CN103449418A - Method for transferring graphene with atomic cleanness - Google Patents
Method for transferring graphene with atomic cleanness Download PDFInfo
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- CN103449418A CN103449418A CN2013103623565A CN201310362356A CN103449418A CN 103449418 A CN103449418 A CN 103449418A CN 2013103623565 A CN2013103623565 A CN 2013103623565A CN 201310362356 A CN201310362356 A CN 201310362356A CN 103449418 A CN103449418 A CN 103449418A
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Abstract
The invention discloses a method for efficiently transferring CVD (Chemical Vapor Deposition) graphene and acquiring atomically clean surfaces. The method comprises the following steps: spin-coating a layer of PMMA (polymethyl methacrylate) solution on the surface of a graphene/metal substrate, removing the metal substrate through corrosion of an (NH4)2S2O8 solution after being cured, cleaning graphene/PMMA, fishing out through a target substrate and then drying, then dissolving the PMMA layer through an organic acid solvent, and finally further removing the residual PMMA on the surface of the graphene through a high-temperature annealing manner, thus acquiring the atomically clean graphene surfaces. The graphene surface is large in area, complete in structure and little in defects and residual PMMA. According to the method, the residual PMMA is little, and the atomically clean surfaces can be more easily acquired. The graphene acquired through adopting the method is applicable to constructing electronic devices such as a field effect transistor, a light-emitting diode and a transparent electrode, and also can be used for theoretical research of surface interfaces.
Description
Technical field
The present invention relates to a kind of method that Atomically clean shifts Graphene, especially a kind of efficient transfer of CVD Graphene and the method for obtaining atomically clean surfaces, belong to nano material and technical field.
Background technology
Graphene is due to the performance with a series of excellences, as the carrier mobility of superelevation, thermal conductivity, physical strength etc., since 2004 find, has been physics always, materialogy, the study hotspot of numerous Disciplinary Frontiers such as surface and interface science.The main obtain manner of Graphene has machinery/solution stripping method, SiC epitaxial growth method, redox graphene method and chemical Vapor deposition process (CVD method).Wherein the CVD method is controlled owing to having the number of plies, and growth size is easy to the advantages such as amplification and in fields such as touch screen-device and transparency electrodes, shows potential application prospect.
Although the growth of CVD Graphene has reached ripe controlled stage at aspects such as pattern and defect controls, but be based on the application of the character such as Graphene carrier mobility, light transmission, as ultra high frequency field-effect transistor, touch screen-device, flexible electrode etc. all have particular requirement (Nature Nanotechnology. to the load substrate of Graphene, 2010,5,722-726), this require the respective substrates that is transferred to that the Graphene of CVD method growth can be efficient controlled.The current main method shifted about the CVD Graphene is the auxiliary transfer method of polymethylmethacrylate (PMMA).In the method, PMMA is easy to repolymerization and the place of the residue problem that the causes bottleneck that to be restriction the method further develop always.The people such as Ruoff find, Graphene surface PMMA residual make the electricity of Graphene and optical property have a greatly reduced quality (Nano Letters., 2013,13,1462-1467).A kind of residual and transfer method that do not introduce additional defects of PMMA that can reduce seems particularly important.
Summary of the invention
The object of the present invention is to provide a kind of efficient transfer of CVD Graphene and obtain the transfer method of atomically clean surfaces.Principal feature of the present invention is to introduce simple organic acid solvent treatment process and the CVD Graphene that obtains having Atomically clean.Graphene area provided by the invention is large, structural integrity, and defect and PMMA are residual few.Than traditional method of being removal of solvents PMMA with acetone, method PMMA provided by the present invention is residual few, the surface that can obtain Atomically clean.The Graphene that the method is obtained is applicable to construct electron device as field-effect transistor, photodiode, transparency electrode etc., also can be used for the theoretical investigation of surface and interface.
The present invention is achieved through the following technical solutions:
A kind of Atomically clean CVD Graphene transfer method, is characterized in that, selects organic acid to make removal of solvents PMMA coating.
According to the present invention, described organic acid is selected from least one in acetic acid, trifluoroacetic acid, formic acid, oxalic acid.Preferred acetic acid, acetic acid is best for solvability and the palliating degradation degree of PMMA.
The present invention adopts organic acid solvent with the degradation property good to PMMA and solvability, method than the single dependence acetone solution of tradition removal PMMA, it is more thorough that method provided by the present invention is removed PMMA, the CVD Graphene surface that can obtain Atomically clean.
According to the present invention, described transfer method comprises: the target substrate that will sprawl Graphene/PMMA is soaked in organic acid soln, dissolves PMMA and can obtain the target substrate of sprawling Graphene.
According to the present invention, in the described target substrate of sprawling Graphene/PMMA, be soaked in before organic acid soln is soaked in organic acid soln, also comprise the steps:
(1) substrate surface spin coating one deck PMMA solution of Graphene, curing molding are arranged in growth;
(2) the PMMA layer of step (1) gained sample is soaked in to the described substrate of corrosion in etchant solution upward, the PMMA that then will be stained with Graphene is transferred in deionized water and cleans survivor ion;
(3) choose suitable target substrate and pick up Graphene/PMMA layer, drying treatment.
According to the present invention, it is the metal base such as Copper Foil, Ni, Pt that described growth has the substrate of Graphene.
According to the present invention, described method specifically comprises the steps:
(1) substrate surface spin coating one deck PMMA solution of Graphene, curing molding are arranged in growth;
(2) the PMMA layer of step (1) gained sample is soaked in upward in etchant solution and corrodes substrate, the PMMA that then will be stained with Graphene is transferred in deionized water and cleans survivor ion;
(3) choose suitable target substrate and pick up Graphene/PMMA layer, drying treatment;
(4) target substrate that will sprawl Graphene/PMMA is soaked in organic acid soln, dissolves PMMA and can obtain the target substrate of sprawling Graphene;
(5) finally will be covered with the substrate of Graphene in H
2anneal in/Ar gas mixture, the Graphene surface that can obtain Atomically clean.
In aforesaid method, the PMMA solution in step (1) is spin-coated on the Graphene surface filming.Then process the adhesive attraction increased between PMMA and Graphene by being heating and curing.
According to the present invention, in step (1), the preparation method of Graphene can be referring to Nanotechnology, 2012,23,0957-4484.
According to the present invention, in growth, the spin coating rotating speed of the surperficial spin coating one deck PMMA solution of substrate (as metal base such as Copper Foil, Ni, Pt) of Graphene being arranged is 3000rpm.The metal base that will be coated with PMMA after the spin coating end is placed in hot-plate and is heating and curing.Preferably, the Heating temperature of described hot-plate is 80-200 ℃, preferably 100-180 ℃.
In aforesaid method, the etchant solution of step (2) can be done corresponding selection according to the substrate material of CVD growing graphene.The growth substrate of CVD Graphene commonly used has Ni and Cu.Wherein the Cu surface is easy to form single-layer graphene, and the Ni surface is easy to form multi-layer graphene.The preferred Cu substrate of this patent.The Cu corrosive fluid mainly contains commercialization copper corrosion liquid (Transene, CE-100), FeCl
3solution and (NH
4)
2s
2o
8three kinds, (NH wherein
4)
2s
2o
8solution can not cause metal ion residual, contributes to construct the devices such as some graphene field effect transistors.Therefore the preferred corrosive fluid of the present invention is (NH
4)
2s
2o
8solution.
According to the present invention, described (NH
4)
2s
2o
8the solubility of solution is 0.05-2mol/L, preferably 0.1-1mol/L.
According to the present invention, the treatment time of described etchant solution is 1-5 hour, preferably 2-3 hour.According to the present invention, after Copper Foil fully dissolves, be transferred in clear water and soak, soak time is 30-90 minute, preferably 40-60 minute.
In aforesaid method, the drying treatment temperature of the PMMA/ Graphene/target substrate in step (3) is 80-180 ℃.
According to the present invention, the target substrate in step (3) is selected from: SiO
2, mica etc.On theoretical method provided by the present invention, the CVD Graphene can be transferred to the nonreactive any substrate of organic acid in addition.
According to the present invention, after cleaning the survivor ion on Graphene surface in step (3), the target substrate of choosing a slice cleaning picks up Graphene and PMMA thin layer.
After in step (3), Graphene is transferred to target substrate, drying treatment can promote interaction and the absorption of Graphene and substrate.
According to the present invention, in step (3), the sample after picking up is transferred to the warm table heating, described Heating temperature is for being preferably 100-150 ℃.Be 1-3h described heat-up time, and Graphene is fully contacted with target substrate.
In aforesaid method, the organic acid soln in step (4) is selected from least one in acetic acid, trifluoroacetic acid, formic acid, oxalic acid.Wherein acetic acid is best for solvability and the palliating degradation degree of PMMA.
According to the present invention, after sample is cooled to room temperature, it is soaked in acetic acid solution, described soak time is 1-5 hour, preferably 2-4 hour.Described soaking temperature is constant temperature, and preferably 40-80 ℃, more have 55 ℃ of-70 ℃ of constant temperature to process.
In aforesaid method, the annealing atmosphere of the Graphene in step (5) is 5-15%H
2/ Ar gas mixture, annealing time is 1-4h, and annealing temperature is 350-500 ℃, and processing pressure is a standard atmospheric pressure.
The present invention also provides the Atomically clean Graphene surface of being processed gained by aforesaid method.
According to the present invention, described Atomically clean Graphene surface tissue is complete.The preferred surface waviness is less than 0.2nm, is the atomically flating surface.
According to the present invention, do not introduce CVD growth additional defects in addition, PMMA is residual few.
The present invention also provides a kind of application of being processed the Atomically clean Graphene surface obtained by aforesaid method, it is characterized in that, described Graphene can be used for constructing the electron device such as field-effect transistor, photodiode, transparency electrode or the microprocess with the research surface and interface as the atomically flating substrate.
According to the present invention, by scanning tunnel microscope, can clearly observe the self-assembled structures of 8-octyloxy CuPc on the Graphene surface at the graphene-based end provided by the invention.
The invention has the advantages that, use organic acid soln instead and dissolve the residue problem that the PMMA coating can greatly be improved polymerization PMMA in conventional acetone treatment method; It is residual that another advantage of the present invention is that Graphene surface PMMA can be removed in the atom level aspect in the Graphene surface after anneal, the Graphene surface that obtains Atomically clean.
Compared with the prior art, the present invention has following features:
(1) organic acid solvent used in the present invention is nontoxic, cheap, and in Graphene surface noresidue and Adsorption Effect.
(2) after anneal, the Graphene surface reaches Atomically clean, and can obtain the micron order on a large scale clean surface residual without PMMA.
(3) Graphene that the present invention obtains, when abundant reduction PMMA is residual, is not introduced extra defect, has greatly retained the initial performance of CVD Graphene.
The accompanying drawing explanation
The transfer that Fig. 1 is CVD Graphene provided by the invention and processing flow chart.
The scanning electron microscope (SEM) photograph that Fig. 2 is the initial pattern of copper foil surface Graphene.
Fig. 3 is that embodiment 1 is transferred to SiO
2the optical microphotograph picture of substrate Graphene.
Fig. 4 is that reference examples 1 is transferred to SiO
2the optical microphotograph picture of substrate Graphene.
Fig. 5 is that embodiment 1 is transferred to SiO
2the atomic force microscope images of substrate surface Graphene.
Fig. 6 is that reference examples 1 is transferred to SiO
2the atomic force microscope images of substrate surface Graphene.
Fig. 7 is the large area scanning tunnel microscope image that embodiment 2 is transferred to mica substrate surface Graphene.
Fig. 8 is the high resolution surface sweeping tunnel microscope atomic diagram picture that embodiment 2 is transferred to mica substrate surface Graphene.
Fig. 9 is that embodiment 3 Graphene surfaces drip 8-octyloxy Copper Phthalocyanine Molecule surface sweeping tunnel microscope image afterwards.
Figure 10 is that embodiment 1 is transferred to SiO
2the Raman spectrogram of substrate surface Graphene, wherein insert pictures for Graphene before shifting at the Initial R aman of copper foil surface spectrogram.
Figure 11 is that embodiment 1 is transferred to SiO
2the face that the substrate surface Graphene is obtained with D peak and the mapping of G peak Raman strength ratio is swept figure.
Wherein the schema of Fig. 1 is described below step: at first at Graphene/copper foil surface spin coating one deck PMMA solution, pass through (NH after it solidifies
4)
2s
2o
8solution corrosion is removed Copper Foil, Graphene/PMMA picks up drying by target substrate after cleaning, then select organic acid solvent to dissolve the PMMA layer, finally by the high temperature annealing mode, further remove Graphene remained on surface PMMA, thereby obtain the Graphene surface of Atomically clean.
In Fig. 2, the SEM result shows, the Graphene uniform surface of CVD method growth is smooth, inclusion-free and obviously damaged.
Comparison diagram 3 and Fig. 4.While selecting acetone to make solvent, the Graphene surface is easy to grey floss in residual PMMA(Fig. 4), organic acid is done the Graphene surface that solvent can obtain the homogeneous cleaning.
In Fig. 5, bright wisp is formed intrinsic fold in the Graphene process of growth, and PMMA is residual less.
In Fig. 6, the Graphene surface is except the intrinsic growth fold of Graphene, and PMMA is residual obviously visible, illustrates that traditional acetone is removed the PMMA effect undesirable, and it is more thorough that organic solvent is removed PMMA.
In Fig. 7, the uniform surface inclusion-free of Graphene, the surface undulation degree is less than 0.2nm, is the atomically flating surface.
In Fig. 8, single bag parameter of cellular high resolving power atomic diagram picture is 0.25nm, consistent with the theoretical size of Graphene, illustrates that graphene-structured is complete.
In Fig. 9,8-octyloxy Copper Phthalocyanine Molecule is obviously visible, and Graphene surfacing cleaning is described, also shows that treatment process provided by the present invention can provide the graphene-based end of atomically flating, can be used for the microscopic theory research of surface and interface simultaneously.
After in Figure 10, Graphene is transferred to the SiO2/Si substrate, D peak (～1350cm in the Raman spectrogram
-1place) without obviously strengthening, peak shape with shift before copper foil surface Graphene signal consistent, illustrate that treatment process provided by the present invention do not introduce Graphene growth additional defects in addition.
In Figure 11, sample surfaces D peak intensity and G peak intensity ratio are less than 0.1 zone and are greater than 90%, illustrate that the good defect of Graphene character is less.
Embodiment
Below by specific embodiment, the present invention will be described, but it will be appreciated by those skilled in the art that the present invention is not limited thereto, and any improvement of making on basis of the present invention and invention are all within protection scope of the present invention.
Experimental technique described in following embodiment, if no special instructions, be ordinary method; Described reagent and material, if no special instructions, all can obtain from commercial channels.
Embodiment 1, the acetic acid of take are transferred to SiO by the CVD Graphene as organic acid soln
2substrate surface
Preparation process is as follows:
(1) the long Copper Foil that Graphene arranged (concrete preparation method can be with reference to Nanotechnology .2012,23,0957-4484.) surperficial spin coating one deck PMMA solution (960PMMA A4, MicroChem), the spin coating rotating speed is 3000rpm.The Copper Foil that will be coated with PMMA after the spin coating end is placed in 180 ℃ of hot-plates and is heating and curing.
(2) sample P MMA faces up and floats on 0.1mol/L (NH
4)
2s
2o
8solution surface, corrosion treatment 3h.After Copper Foil fully dissolves, be transferred in clear water and soak 60min.
(3), after cleaning the survivor ion on Graphene surface, choose the SiO of a slice cleaning
2substrate picks up Graphene and PMMA thin layer.Shift sample to 180 ℃ of heating 1h of warm table, make Graphene and SiO
2substrate fully contacts.
(4) after sample is cooled to room temperature, it is soaked in acetic acid solution, 55 ℃ of constant temperature are processed 1h.
(5) by clean Graphene/SiO
2substrate is transferred to 350 ℃ of normal pressure anneal in tube furnace, and the treatment time is 1h, and processing atmosphere is 5%H
2/ Ar gas mixture.
Reference examples 1, the acetone of take are transferred to SiO by the CVD Graphene as solvent
2substrate surface
Adopt the traditional acetone solvent to shift the CVD Graphene to SiO
2substrate surface, except being transferred in acetone soln by sample in step 4, all the other operations are all identical with embodiment 1.
Adopt organic acid to make solvent and shift the CVD Graphene to the mica substrate surface, except in step (3) by target substrate by SiO
2change into outside mica, all the other operations are all identical with embodiment 1.
Embodiment 3, the resulting Graphene of embodiment 2 of take are substrate, at the self-assembly layer of its surface construction 8-octyloxy Copper Phthalocyanine Molecule.
The Graphene that the embodiment 2 of take is obtained is substrate, drips concentration on its surface and is about 10
-5the toluene solution of mol/L8-octyloxy CuPc, treat can obtain the self-assembly layer of 8-octyloxy CuPc on the Graphene surface after solvent evaporates.
Comparison diagram 3 and Fig. 4 can find, though conventional solvent acetone can be dissolved most PMMA coatings, but excessively the PMMA of polymerization is residual still very serious for part, and the acetic acid of take can greatly improve the residue problem of Graphene surface PMMA as solvent.In the afm scan image, the residual acetone that obviously is less than of Graphene surface PMMA that organic acid is crossed as solvent treatment is done the Graphene surface that solvent was processed, and accordingly result as shown in Figure 5 and Figure 6.
In addition, to mica surface Graphene in embodiment 2, optional zone is done the scanning tunnel microscope imaging and can be obtained atomically flating image on a large scale, and accordingly result as shown in Figure 7.
High resolution atom picture shown in Fig. 8 also shows that the cell parameter of the cellular hexagonal structure of sample surfaces is 0.25nm, and it is consistent with theoretical Graphene cell parameter, has further verified existence and the structural integrity of Graphene.
In Fig. 9, in embodiment 3,8-octyloxy Copper Phthalocyanine Molecule is high-visible, and surface is residual without PMMA, and the substrate waviness is in the molecular level scope.This illustrate that transfer method provided by the present invention can obtain the Graphene surface of Atomically clean.
The sample of processing is done to the Raman spectrogram, result as shown in figure 10, wherein 2D peak intensity and G peak intensity ratio are about 2, a little less than the D peak intensity, this result is consistent with the CVD Graphene before transfer, this prove, jump operation is the Graphene characteristic of former CVD Graphene that substantially gone up intact preservation later, and transfer method provided by the present invention does not produce obvious defective effect to Graphene.The Raman face is done to D peak intensity and G peak intensity ratio in the optional zone of Graphene sample surfaces and sweep, experimental result is as Figure 11, and it also shows that the Graphene defect shifted is less, best in quality.
Embodiment 4, the acetic acid of take are transferred to SiO by the CVD Graphene as organic acid soln
2substrate surface
Preparation process is as follows:
(1) the long Pt substrate that Graphene arranged (concrete preparation method can be with reference to Nanotechnology .2012,23,0957-4484.) surperficial spin coating one deck PMMA solution (960PMMA A4, MicroChem), the spin coating rotating speed is 3000rpm.The Pt substrate that will be coated with PMMA after the spin coating end is placed in 160 ℃ of hot-plates and is heating and curing.
(2) sample P MMA faces up and floats on 0.15mol/L (NH
4)
2s
2o
8solution surface, corrosion treatment 2.5h.After Copper Foil fully dissolves, be transferred in clear water and soak 40min.
(3), after cleaning the survivor ion on Graphene surface, choose the SiO of a slice cleaning
2substrate picks up Graphene and PMMA thin layer.Shift sample to 180 ℃ of heating 2h of warm table, make Graphene and SiO
2substrate fully contacts.
(4) after sample is cooled to room temperature, it is soaked in acetic acid solution, 55 ℃ of constant temperature are processed 1h.
(5) by clean Graphene/SiO
2substrate is transferred to 350 ℃ of normal pressure anneal in tube furnace, and the treatment time is 1.5h, and processing atmosphere is 8%H
2/ Ar gas mixture.
Claims (10)
1. the transfer method of an Atomically clean CVD Graphene, is characterized in that, selects organic acid to make removal of solvents PMMA coating.
Preferably, described organic acid is selected from least one in acetic acid, trifluoroacetic acid, formic acid, oxalic acid.Preferred acetic acid.
2. according to the transfer method of claim 1, it is characterized in that, described transfer method comprises: the target substrate that will sprawl Graphene/PMMA is soaked in organic acid soln, dissolves PMMA and can obtain the target substrate of sprawling Graphene.
3. according to the transfer method of claim 1-2 any one, it is characterized in that, described method comprises the steps:
(1) the surperficial spin coating one deck PMMA solution of metal base (as Copper Foil or other metal base) of Graphene, curing molding are arranged in growth;
(2) the PMMA layer of sample step (1) obtained is soaked in corroding metal substrate in etchant solution upward, and the PMMA that then will be stained with Graphene is transferred in deionized water and cleans survivor ion;
(3) choose suitable target substrate and pick up Graphene/PMMA layer, drying treatment;
(4) target substrate that will sprawl Graphene/PMMA is soaked in organic acid soln, dissolves PMMA and can obtain the target substrate of sprawling Graphene;
(5) finally will be covered with the substrate of Graphene in H
2anneal in/Ar gas mixture, the Graphene surface that can obtain Atomically clean.
4. according to the method for claim 1-3 any one, it is characterized in that: in step (1), PMMA solution is coated on CVD Graphene surface by the spin coating mode.Preferably by being heating and curing, processing and increase adhesive attraction between PMMA and Graphene.
Preferably, in length, the spin coating rotating speed of copper foil surface spin coating one deck PMMA solution of Graphene being arranged is 3000rpm.
Preferably, the Copper Foil that spin coating will be coated with PMMA after finishing is placed in hot-plate and is heating and curing.Preferably, the Heating temperature of described hot-plate is 80-200 ℃, preferably 100-180 ℃.
5. according to the method for claim 1-4 any one, it is characterized in that: the etchant solution of step (2) is selected from commercialization copper corrosion liquid (Transene, CE-100), FeCl
3solution or (NH
4)
2s
2o
8three kinds.Described growth substrate has Ni and Cu.Its
Preferably, described corrosive fluid is (NH
4)
2s
2o
8solution.Graphene surface survivor ion is cleaned by deionized water.
Preferably, described (NH
4)
2s
2o
8the solubility of solution is 0.05-2mol/L, preferably 0.1-1mol/L.
Preferably, the treatment time of described etchant solution is 1-5 hour, preferably 2-3 hour.Preferably, after Copper Foil fully dissolves, be transferred in clear water and soak, soak time is 30-90 minute, preferably 40-60 minute.
6. according to the method for claim 1-5 any one, it is characterized in that: the drying treatment temperature of the PMMA/ Graphene/target substrate in step (3) is 80-180 ℃.Preferably, target substrate is selected from: SiO
2, mica etc.
Preferably, after cleaning the survivor ion on Graphene surface in step (3), choose the SiO of a slice cleaning
2substrate picks up Graphene and PMMA thin layer.After in step (3), Graphene is transferred to target substrate, drying treatment can promote interaction and the absorption of Graphene and substrate.
Preferably, in step (3), the sample after picking up is transferred to the warm table heating, described Heating temperature is for being preferably 100-150 ℃.Be 1-3h described heat-up time, makes Graphene and SiO
2substrate fully contacts.
7. according to the method for claim 1-6 any one, it is characterized in that: PMMA removes by organic acid solvent in step (4), wherein the organic acid solvent choosing to following at least one: acetic acid, trifluoroacetic acid, formic acid, oxalic acid.Preferred acetic acid.
Preferably, after sample is cooled to room temperature, it is soaked in acetic acid solution, described soak time is 1-5 hour, preferably 2-4 hour.Described soaking temperature is constant temperature, and preferably 40-80 ℃, more have 55 ℃ of-70 ℃ of constant temperature to process.
8. according to the method for claim 1-7 any one, it is characterized in that: in step (5), the remaining PMMA on Graphene surface passes through H
2the annealing of/Ar mixed atmosphere is further removed.The annealing atmosphere of described Graphene is 5-15%H
2/ Ar gas mixture, annealing time is 1-4h, and annealing temperature is 350-500 ℃, and the pressure of processing is a normal atmosphere.
9. the method by claim 1-8 any one is processed the Atomically clean Graphene surface obtained.
Preferably, described Atomically clean Graphene surface tissue is complete.The preferred surface waviness is less than 0.2nm, is the atomically flating surface.
10. the method for claim 1-8 any one is processed the Atomically clean Graphene surface of acquisition for constructing electron device or the application with the microprocess of research surface and interface as the atomically flating substrate.Be preferred in field-effect transistor, photodiode, transparency electrode.
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