CN104108704B - A kind of Graphene transfer method - Google Patents
A kind of Graphene transfer method Download PDFInfo
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- CN104108704B CN104108704B CN201410331217.0A CN201410331217A CN104108704B CN 104108704 B CN104108704 B CN 104108704B CN 201410331217 A CN201410331217 A CN 201410331217A CN 104108704 B CN104108704 B CN 104108704B
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Abstract
The invention discloses a kind of Graphene transfer method, comprising: drop-burette is fixed on iron stand, have one of Graphene to face down tinsel length and be placed in target substrate surface, substrate be put in the below of drop-burette, tinsel is flattened; By the FeCl in drop-burette
3solution drips above tinsel, the FeCl flowed out by the on-off control controlling drop-burette
3amount of solution, makes do not have FeCl between Graphene and substrate
3solution enters; After soaking with dilute hydrochloric acid solution, repeatedly above-mentioned substrate is rinsed with deionized water, remove residual Fe
3+ion; Afterwards the substrate cleaned up is taken out, and with air gun, it is dried up.Present method adopts inorganic solution directly etching metal catalytic film by simple drop-burette system, have easy and simple to handle, cost is low, without organic residue, easily realize the advantages such as broad area device is integrated.
Description
Technical field
The invention provides a kind of Graphene transfer method getting involved (comprising organic film and organic solvent etc.) without the need to organism, relate to the new device preparation field of graphene-containing functional unit.
Background technology
Graphene arranges by monolayer carbon atom the two dimensional crystal formed by hexagon cellular shape.It has dirac taper energy band structure, excellent electrical and optical properties, has become a study hotspot of physics, chemistry, biology and material science.The Graphene size adopting micromechanics stripping method to prepare is little, yields poorly, and limits its application in device.In recent years, people adopt chemical vapour deposition (CVD) method to prepare big area, high-quality graphene on the catalytic films such as Ni or Cu paper tinsel.Can this Graphene be transferred in target substrate by the figure art of composition, prepare for device.Up to now, it take Graphene as the device of basic functional units that people have prepared multiple, comprises field-effect transistor, solar cell, nano generator, sensor.Owing to using organic materials and the acetone and other organic solvent such as PMMA (polymethylmethacrylate) in figure art of composition transfer Graphene process, and organic residue can bring infringement to the performance of grapheme material and device.A kind of Graphene transfer method got involved without the need to organism (comprising organic film and organic solvent etc.) of invention for the research of Graphene basic physics or device application aspect all very important.
Summary of the invention
The object of this invention is to provide a kind of Graphene transfer method got involved without the need to organism newly.
Graphene wherein used is prepared in tinsel (such as: Copper Foil, nickel foil etc.) by CVD.The scope of tinsel length and width is 0.3cm ~ 10cm, and individual layer or bilayer graphene cover its surface overwhelming majority.
Technical scheme provided by the invention is as follows:
A kind of Graphene transfer method, it is characterized in that, be fixed on by drop-burette on iron stand have one of Graphene to face down tinsel length and be placed in target substrate surface, substrate is put in the below of drop-burette, tinsel is flattened (such as: by other smooth substrate pressures); By the FeCl in drop-burette
3solution drips above tinsel, the FeCl flowed out by the on-off control controlling drop-burette
3amount of solution, makes do not have FeCl between Graphene and substrate
3solution enters, thus avoids Fe
3+remain on substrate and pollution is produced to Graphene sample.
Preferred:
Described Graphene transfer method, is characterized in that, described tinsel is Copper Foil or nickel foil.
Described Graphene transfer method, is characterized in that, substrate used is solid substrate.
Described Graphene transfer method, is characterized in that, substrate used is silicon chip.
Another kind of Graphene transfer method, is characterized in that, be fixed on by drop-burette on iron stand, has one of Graphene to face down tinsel length and is placed in target substrate surface, substrate is put in the below of drop-burette, tinsel is flattened; By rare HCl and the H in drop-burette
2o
2mixed solution etchant solution drips above tinsel, and the etchant solution amount flowed out by the on-off control controlling drop-burette, makes do not have etchant solution to enter between Graphene and substrate.
Another Graphene transfer method, is characterized in that, comprise the steps:
1) Graphene is prepared in the upper CVD that adopts of tinsel (Ni or Cu etc.);
2) have one of Graphene to face down tinsel growth to be placed in target substrate (such as: silicon chip etc.) surface, tinsel to be flattened, such as: by other smooth substrate pressures;
3) substrate with tinsel is placed in the below of titration system, makes FeCl by drop-burette
3solution flows in tinsel, controls the FeCl above Graphene by the spile below drop-burette simultaneously
3the amount of solution; Ensure that the solution in dropper is communicated with in corrosion process all the time with the solution in tinsel;
4) sample is left standstill, until FeCl
3by its region tinsel corrosion completely, final Graphene can at FeCl for solution
3adhere to target substrate under the acting in conjunction of solution gravity and Van der Waals for;
5) after soaking (such as: soak 30 minutes) with dilute hydrochloric acid solution, repeatedly above-mentioned substrate is rinsed with deionized water, remove residual Fe
3+ion; Afterwards the substrate cleaned up is taken out, and with air gun, it is dried up.
Preferred:
Described Graphene transfer method, is characterized in that, step 3) in, FeCl
3the concentration of solution is 0.01g/ml-1g/ml.
Described Graphene transfer method, is characterized in that, step 3) in, FeCl
3the concentration of solution is 0.1g/ml.
Described Graphene transfer method, is characterized in that, step 4) in, sample is being left standstill period, and to sample heating with fast reaction speed, Heating temperature is 70 DEG C, corrode 30 minutes, but temperature can not higher than 90 DEG C.
Described Graphene transfer method, is characterized in that, step 5) in, the concentration of dilute hydrochloric acid solution is 0.01mol/L-2mol/L, preferred 1mol/L.
Compared with prior art, the invention has the beneficial effects as follows:
Get involved without the need to organism, easy and simple to handle, the organic impurity such as PMMA or acetone can not be remained, thus avoid the infringement of organic residue to grapheme material quality and device performance.The method has wide practical use in the new device taking Graphene as functional unit.
Accompanying drawing explanation
Fig. 1 is the Graphene transfer method schematic diagram (for Copper Foil) that the present invention proposes.
Fig. 2 transfers to 300nmSiO by the present invention
2the optical microscope photograph of the Graphene on/Si substrate.
Fig. 3 is the Raman spectrum of the Graphene in Fig. 1.
Embodiment
The present invention adopts the Graphene transfer method of the directly etching tinsel getting involved (comprising organic film and organic solvent etc.) without the need to organism.As shown in Figure 1, step is as follows for major experimental process:
1) Graphene is prepared in the upper CVD that adopts of tinsel (such as: Cu, Ni etc.).
2) have one of Graphene to face down tinsel growth to be placed in target substrate (such as: silicon chip etc.) surface, tinsel to be flattened, such as: by other smooth substrate pressures.。
3) target substrate with tinsel is placed in the below of titration system.FeCl is made by drop-burette
3(0.1g/ml) solution flows in tinsel, is controlled the FeCl remained on above Graphene by the spile below drop-burette simultaneously
3the amount of solution; Ensure that the solution in dropper is communicated with in corrosion process all the time with the solution in tinsel.
4) sample is left standstill, until FeCl
3solution by its region tinsel corrosion completely.70 DEG C are heated to, with fast reaction speed to sample therebetween.Heat-processed continues 30 minutes altogether.Final Graphene can at FeCl
3adhere to target substrate under the acting in conjunction of solution gravity and Van der Waals for.
5) after soaking (such as: soak 10 minutes) with dilute hydrochloric acid solution (1mol/L), repeatedly above-mentioned substrate is rinsed with deionized water, remove residual Fe
3+ion.Afterwards the substrate cleaned up is taken out, and with air gun, it is dried up.
Embodiment 1
The organic film material (such as: PMMA etc.) of the present invention without the need to using in ordinary graphite alkene tranfer system (the figure art of composition), Graphene in the upper growth of tinsel (Ni or Cu etc.) can be transferred directly to other solid substrate surfaces (such as: silicon chip, quartz plate, PET etc.) on.
As shown in Figure 1, for Copper Foil, transfer process is as follows:
There is the Copper Foil of Graphene to be positioned over target substrate surface growth, make to face down with one of Graphene; By FeCl
3solution (0.1g/ml) drips in the middle part of Copper Foil by drop-burette; After copper is corroded completely, Graphene will adhere to solid substrate intimate surface under the gravity of solution and the acting in conjunction of Van der Waals for; Use dilute hydrochloric acid solution (1mol/L) and deionized water to clean sample afterwards, then can obtain clean Graphene in target substrate.
The method is compared traditional transfer method and is had easy and simple to handle, without the need to the organic materials such as PMMA, acetone, thus can not remain the advantages such as organic impurity.
Fig. 2 transfers to 300nmSiO by the present invention
2the optical microscope photograph of the Graphene on/Si substrate.201 regions, figure top are the substrate not having Graphene to cover, and region, below 202 is Graphene.
Fig. 3 is the Raman spectrum of the Graphene in Fig. 1.It is made up of two main peaks: G peak and 2D peak.The ratio at 2D peak and G peak is approximately 2, describes the individual layer characteristic of this Graphene.In addition, the D peak relevant to Graphene defect is more weak, illustrates that this Graphene quality is better.
Table 1 is the hall measurement data such as the square resistance of the Graphene adopting the present invention to obtain.
The hall measurement result of the Graphene after table 1. adopts the present invention to shift.Wherein, the mobility of sample is up to 941cm
2/ Vs.Show that shifting rear Graphene still has good electrology characteristic.
Claims (9)
1. a Graphene transfer method, is characterized in that, is fixed on by drop-burette on iron stand, has one of Graphene to face down tinsel length and is placed in target substrate surface, substrate is put in the below of drop-burette, tinsel is flattened; By the FeCl in drop-burette
3solution drips above tinsel, the FeCl flowed out by the on-off control controlling drop-burette
3amount of solution, makes do not have FeCl between Graphene and substrate
3solution enters, and described tinsel is Copper Foil or nickel foil.
2. Graphene transfer method as claimed in claim 1, it is characterized in that, substrate used is solid substrate.
3. Graphene transfer method as claimed in claim 1, it is characterized in that, substrate used is silicon chip.
4. a Graphene transfer method, is characterized in that, is fixed on by drop-burette on iron stand, has one of Graphene to face down tinsel length and is placed in target substrate surface, substrate is put in the below of drop-burette, tinsel is flattened; By rare HCl and the H in drop-burette
2o
2mixed solution etchant solution drips above tinsel, and the etchant solution amount flowed out by the on-off control controlling drop-burette, make do not have etchant solution to enter between Graphene and substrate, described tinsel is Copper Foil or nickel foil.
5. a Graphene transfer method, is characterized in that, comprises the steps:
1) adopt CVD to prepare Graphene on metal foil, described tinsel is Copper Foil or nickel foil;
2) have one of Graphene to face down tinsel growth to be placed in target substrate surface, tinsel is flattened;
3) substrate with tinsel is placed in the below of titration system, makes FeCl by drop-burette
3solution flows in tinsel, controls the FeCl above Graphene by the spile below drop-burette simultaneously
3the amount of solution; Ensure that the solution in drop-burette is communicated with in corrosion process all the time with the solution in tinsel;
4) sample is left standstill, until FeCl
3by its region tinsel corrosion completely, final Graphene can at FeCl for solution
3adhere to target substrate under the acting in conjunction of solution gravity and Van der Waals for;
5) after soaking with dilute hydrochloric acid solution, repeatedly above-mentioned substrate is rinsed with deionized water, remove residual Fe
3+ion; Afterwards the substrate cleaned up is taken out, and with air gun, it is dried up.
6. Graphene transfer method as claimed in claim 5, is characterized in that, step 3) in, FeCl
3the concentration of solution is 0.01g/mL-1g/mL.
7. Graphene transfer method as claimed in claim 5, is characterized in that, step 3) in, FeCl
3the concentration of solution is 0.1g/mL.
8. Graphene transfer method as claimed in claim 5, is characterized in that, step 4) in, sample is being left standstill period, and to sample heating with fast reaction speed, Heating temperature is 70 DEG C.
9. Graphene transfer method as claimed in claim 5, is characterized in that, step 5) in, the concentration of dilute hydrochloric acid solution is 0.01mol/L-2mol/L.
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| CN104108704B true CN104108704B (en) | 2016-01-20 |
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| CN105140083B (en) * | 2015-06-24 | 2017-05-10 | 中国科学院生物物理研究所 | Preparation method of grid of transmission electron microscope |
| CN105321808B (en) * | 2015-07-30 | 2018-09-28 | 中国电子科技集团公司第五十五研究所 | A kind of CVD graphene FET device manufacturing methods of avoidable organic contamination |
| CN107311158B (en) * | 2017-06-24 | 2019-11-08 | 南昌航空大学 | A method of it preparing graphene film on Ni-based and is transferred to other substrates |
| CN114852999B (en) * | 2022-04-27 | 2024-04-05 | 云南大学 | Method for transferring graphene |
| CN115650219B (en) * | 2022-10-08 | 2024-04-16 | 复旦大学 | Transfer method of CVD graphene |
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| CN102616769A (en) * | 2012-03-19 | 2012-08-01 | 浙江大学 | Direct graphene film transfer method |
| CN103342472A (en) * | 2013-07-11 | 2013-10-09 | 常州二维碳素科技有限公司 | Method for transferring graphene film |
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| TWI485290B (en) * | 2012-12-19 | 2015-05-21 | Univ Nat Taiwan | Method for transferring graphene layer |
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| CN102616769A (en) * | 2012-03-19 | 2012-08-01 | 浙江大学 | Direct graphene film transfer method |
| CN103342472A (en) * | 2013-07-11 | 2013-10-09 | 常州二维碳素科技有限公司 | Method for transferring graphene film |
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