CN104591164B - A kind of preparation method of Graphene microbody - Google Patents
A kind of preparation method of Graphene microbody Download PDFInfo
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- CN104591164B CN104591164B CN201410841690.3A CN201410841690A CN104591164B CN 104591164 B CN104591164 B CN 104591164B CN 201410841690 A CN201410841690 A CN 201410841690A CN 104591164 B CN104591164 B CN 104591164B
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Abstract
The present invention relates to new material technology field, specifically disclose the preparation method of a kind of Graphene microbody, comprise the following steps: first graphite oxide is added in deionized water, ultrasonic disperse forms the graphene oxide dispersion of 0.05mg/mL～2mg/mL, is then dripped on the substrate of super hydrophobic surface by this graphene oxide dispersion dropper；Putting into baking oven, regulation oven temperature is 55～65 DEG C, dries；Finally with hydrazine steam, graphene oxide sheet is carried out reduction and obtain Graphene microbody.The present invention prepares that the method for Graphene microbody is simple to operate, energy consumption is low, utilizes the not wellability of super hydrophobic surface, allows graphene oxide from being agglomerated into graphene oxide microbody, obtains Graphene microbody after simple reduction.
Description
Technical field
The present invention relates to new material technology field, particularly relate to the preparation method of a kind of Graphene microbody.
Background technology
Graphene is with sp by carbon atom2The monoatomic layer that hydridization connects is constituted, and its basic structural unit is six
The hexatomic ring that individual carbon atom is constituted, its theoretic throat is only 0.35nm, is the thinnest two dimension found at present
Material.Graphene have excellence character (J.APPL.POLYM.SCI., 2014, DOI:
10.1002/APP.39628), it is the strongest material, and Young's modulus has reached 1TPa.It addition,
Its thermal conductivity height has reached 2300m to 5300W/Mk, specific surface area2/ g, the electronics with superelevation moves
Shifting rate 200000cm2/ Vs, all these performances make Graphene become the favorite in the world.But prepare in reality
During, due to the hydrophobic character of Graphene, always there is the reunion of blade, thus bury its height and compare table
The advantage of area, finally hinders its further application in fields such as microelectronics, composite, catalysis.
The Graphene of surface folding, the fold on its surface can stop and is superimposed with each other between oxyalkylene lamella, thus
Make it have higher specific surface area, it is simple to Graphene is extensively applied in fields such as catalysis.Therefore, how to make
Graphene oxide lamella forms more fold, becomes a focus of current research.At present, stone is being prepared
It is will to contain at 800 DEG C that ink alkene oxidation of precursor graphene sheet layer forms a kind of preferably method of more fold
There is the small aerosol rapid evaporation of the mixture of graphene oxide or graphene oxide and other material, thus
Obtain the graphene film Rotating fields (ACSNANO, 2011,5,8943-8949) of high fold.But this method
Needing the highest temperature, energy consumption is higher.In prior art, prepare Graphene microbody process the most comparatively laborious,
Universal long processing time and heating-up temperature are high, cause power consumption bigger.Improve the another of graphene oxide specific surface area
A kind of effective way is to regulate and control its self assembly behavior, stops and overlaps between graphene oxide lamella, makes the most easily
In the unordered accumulation of single-layer graphene fragment of formation stacked in layers, form spherical or more complicated polyhedron knot
Structure.For in theory, graphene oxide lamella interlock and pile up the most stable spheroid formed by tool
Standby bigger pore volume, porosity and specific surface area.
Summary of the invention
The present invention is in order to overcome the deficiency of above-mentioned technical problem, it is provided that the preparation method of a kind of Graphene microbody,
Graphene microbody specific surface area prepared by the method is big, and the method is simple to operate, with low cost, production efficiency
Higher.
The technical scheme solving above-mentioned technical problem is as follows:
The preparation method of a kind of Graphene microbody, comprises the following steps:
First adding in deionized water by graphite oxide, ultrasonic disperse forms the oxygen of 0.05mg/mL～2mg/mL
Functionalized graphene dispersion liquid, then drips the substrate in super hydrophobic surface by this graphene oxide dispersion dropper
On；Putting into baking oven, regulation oven temperature is 55～65 DEG C, dries；Finally with hydrazine steam to oxidation
Graphene film carries out reduction and obtains Graphene microbody.
Further, the substrate of described super hydrophobic surface includes: lotus leaf, polytetrafluoroethylene (PTFE), seven fluoropropene
Acid esters, Fluorine containing olefine and the glass processed by low-surface energy substance, silicon chip, sheet metal, plastics are appointed
Meaning one.
Further, described low-surface energy substance is containing fluoropropyl caged silsesquioxane or dimethyl-silicon
Oil.
Further, the water dropper internal diameter of described dropper is 0.1～4mm.
The invention have the benefit that the present invention prepares that the method for Graphene microbody is simple to operate, energy consumption is low,
Utilize the not wellability of super hydrophobic surface, allow graphene oxide from being agglomerated into graphene oxide microbody, Jing Guojian
Graphene microbody is obtained after single reduction.The present invention utilizes the super hydrophobic surfaces such as lotus leaf by simply dripping at it
Surface groups is conglobulated and is formed the method for drop and make Graphene microbody, microbody size on the one hand can by
Drop size (dropper water dropper internal diameter size) during dropping is adjusted, on the other hand can be by controlling oxygen
The concentration of functionalized graphene dispersion liquid is adjusted.This preparation method is simple and baking temperature is relatively low, significantly
Reduce power consumption.
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 low power scanning electron micrographs of the Graphene microbody of embodiment 1 preparation；
Fig. 2 is the high power scanning electron micrographs of the Graphene microbody of embodiment 1 preparation；
Detailed description of the invention
Embodiment 1
The preparation method of a kind of Graphene microbody, comprises the following steps:
The first step, first adds in deionized water by graphite oxide, and ultrasonic disperse forms 0.05mg/mL's
Graphene oxide dispersion, drops in lotus leaf surface by the dropper of this dispersion liquid water dropper internal diameter 1mm, described
Lotus leaf is in advance with deionized water and ethanol purge；
Second step, has the lotus leaf of graphene oxide to put into baking oven by dripping, and regulation oven temperature is 55 DEG C, enters
Row is dried；To be dried complete, take off from lotus leaf；
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 microbody.Fig. 1 is institute
The low power scanning electron microscope (SEM) photograph of Graphene microbody processed, Fig. 2 is the high power scanning electron microscope (SEM) photograph of made Graphene microbody,
Form it is obvious that microbody is reunited by the graphene film of a large amount of folds.
Embodiment 2
The preparation method of a kind of Graphene microbody, comprises the following steps:
The first step, first adds in deionized water by graphite oxide, and ultrasonic disperse forms the oxygen of 0.1mg/mL
Functionalized graphene dispersion liquid, drops in lotus leaf surface by the dropper of this dispersion liquid water dropper internal diameter 0.2mm, described
Lotus leaf is in advance with deionized water and ethanol purge；
Second step, has the lotus leaf of graphene oxide to put into baking oven by dripping, and regulation oven temperature is 60 DEG C, enters
Row is dried；To be dried complete, take off from lotus leaf；
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 microbody.Obtained is micro-
Body is similar to shown in Fig. 1, simply increased on volume.
Embodiment 3
The preparation method of a kind of Graphene microbody, comprises the following steps:
The first step, first adds in deionized water by graphite oxide, and ultrasonic disperse forms the oxygen of 0.1mg/mL
Functionalized graphene dispersion liquid, drops in ptfe surface by the dropper of this dispersion liquid water dropper internal diameter 1mm, institute
The polytetrafluoroethylene (PTFE) stated is in advance with deionized water and ethanol purge；
Second step, has the polytetrafluoroethylene (PTFE) of graphene oxide to put into baking oven by dripping, and regulation oven temperature is
60 DEG C, dry；To be dried complete, take off from polytetrafluoroethylene (PTFE)；
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 microbody.
Embodiment 4
The preparation method of a kind of Graphene microbody, comprises the following steps:
The first step, first adds in deionized water by graphite oxide, and ultrasonic disperse forms the oxidation of 2mg/mL
Graphene dispersing solution, drops in substrate surface, described substrate by the dropper of this dispersion liquid water dropper internal diameter 1mm
In advance with deionized water and ethanol purge；Described substrate is containing fluoropropyl caged silsesquioxane
(fluoroPOSS) glass modified；
Second step, has the substrate of graphene oxide to put into baking oven by dripping, and regulation oven temperature is 65 DEG C, enters
Row is dried；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 and maintain 24h, utilize hydrazine steam that it is reduced, i.e. can get Graphene microbody.The stone of gained
Ink alkene microbody significantly reduces on volume.
Embodiment 5
The preparation method of a kind of Graphene microbody, comprises the following steps:
The first step, first adds in deionized water by graphite oxide, and ultrasonic disperse forms the oxidation of 2mg/mL
Graphene dispersing solution, drops in substrate surface by the liquid-transfering gun of this dispersion liquid water dropper internal diameter 0.1mm, described
Substrate is in advance with deionized water and ethanol purge；Described substrate is containing fluoropropyl caged silsesquioxane
(fluoroPOSS) glass modified；
Second step, has the substrate of graphene oxide to put into baking oven by dripping, and regulation oven temperature is 65 DEG C, enters
Row is dried；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 and maintain 24h, utilize hydrazine steam that it is reduced, i.e. can get Graphene microbody.The graphite of gained
Alkene microbody significantly reduces on volume.
Embodiment 6
The preparation method of a kind of Graphene microbody, comprises the following steps:
The first step, first adds in deionized water by graphite oxide, and ultrasonic disperse forms 0.06mg/mL's
Graphene oxide dispersion, drops in substrate surface by the dropper of this dispersion liquid water dropper internal diameter 4mm, described
Substrate is in advance with deionized water and ethanol purge；Described substrate is dimethicone
(polydimethysiloxane) plastics processed；
Second step, has the substrate of graphene oxide to put into baking oven by dripping, and regulation oven temperature is 60 DEG C, enters
Row is dried；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 and maintain 24h, utilize hydrazine steam that it is reduced, i.e. can get Graphene microbody.The graphite of gained
Alkene microbody significantly increases on volume.
Embodiment 7
The preparation method of a kind of Graphene microbody, comprises the following steps:
The first step, first adds in deionized water by graphite oxide, and ultrasonic disperse forms 0.06mg/mL's
Graphene oxide dispersion, drops in substrate surface by the dropper of this dispersion liquid water dropper internal diameter 2.5mm, described
Substrate in advance with deionized water and ethanol purge；Described substrate is dimethicone
(polydimethysiloxane) silicon chip processed；
Second step, has the substrate of graphene oxide to put into baking oven by dripping, and regulation oven temperature is 60 DEG C, enters
Row is dried；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 and maintain 24h, utilize hydrazine steam that it is reduced, i.e. can get Graphene microbody.
Embodiment 8
The preparation method of a kind of Graphene microbody, comprises the following steps:
The first step, first adds in deionized water by graphite oxide, and ultrasonic disperse forms 0.15mg/mL's
Graphene oxide dispersion, drops in substrate surface by the dropper of this dispersion liquid water dropper internal diameter 3mm, described
Substrate is in advance with deionized water and ethanol purge；Described substrate is dimethicone
(polydimethysiloxane) the copper sheet metal processed；
Second step, has the substrate of graphene oxide to put into baking oven by dripping, and regulation oven temperature is 60 DEG C, enters
Row is dried；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 and maintain 24h, utilize hydrazine steam that it is reduced, i.e. can get Graphene microbody.
Embodiment 9
The preparation method of a kind of Graphene microbody, comprises the following steps:
The first step, first adds in deionized water by graphite oxide, and ultrasonic disperse forms 0.16mg/mL's
Graphene oxide dispersion, drops in substrate surface by the dropper of this dispersion liquid water dropper internal diameter 3.4mm, described
Substrate in advance with deionized 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 60 DEG C, enters
Row is dried；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 and maintain 24h, utilize hydrazine steam that it is reduced, i.e. can get Graphene microbody.
Embodiment 10
The preparation method of a kind of Graphene microbody, comprises the following steps:
The first step, first adds in deionized water by graphite oxide, and ultrasonic disperse forms 0.09mg/mL's
Graphene oxide dispersion, drops in substrate surface by the dropper of this dispersion liquid water dropper internal diameter 2.4mm, described
Substrate in advance with deionized water and ethanol purge；Described substrate is containing fluoropropyl caged silsesquioxane
(fluoroPOSS) aluminum metal film processed；
Second step, has the substrate of graphene oxide to put into baking oven by dripping, and regulation oven temperature is 63 DEG C, enters
Row is dried；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 and maintain 24h, utilize hydrazine steam that it is reduced, i.e. can get Graphene microbody.
Embodiment 11
The preparation method of a kind of Graphene microbody, comprises the following steps:
The first step, first adds in deionized water by graphite oxide, and ultrasonic disperse forms 0.08mg/mL's
Graphene oxide dispersion, drops in substrate surface by the dropper of this dispersion liquid water dropper internal diameter 1.5mm, described
Substrate in advance with deionized water and ethanol purge；Described substrate is containing fluoropropyl caged silsesquioxane
(fluoroPOSS) the ferrous metal sheet processed；
Second step, has the substrate of graphene oxide to put into baking oven by dripping, and regulation oven temperature is 60 DEG C, enters
Row is dried；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 and maintain 24h, utilize hydrazine steam that it is reduced, i.e. can get Graphene microbody.
Embodiment 12
The preparation method of a kind of Graphene microbody, comprises the following steps:
The first step, first adds in deionized water by graphite oxide, and ultrasonic disperse forms 0.15mg/mL's
Graphene oxide dispersion, drops in substrate surface by the dropper of this dispersion liquid water dropper internal diameter 2mm, described
Substrate is in advance with deionized water and ethanol purge；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 60 DEG C, enters
Row is dried；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 and maintain 24h, utilize hydrazine steam that it is reduced, i.e. can get Graphene microbody.
The above, be only presently preferred embodiments of the present invention, and the present invention not does any pro forma restriction,
Any simple modification of in every technical spirit according to the present invention, above example being made, equivalent variations,
Within each falling within protection scope of the present invention.
Claims (3)
1. the preparation method of a Graphene microbody, it is characterised in that comprise the following steps:
First adding in deionized water by graphite oxide, ultrasonic disperse forms the oxygen of 0.05mg/mL～2mg/mL
Functionalized graphene dispersion liquid, then drips the substrate in super hydrophobic surface by this graphene oxide dispersion dropper
On；Putting into baking oven, regulation oven temperature is 55～65 DEG C, dries；Finally with hydrazine steam to oxidation
Graphene film carries out reduction and obtains Graphene microbody；The substrate of described super hydrophobic surface includes: lotus leaf, poly-
Tetrafluoroethene, seven fluorinated monomers, Fluorine containing olefine and the glass processed by low-surface energy substance, silicon chip,
In sheet metal, plastics any one.
The preparation method of a kind of Graphene microbody the most according to claim 1, it is characterised in that institute
The low-surface energy substance stated is for containing fluoropropyl caged silsesquioxane or dimethicone.
The preparation method of a kind of Graphene microbody the most according to claim 1, it is characterised in that institute
The water dropper internal diameter of the dropper stated is 0.1～4mm.
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| CN105582751B (en) * | 2015-12-17 | 2018-05-22 | 常州碳星科技有限公司 | Filter core and its preparation method and application |
| CN108565435B (en) * | 2018-05-09 | 2020-10-23 | 东南大学 | Preparation method of graphene porous particles |
| 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 |
| CN113583495B (en) * | 2021-08-27 | 2022-08-09 | 西安应用光学研究所 | Low-air-out-rate antistatic optical absorption coating and preparation method thereof |
| CN113788477B (en) * | 2021-09-26 | 2023-08-04 | 深圳华算科技有限公司 | Wrinkled graphene coating and preparation method thereof |
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| US8182917B2 (en) * | 2008-03-20 | 2012-05-22 | The United States Of America, As Represented By The Secretary Of The Navy | Reduced graphene oxide film |
| CN103043654B (en) * | 2011-10-12 | 2014-12-10 | 国家纳米科学中心 | Film containing graphene and/or graphene oxide, and preparation method thereof |
| CN103508447A (en) * | 2012-06-26 | 2014-01-15 | 海洋王照明科技股份有限公司 | Preparation method of graphene |
| CN103086372B (en) * | 2013-01-24 | 2015-07-01 | 东南大学 | Method for preparing large-area graphene sponge |
| CN103101908B (en) * | 2013-01-24 | 2015-06-03 | 东南大学 | Method for preparing graphene film |
| CN103172062B (en) * | 2013-04-17 | 2015-07-01 | 东南大学 | Preparation method of graphene film for dye-sensitized solar cell counter electrodes |
| CN103449423B (en) * | 2013-08-27 | 2016-03-16 | 常州第六元素材料科技股份有限公司 | A kind of Graphene heat conducting film and preparation method thereof |
| CN103964424A (en) * | 2014-05-13 | 2014-08-06 | 桂林理工大学 | Method for preparing photoreduction graphene oxide thin film |
| CN104085143B (en) * | 2014-05-29 | 2016-05-04 | 深圳市铭晶科技有限公司 | Preparation method and the product of Graphene composite guide hotting mask |
| CN104071783B (en) * | 2014-06-30 | 2016-01-06 | 吉林大学 | A kind of preparation method of flexible paper-like redox graphene diaphragm |
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