrate uses deionized water and ethanol purge in advance; Described substrate is the ferrous metal sheet that dimethyl silicone oil (polydimethysiloxane) processed;
Second step, having the substrate of graphene oxide to put into baking oven by dripping, regulating oven temperature to be 85 DEG C, drying; To be dried complete, take off from substrate;
3rd step, by dried product, puts into the container filling hydrazine hydrate, and good seal, be heated to 95 DEG C and maintain 24h, utilizing hydrazine steam to reduce to it, Graphene millimeter sheet can be obtained.
The above is only preferred embodiment of the present invention, not does any pro forma restriction to the present invention, every according in technical spirit of the present invention to any simple modification, equivalent variations that above embodiment is done, all fall within protection scope of the present invention.
Claims (3)
1. a preparation method for Graphene millimeter sheet, is characterized in that this preparation method comprises the following steps:
First add in deionized water by graphite oxide, ultrasonic disperse forms the graphene oxide dispersion of 4wt ‰ ~ 500wt ‰, then drips on the substrate of super hydrophobic surface by this graphene oxide dispersion; Put into baking oven, regulate oven temperature to be 45 ~ 85 DEG C, dry; Finally with hydrazine steam, reduction is carried out to graphene oxide sheet and obtain Graphene millimeter sheet.
2. the preparation method of a kind of Graphene millimeter sheet according to claim 1, it is characterized in that, the substrate of described super hydrophobic surface comprises: lotus leaf, tetrafluoroethylene, seven fluorinated monomers, Fluorine containing olefine or with in the glass of low-surface energy substance process, silicon chip, tinsel or plastics any one.
3. the preparation method of a kind of Graphene millimeter sheet according to claim 2, is characterized in that, described low-surface energy substance is for containing fluoropropyl caged silsesquioxane or dimethyl silicone oil.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105732038A (en) * | 2016-01-15 | 2016-07-06 | 东南大学 | Highly conductive flexible self-supported graphene film and preparation method thereof |
| CN105967172A (en) * | 2016-05-06 | 2016-09-28 | 电子科技大学 | Preparation method of foldable graphene thin 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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| KR20100121978A (en) * | 2009-05-11 | 2010-11-19 | 울산대학교 산학협력단 | Methods for fabricating the thin film graphene |
| KR20110121569A (en) * | 2010-04-30 | 2011-11-07 | 연세대학교 산학협력단 | Graphene thin film by electrostatic spraying deposition and manufacturing method thereof |
| CN103101908A (en) * | 2013-01-24 | 2013-05-15 | 东南大学 | Method for preparing graphene film |
| CN103172062A (en) * | 2013-04-17 | 2013-06-26 | 东南大学 | Preparation method of graphene film for dye-sensitized solar cell counter electrodes |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| KR20100121978A (en) * | 2009-05-11 | 2010-11-19 | 울산대학교 산학협력단 | Methods for fabricating the thin film graphene |
| KR20110121569A (en) * | 2010-04-30 | 2011-11-07 | 연세대학교 산학협력단 | Graphene thin film by electrostatic spraying deposition and manufacturing method thereof |
| CN103101908A (en) * | 2013-01-24 | 2013-05-15 | 东南大学 | Method for preparing graphene film |
| CN103172062A (en) * | 2013-04-17 | 2013-06-26 | 东南大学 | Preparation method of graphene film for dye-sensitized solar cell counter electrodes |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105732038A (en) * | 2016-01-15 | 2016-07-06 | 东南大学 | Highly conductive flexible self-supported graphene film and preparation method thereof |
| CN105967172A (en) * | 2016-05-06 | 2016-09-28 | 电子科技大学 | Preparation method of foldable graphene thin film of large area |
| 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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