CN103011144A - Fabrication method of graphene nanobelt with visible-light response - Google Patents
Fabrication method of graphene nanobelt with visible-light response Download PDFInfo
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- CN103011144A CN103011144A CN2012105659834A CN201210565983A CN103011144A CN 103011144 A CN103011144 A CN 103011144A CN 2012105659834 A CN2012105659834 A CN 2012105659834A CN 201210565983 A CN201210565983 A CN 201210565983A CN 103011144 A CN103011144 A CN 103011144A
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Abstract
The invention relates to a fabrication method of a graphene nanobelt with a visible-light response. The fabrication method is characterized in that the fabrication method comprises the steps that with the adoption of a vacuum reduction method, oxidized graphene is reduced to graphene at 300 DEG C; in addition, a C=C bond in a graphene framework is damaged; the ultrasonic treatment is adopted; and the graphene nanobelt that is 100-400nm in length and 20-80nm in width is obtained. The nanobelt exposes more edges, can serve as an ideal carrier, and reflects a characteristic of a semiconductor. The prepared graphene nanobelt has strong photoproduction electron ability and electron transmission ability under the exposure of simulating sunlight.
Description
Technical field
The present invention relates to a kind of preparation method with visible light-responded graphene nanobelt.
Background technology
Graphene is nova that rises up slowly in Materials science and the condensed matter physics.Graphene is because its absolute two-dirnentional structure and excellent machinery, calorifics, optics and electric property, greatly excite people to designing take Graphene as the basis, can be applicable to the interest of the type material of the technical fields such as nanoelectronics, bio-sensing, polymer composite, hydrogen gas production and storage, drug conveying and photochemical catalysis.In addition, because its excellent electroconductibility and chemical stability, Graphene is considered to transmit better than carbon nanotube the multifunctional material in electronics or hole.
As a kind of perfect two dimensional crystal, Graphene has caused the extensive concern of scientific circles because of its unique structure.The current carrier of Graphene is similar to relativistic particles, has the room temperature quantum hall effect, and carrier concentration is up to 10
13Cm
-2The carrier mobility of the Graphene of tape stripping surpasses 2.0 * 10
5Cm
2/ Vs exceeds 100 times than silicon commonly used in the semi-conductor industry.The transistorized limiting frequency of single-layer graphene is up to 427 GHz, and thermal conductivity is 10 times of copper, and the transmitance of light can reach 97.7%, and intensity is 100 times of steel.2010, Nobel Prize in physics was authorized two discoverer K. S. Novoselov and the A. K. Geim of Graphene, to commend them in the huge contribution of making aspect the Graphene discovery.But Graphene will still have some Fundamental Aspects to need to be resolved hurrily really being applied aspect electronics and the photochemistry, such as the control of Graphene pattern, particularly also has huge challenge aspect the Graphene of preparation mono-dispersed nano size.
Summary of the invention
One of purpose of the present invention is to provide a kind of preparation method with visible light-responded graphene nanobelt.
The inventive method takes the lead in adopting the realization of cryogenic vacuum activation method to the modified with reduction of graphene oxide, the vacuum activating process also can be destroyed the two keys of C=C in the Graphene skeleton simultaneously, pass through again further supersound process, just obtain the graphene nanobelt of the nano-scale of high dispersive.The gained graphene nanobelt is of a size of: about length 100nm, about width 20nm.
For achieving the above object, the present invention adopts following technical scheme:
A kind of preparation method with visible light-responded graphene nanobelt, the concrete steps that it is characterized in that the method are: with graphene oxide, be scattered in the ultrapure water, the mass percent of graphene oxide and water is 0.025:100, ultra-sonic dispersion is to the rear evaporate to dryness that is uniformly dispersed, 300 ℃ of lower vacuum reducings 3 hours, and again be scattered in the ultrapure water ultra-sonic dispersion 10min～8 hour, wherein the mass percent of graphene oxide and water is 0.003:100, through after the water washing, be scattered at last in the ultrapure water, obtain graphene nanobelt.
The size of above-mentioned graphene nanobelt is greatly: long 100～400nm, wide 20～80nm.
Above-mentioned resulting graphene nanobelt shows semi-conductive characteristic and better optical property, has the more ability of high light electric current that produces under the simulated solar rayed.
The inventive method is take micron-sized graphene oxide thin slice as raw material, when realizing the graphene oxide modified with reduction, can be with micron-sized graphene platelet, cut into homodisperse, nano level graphene nano band structure.Advantage of the present invention is embodied in:
1): with respect to traditional doping, the method for modifying such as compound, vacuum activating is in conjunction with ultrasonic method, and is simple to operate, and equipment is simple, greatly reduces production cost, is conducive to industrialization promotion.
2): the graphene nanobelt of preparation is uniformly dispersed the little and distribution homogeneous of size.Nano belt can expose more edge, thereby is conducive to compound with other material, is a kind of ideal carrier.
3): the vacuum activating method can realize the modified with reduction to graphene oxide simultaneously, reaches the destruction to Graphene skeleton C=C key, again in conjunction with supersound process, can make the graphene nanobelt of high dispersive.
4): the graphene nanobelt of preparation shows semi-conductive characteristic and better optical property, has the more ability of high light electric current that produces under the simulated solar rayed.
Description of drawings
Fig. 1 is the graphene oxide of embodiment 1 preparation and the TEM photo of graphene nanobelt.
Fig. 2 is the graphene oxide of embodiment 1 preparation and the XRD spectra of graphene nanobelt.
Fig. 3 is the graphene oxide of embodiment 1 preparation and the photoelectric current test pattern of graphene nanobelt.
Embodiment
The present invention adopts " Hummer " method to prepare graphene oxide GO, and concrete grammar is as follows: 3g graphite is scattered in the vitriol oil that 12ml contains 2.5g Potassium Persulphate and 2.5g Vanadium Pentoxide in FLAKES, and 80 ℃ are stirred 4.5h, then are cooled to room temperature and normal temperature and place 12h.Gained mixture filtration washing and seasoning 12h.Pretreated graphite adds in the 120ml vitriol oil, maintains the temperature to add while stirring 15g potassium permanganate below 20 ℃ 35 ℃ of lower 2h that stir.Mixture keeps temperature to be lower than 50 ℃ with 250ml deionized water dilution, ice-water bath.After stirring 2h, add the 0.7L deionized water, slowly add subsequently 20ml 30% hydrogen peroxide.Mixing solutions presents glassy yellow, and bubbling.Leave standstill, remove supernatant liquid, add 10% salt acid elution for several times, with deionized water wash for several times until leave standstill be not easy sedimentation till, dialysed 10～15 days.The gained sample ultrasonic disperses to obtain homodisperse graphite oxide aqueous solution.
Embodiment one: graduated cylinder measures the graphene oxide (GO, 2.1mg/ml) of 5ml, be scattered in the 40ml ultrapure water, and behind the ultra-sonic dispersion 1h, 60 ℃ of lower evaporates to dryness.GO thin slice with evaporate to dryness is transferred in the vacuum tube furnace again, 300 ℃ of lower vacuum reducing 3h.The Graphene that obtains after the reduction is scattered in the 20ml ultrapure water again, and ultra-sonic dispersion 10min, 30min, 1h, 2h, 4h, 8h wash 3 times respectively.Be scattered at last in the 5ml ultrapure water, obtain graphene nanobelt, be labeled as GR.
Photoelectric current test evaluation method provided by the invention is as follows: what we adopted is the test macro of three standard electrodes, and take the sodium sulfate of 0.5 M as electrolytic solution, (area of sample is 0.5 cm on conductive glass with the sample dispersion of preparation
-2), as working electrode; With platinum electrode electrode as a comparison; With saturated Ag/AgCl as reference electrode.Use the xenon lamp of 300W as the simulated solar light source.The test of photoelectric current (CHI Instruments Inc.) on CHI 660 D electrochemical workstations is carried out.
Fig. 1 shows, adopting the graphene oxide of " Hummers " method preparation is a micron-sized single sheet structure, and the surface has certain fold.And we adopt vacuum reducing to have obvious nano belt structure in conjunction with the Graphene of ultrasonic method preparation, and disperse comparatively even.The length of nano belt is 100nm, and width is 20nm.
Fig. 2 shows, after processing through vacuum reducing, graphene oxide has been reduced into Graphene.10.14 ° the characteristic peak of graphene oxide after processing through vacuum reducing, disappear, this explanation graphene oxide successfully is reduced into Graphene.
Fig. 3 shows, under the simulated solar rayed, graphene nanobelt has the light induced electron ability stronger than graphene oxide, and electron transport ability.
Claims (3)
1. preparation method with visible light-responded graphene nanobelt, the concrete steps that it is characterized in that the method are: with graphene oxide, be scattered in the ultrapure water, the mass percent of graphene oxide and water is 0.025:100, ultra-sonic dispersion is to the rear evaporate to dryness that is uniformly dispersed, 300 ℃ of lower vacuum reducings 3 hours, and again be scattered in the ultrapure water ultra-sonic dispersion 10min～8 hour, wherein the mass percent of graphene oxide and water is 0.003:100, through after the water washing, be scattered at last in the ultrapure water, obtain graphene nanobelt.
2. the preparation method with visible light-responded graphene nanobelt according to claim 1 is characterized in that the size of described graphene nanobelt greatly: long 100～400nm, wide 20～80nm.
3. the preparation method with visible light-responded graphene nanobelt according to claim 1, it is characterized in that resulting graphene nanobelt shows semi-conductive characteristic and better optical property, under the simulated solar rayed, have the more ability of high light electric current that produces.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103526333A (en) * | 2013-10-10 | 2014-01-22 | 湖北大学 | Photostimulation-responsive nanometer composite fiber and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102125853A (en) * | 2011-01-19 | 2011-07-20 | 南京理工大学 | Nano zinc ferrite-graphene composite photocatalyst of visible light response and preparation method thereof |
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|---|---|---|---|---|
| CN102125853A (en) * | 2011-01-19 | 2011-07-20 | 南京理工大学 | Nano zinc ferrite-graphene composite photocatalyst of visible light response and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 刑明阳: "新型高效改性纳米二氧化钛光催化剂的制备、表征及其降解污染物的研究", 《中国博士学位论文全文数据库 工程科技I程》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103526333A (en) * | 2013-10-10 | 2014-01-22 | 湖北大学 | Photostimulation-responsive nanometer composite fiber and preparation method thereof |
| CN103526333B (en) * | 2013-10-10 | 2015-10-21 | 湖北大学 | Light stimulus responsive nano composite fibre and preparation method thereof |
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Application publication date: 20130403 |