CN108083267A - The preparation method of electron adulterated bilayer graphene - Google Patents
The preparation method of electron adulterated bilayer graphene Download PDFInfo
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- CN108083267A CN108083267A CN201810025805.XA CN201810025805A CN108083267A CN 108083267 A CN108083267 A CN 108083267A CN 201810025805 A CN201810025805 A CN 201810025805A CN 108083267 A CN108083267 A CN 108083267A
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- C01—INORGANIC CHEMISTRY
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- C01B2204/00—Structure or properties of graphene
- C01B2204/04—Specific amount of layers or specific thickness
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
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Abstract
The preparation method of electron adulterated bilayer graphene is related to graphene, especially a kind of that melamine molecule is deposited on bilayer graphene surface by thermal evaporation, to modulate the preparation method of the electron adulterated bilayer graphene of graphene electrical properties.The preparation method of the electron adulterated bilayer graphene of the present invention, it is characterized in that this preparation method prepares large area bilayer graphene with chemical vapour deposition technique, reusable heat evaporation technique modulates graphene electrical properties in one layer of melamine molecule of bilayer graphene surface evaporation.This technology and the difference for preparing single-layer graphene maximum are to have tuned up the amount of hydrogen argon gas mixed gas and extended preparation time, can be by adjusting the amount of melamine, rate-determining steps 3）In be covered in the thickness of bilayer graphene surface film；The doping of melamine enables the conduction type of graphene to realize the modulating action from strong p-type to weak p-type, is large-area graphenenType doping provides feasible program.
Description
Technical field
It is especially a kind of that melamine point is deposited on bilayer graphene surface by thermal evaporation the present invention relates to graphene
Son, to modulate the preparation method of the electron adulterated bilayer graphene of graphene electrical properties.
Background technology
Graphene be it is a kind of by carbon atom withsp 2Orbital hybridization forms the two-dimensional material of honeycomb structure.From 2004, health
Si Tandingnuowoxiao loves and An Deliehaimu find graphene and prepare first graphene field effect transistor with
Come, be subject to extensively in field of photodetectors due to having very high carrier mobility, wide spectrum absorption and quick response
Concern, however, intrinsic single-layer graphene is due to zero band gap and weak light absorption（2.3%）, cause graphene-based photoelectricity and visit
It is small low with responsiveness to survey device on-off ratio, limits its application in photoelectric field, becomes its on-off ratio graphene band gap opening
It is most important in the application of photoelectric field to graphene greatly.Bilayer graphene is except there is the quantum anomaly similar to single-layer graphene
Hall effect and outer greatly than single-layer graphene photon absorbing intensity, bilayer graphene has higher carrier mobility, and by additional
Vertical electric field or doping can be with openings.
Chemical vapour deposition technique is to prepare one of large area, high quality monolayer graphene the best way at present, however by
In causing from restriction effect, preparation bilayer graphene is difficult, and only a few experiments team prepares the bilayer graphene of high quality.
So in order to which graphene is applied to photodetection field, it is necessary to prepare bilayer graphene enhancing to light absorption and it is adulterated
Realize electricity modulation.
The content of the invention
To be solved by this invention is exactly the problem of existing preparation bilayer graphene is difficult, provides one kind and is existed by thermal evaporation
Melamine molecule is deposited in bilayer graphene surface, to modulate the preparation of the electron adulterated bilayer graphene of graphene electrical properties
Method.
The preparation method of the electron adulterated bilayer graphene of the present invention, it is characterised in that this preparation method is with chemical vapor deposition
Area method prepares large area bilayer graphene, and reusable heat evaporation technique comes in one layer of melamine molecule of bilayer graphene surface evaporation
Graphene electrical properties are modulated, specific preparation process is as follows：
1）, bilayer graphene prepared on copper foil using chemical vapour deposition technique：Copper foil substrate is put into tube furnace, afterwards
It is evacuated to below 1Pa；Hydrogen argon gas mixed gas is passed through with 60sccm in tube furnace and was warming up to 1000 in 120 minutes
℃；Then methane is passed through 60 minutes with 20sccm amounts, pressure is maintained at 1500 Pa in tube furnace at this time；Then it is cooled to room temperature
Afterwards, turn off hydrogen argon gas mixed gas, take out the bilayer graphene sample for being grown on copper foil surface；
2）, transfer bilayer graphene：In step 1）One strata methyl methacrylate of spin coating above obtained bilayer graphene sample
Heating is evaporated 20 minutes and forms firm film in 80 DEG C of drying box after ester solution；It is molten polymethyl methacrylate will to be scribbled
Liquid, the copper foil with bilayer graphene be immersed in ferric chloride solution etch copper foil 1 to 2 it is small when；With load glass after to be etched
Copper foil is transferred in deionized water by piece to be impregnated 30 minutes, cleans remained on surface iron chloride and copper；After copper foil, band will be etched
The film for having graphene is transferred in target substrate, can obtain shifting in mesh with acetone removal polymethyl methacrylate solution
Mark the bilayer graphene in substrate.
3）, vapor deposition melamine：Using melamine as dopant, melamine is deposited to double-layer graphite with thermal evaporation
Alkene forms thin film on surface, you can obtains electron adulterated bilayer graphene.
Difference of this technology with preparing single-layer graphene maximum is to have tuned up the amount of hydrogen argon gas mixed gas and extended
Preparation time, can be by adjusting the amount of melamine, rate-determining steps 3）In be covered in the thickness of bilayer graphene surface film；
The doping of melamine enables the conduction type of graphene to realize the modulating action from strong p-type to weak p-type, is large area graphite
AlkenenType doping provides feasible program.
The preparation method of the electron adulterated bilayer graphene of the present invention, has the following advantages：
1）The innovation of overall technology route has that equipment and technical process are simple, preparation efficiency is high, at low cost and with obvious effects etc. special
Point is realized with reference to classical CVD method and thermal evaporation method to bilayer graphene surface doping, is realized electricity modulation, is avoided
The shortcomings that displacement doping causes carrier mobility low；
2）The method preparation doping bilayer graphene operation is feasible, and the doping bilayer graphene being prepared can realize double-deck stone
Black alkene conduction type, to the modulating action of weak p-type, direction and reference is specified for the modulation of graphene n-type from strong p-type；
3）Due to containing carbonnitrogen bond in melamine, there is absorption to ultraviolet, available in ultraviolet detector.
Description of the drawings
Fig. 1 is the AFM figures that chemical vapour deposition technique prepares bilayer graphene.
Fig. 2 is the Raman spectrogram that chemical vapour deposition technique prepares bilayer graphene.
Fig. 3 is bilayer graphene and doping bilayer graphene field-effect test result.
Specific embodiment
Embodiment 1：It is double to prepare large area with chemical vapour deposition technique for a kind of preparation method of electron adulterated bilayer graphene
Layer graphene, reusable heat evaporation technique modulate graphene electrical property in one layer of melamine molecule of bilayer graphene surface evaporation
Matter, specific preparation process are as follows：
1）, bilayer graphene prepared on copper foil using chemical vapour deposition technique：Copper foil substrate is put into tube furnace, afterwards
It is evacuated to below 1Pa；Hydrogen argon gas mixed gas is passed through with 60sccm in tube furnace and was warming up to 1000 in 120 minutes
℃；Then methane is passed through 60 minutes with 20sccm amounts, pressure is maintained at 1500 Pa in tube furnace at this time；Then it is cooled to room temperature
Afterwards, turn off hydrogen argon gas mixed gas, take out the bilayer graphene sample for being grown on copper foil surface；
2）, transfer bilayer graphene：In step 1）One strata methyl methacrylate of spin coating above obtained bilayer graphene sample
Heating is evaporated 20 minutes and forms firm film in 80 DEG C of drying box after ester solution；It is molten polymethyl methacrylate will to be scribbled
Liquid, the copper foil with bilayer graphene be immersed in ferric chloride solution etch copper foil 1 to 2 it is small when；With load glass after to be etched
Copper foil is transferred in deionized water by piece to be impregnated 30 minutes, cleans remained on surface iron chloride and copper；After copper foil, band will be etched
The film for having graphene is transferred in target substrate, can obtain shifting in mesh with acetone removal polymethyl methacrylate solution
Mark the bilayer graphene in substrate；
3）, vapor deposition melamine：Using melamine as dopant, melamine is deposited to bilayer graphene table with thermal evaporation
Thin film is formed on face.It weighs 0.5 g melamine powders to evaporate under vacuum on bilayer graphene surface, i.e.,
It can obtain electron adulterated bilayer graphene.
It, can be by adjusting the amount of melamine, rate-determining steps 3 in actual fabrication process）In be covered in double-layer graphite
The thickness of alkene surface film.
As shown in Figure 1, the bilayer graphene to be prepared with chemical vapour deposition technique is transferred to the AFM figures in target substrate,
See from figure in addition to the film of fold, there be one layer of discontinuous film on surface, shows the surface of bilayer graphene film
Pattern.
As shown in Fig. 2, be the Raman spectrogram of bilayer graphene film, Raman tests to obtain the D peak intensities of multiple points all
Very weak, it is possible thereby to which the defects of judging the graphene of growth rate is relatively low, graphene sample quality is higher；For 2D peaks and G peaks
Intensity ratio（I2D/IG≈1）, can clearly find out the number of plies of this graphene for bilayer.
Field-effect transistor after graphene surface adulterates one layer of melamine molecule, and electric property has been carried out to it
Test, as shown in figure 3, aerial electrical performance testing shows：The doping of melamine enables the conduction type of graphene
It is enough to realize from strong p-type to the modulating action of weak p-type, provide reference scheme to prepare the doping of large-area graphene n-type future.
Claims (1)
1. a kind of preparation method of electron adulterated bilayer graphene, it is characterised in that this preparation method is with chemical vapour deposition technique system
Standby large area bilayer graphene, reusable heat evaporation technique modulate stone in one layer of melamine molecule of bilayer graphene surface evaporation
Black alkene electrical properties, specific preparation process are as follows：
1）, bilayer graphene prepared on copper foil using chemical vapour deposition technique：Copper foil substrate is put into tube furnace, afterwards
It is evacuated to below 1Pa；Hydrogen argon gas mixed gas is passed through with 60sccm in tube furnace and was warming up to 1000 in 120 minutes
℃；Then methane is passed through 60 minutes with 20sccm amounts, pressure is maintained at 1500 Pa in tube furnace at this time；Then it is cooled to room temperature
Afterwards, turn off hydrogen argon gas mixed gas, take out the bilayer graphene sample for being grown on copper foil surface；
2）, transfer bilayer graphene：In step 1）One strata methyl methacrylate of spin coating above obtained bilayer graphene sample
Heating is evaporated 20 minutes and forms firm film in 80 DEG C of drying box after ester solution；It is molten polymethyl methacrylate will to be scribbled
Liquid, the copper foil with bilayer graphene be immersed in ferric chloride solution etch copper foil 1 to 2 it is small when；With load glass after to be etched
Copper foil is transferred in deionized water by piece to be impregnated 30 minutes, cleans remained on surface iron chloride and copper；After copper foil, band will be etched
The film for having graphene is transferred in target substrate, can obtain shifting in mesh with acetone removal polymethyl methacrylate solution
Mark the bilayer graphene in substrate；
3）, vapor deposition melamine：Using melamine as dopant, melamine is deposited to bilayer graphene table with thermal evaporation
Thin film is formed on face, you can obtain electron adulterated bilayer graphene.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110739399A (en) * | 2019-10-24 | 2020-01-31 | 昆明物理研究所 | NPB/nitrogen-doped graphene nano heterojunction ultraviolet detector with flexible vertical structure and preparation method thereof |
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| CN103072978A (en) * | 2013-02-04 | 2013-05-01 | 杭州格蓝丰纳米科技有限公司 | Chemical vapor deposition method for preparing dual-layer graphene |
| EP3181516A1 (en) * | 2015-12-16 | 2017-06-21 | Samsung Electronics Co., Ltd | Multilayer graphene, method of forming the same, device including the multilayer graphene, and method of manufacturing the device |
| CN105752965A (en) * | 2016-01-26 | 2016-07-13 | 无锡格菲电子薄膜科技有限公司 | Etching method for directly forming multi-layer graphene film in graphene prepared through CVD method |
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| CN110739399A (en) * | 2019-10-24 | 2020-01-31 | 昆明物理研究所 | NPB/nitrogen-doped graphene nano heterojunction ultraviolet detector with flexible vertical structure and preparation method thereof |
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