CN103924188A - Method for graphene in-situ growth on insulation substrate through double-flame method under atmospheric environment - Google Patents
Method for graphene in-situ growth on insulation substrate through double-flame method under atmospheric environment Download PDFInfo
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Abstract
The invention discloses a method for graphene in-situ growth on an insulation substrate through a double-flame method under the atmospheric environment. A nickel film is deposited on a SiO2 substrate first, then the carburization/decarbonization mechanism of the nickel film and an unbalance surface segregation process are used, and graphene thin films are formed on the SiO2 substrate. The graphene thin films can grow on the upper face and the lower face of the nickel film, then the nickel film and a graphene outer film are removed, and an in-situ growing graphene thin film is directly obtained on the SiO2 substrate. The novel method for high-quality graphene in-situ deposition on insulation medium such as the SiO2 substrate is provided. Double layers or a few layers of graphene are directly prepared on the SiO2 substrate in a batch mode, and traditional complex procedures and processes for graphene growing and transferring are removed. The method for direct graphene in-situ growth on the insulation substrate has the advantages of being high in efficiency and low in cost, energy is saved, and accordingly the future practical application of graphene can be obviously and well improved.
Description
Technical field
The present invention relates to the method for the lower pair flame method of a kind of atmospheric environment growth in situ Graphene in dielectric base.
Background technology
Graphene has 3 kinds of forms conventionally: single-layer graphene, double-layer graphite alkene and few layer graphene, wherein less the layer graphene number of plies generally in 4 layers, surpasses 5 layers and just thinks block graphite.
Graphene is a kind of carbon atom plane layer that only has monatomic thickness, and carbon atom, by cellular lattice arrangement, forms hexagonal mesh material.It is considered to following promising electronic application candidate materials.The carrier mobility of Graphene can be up to 200,000cm
2v
-1s
-1, its thermal conductivity can reach approximately 5,000Wm
-1k
-1. its outstanding characteristic receives the very big concern of scientists.Conventionally, mechanically peel method, graphite oxidation method, liquid phase epitaxial method, chemical Vapor deposition process, silicon carbide thermal decomposition method, carbon nanotube incision and flame method are studied for individual layer or a few layer graphene of growing.
With the standby Graphene of mechanically peel legal system, have very high quality and outstanding electronic property, owing to being limited by graphite flake size, the size of the Graphene obtaining is always less than hundreds of micron.
Utilize silicon to distil from monocrystalline silicon carbide, can on Surface Insulation, directly generate Graphene.Yet because the fusing point of silicon is very high expensive with the growth apparatus needing, this method needs very high temperature and very high production cost.
The method of utilizing chemical vapour deposition (CVD) growing graphene on nickel or copper is being prepared tool potentiality aspect Graphene on a large scale.Yet, the high-quality Graphene of growing large-area and Graphene is transferred in dielectric base and still had difficulties and face the challenge from metal base.
Prior art is all by first prepare Graphene on transition metal, and then the Graphene of preparation is transferred in dielectric base, transfer process has been used complicated wet chemistry process, defect is introduced inevitable, this greatly reduces the electronic mobility of Graphene, and how avoiding shifting and reducing process complexity is the technical issues that need to address of the present invention.
In prior art, have and mention a kind of MBE method in the method for mica surface growing graphene, but the Graphene obtaining is second-rate.
Prior art is mentioned a kind of hBN of take and is prepared Graphene as substrate CVD method, although realized the method for growing graphene, the process of its realization is very complicated and difficult.
Also do not see at present the case of directly utilizing flame method direct growth in dielectric base to go out high-quality Graphene.
Chinese invention patent (application number: 201110206608.6, patent name: a kind of method of preparing graphene nanobelt in dielectric base), although this patent is direct growth Graphene in dielectric base, but be its step 1) in dielectric base, to prepare monoatomic layer step, and those skilled in the art all know and prepare monoatomic layer step this is a very complicated process, equipment and the condition of preparation are had to higher requirement.
Summary of the invention
Object of the present invention is exactly, in order to address the above problem, to provide the method for the lower pair flame method of a kind of atmospheric environment growth in situ Graphene in dielectric base, and it has efficient, energy-conservation and advantage cheaply.
To achieve these goals, the present invention adopts following technical scheme:
The method of the lower pair flame method of atmospheric environment growth in situ Graphene in dielectric base, nickel deposited film in dielectric base in advance, then under atmospheric environment, and then utilize carburizing/decarburization mechanism and the non-equilibrium surface segregation process of nickel film, utilize two flame method in dielectric base, to form graphene film; Upper and lower surfaces at nickel film all can grow graphene film, then nickel film and the outer field Graphene of nickel film are got rid of, thereby in dielectric base, are directly obtained the graphene film of growth in situ.
Described in advance in dielectric base the step of nickel deposited film be: the nickel film that evaporation thickness is 100nm～700nm in dielectric base.
The described nickel film that evaporation thickness is 100nm～700nm in dielectric base is used thermal evaporation.
The step that the two flame method of described employing form graphene film in dielectric base is:
Step (1): preprocessing process: the dielectric base after plated nickel film is put into first burner that can the produce cold flame setting-up time that burns;
Step (2): cementation process: the flame of the first burner is overlapped with the flame that can produce the second burner of thermal-flame, after flame overlaps, dielectric base enters the flame of the second burner under the state of the hypoxia protection of the flame of the first burner, the flame of the second burner is by the heating and continuous setting-up time of dielectric base, and carbon seed is diffused in whole nickel film;
Step (3): in the cementation process of step (2), the flame that can produce the first burner of cold flame keeps overlapping with the flame that can produce the second burner of thermal-flame;
Step (4): first turn off the flame of the second burner, after setting-up time, then turn off the flame of the first burner, need to adopt anaerobic environment in the process of turning off the first burner; Dielectric base in anaerobic environment is cooled to ambient temperature; In temperature-fall period, the solubleness of carbon in nickel film reduces, and the surface that carbon atom is just liquated out nickel from nickel film inside, forms respectively two Graphene retes in the upper and lower surfaces of nickel.
The step that nickel film and the outer field Graphene of nickel film are got rid of is:
Use the etchant solution of preparation that nickel film and the outer field graphene film of nickel film are eroded, just obtain being attached to the few layer graphene film of big area in dielectric base.
The setting-up time of described step (2) is 20 seconds.
The setting-up time of described step (4) is 50 seconds to 60 seconds.
The etchant solution of described preparation is CuSiO
4: H
2o:HCl=10g:50ml:50ml.
Described the first burner is the burner that spirit lamp, acetylene lamp, methyl alcohol lamp maybe can produce cold flame and chemistry of fuel composition carbon elements.
Described the second burner is the burner that alcohol blast burner, methyl alcohol blowtorch, acetylene burner, methane blowtorch maybe can produce thermal-flame and chemistry of fuel composition carbon elements.
Described dielectric base is SiO
2, Al
2o
3or other dielectric base.
The flame of the second burner is 950 ℃;
Beneficial effect of the present invention:
1 pair of flame method is the method for a quick and economic growing high-quality Graphene under normal pressure open environment.This method only needs tens seconds and a single step process just can be produced n (n is not more than 4 natural number) layer graphene.The present invention uses this method at SiO
2in/Si substrate, directly prepare in batches the graphene film of double-deck and few layer, saved the operation process of traditional method complexity.Because flame method has efficient, energy-conservation and feature cheaply, this obviously contributes to the practical application of following Graphene.
2 use flame method growing graphene, only need a single step process.Here, the present invention adopts the two flame method after improvement, under atmospheric environment, successfully at SiO
2upper direct in-situ has grown the Graphene of large-area high-quality.The method of two flame growing graphenes is not only easy to realize, and saves time and energy consumption, and the method can be prepared the graphene film of high quality big area size under open Atmospheric Condition.
3 the present invention direct in-situ in dielectric base has grown the Graphene of large-area high-quality, without transfer process.
Accompanying drawing explanation
Fig. 1 is at SiO
2in substrate, use the schematic diagram of flame method direct in-situ growing graphene;
Fig. 2 (a) is the Raman spectrogram that uses the Graphene that two flame method grow in different substrates.Topmost (in 25 micron thickness nickel foil substrates), middle (at SiO
2plated nickel film outside), bottom (at SiO
2on);
Fig. 2 (b) SiO
2on the optical microscopic image of Graphene;
Fig. 3 (a) is at SiO
2in substrate the continuous graphite alkene of growth in situ～40 μ m * 40 μ m optical microscope image;
The Raman image of the G peak intensity of Fig. 3 (b) 40 μ m * 40 μ m area Graphenes;
The Raman image of the 2D peak intensity of Fig. 3 (c) area Graphene;
Fig. 3 (d) Graphene is respectively at the Raman spectrum at A, B and C point place;
Fig. 4 (a) plates the nickel film of different thickness (25nm, 50nm, 100nm～700nm) at SiO
2the Raman spectrum of the Graphene of growing in substrate;
Fig. 4 (b) is at SiO
2the ratio IG/I2D value of the ratio ID/IG value of the D peak of the Graphene of growth in situ and G peak intensity and G peak and 2D peak intensity in substrate.
Embodiment
Below in conjunction with accompanying drawing and embodiment, the invention will be further described.
Fig. 1 has provided the process with two flame method growing graphenes.The flame of two differing tempss that produced by two combustion lamps provides different functions in the process of growth of Graphene.By the cotton of having soaked ethanol, be called as burner 1, alcohol blast burner is called as burner 2.In the process of whole growing graphene, the flame that burner 1 produces will surround Ni/SiO always
2/ Si substrate, to be used for protecting nickel film and Graphene not by high temperature oxidation, and as the carbon source of the needs of Graphene liquate.The flame that burner 2 produces is mainly as the heating source of nickel film high-temp. carburizing, and also for Graphene growth provides carbon.
Step (1): use thermal evaporation at SiO
2the nickel film of evaporation different thickness in/Si substrate (25nm, 50nm, 100nm～700nm).
Step (2): wrap Ni/SiO with the bale of cotton
2after/Si sample, they are immersed in ethanol liquid until cotton completely by alcohol immersion.
Step (3): Ni/SiO
2the internal flame that burner 1 is put into in/Si substrate burns the time of 20 seconds.
In this process, the carbon that derives from flame 1 is diffused into nickel film.
Step (4): Ni/SiO
2the flame envelope that burner 2 is put into in/Si substrate is heated to about 950 ℃, time remaining 50 seconds to 60 seconds.
This process is called as cementation process.In this process, carbon seed is diffused in whole nickel film.
Step (5): after cementation process, first turn off the flame of burner 2, then cover burner 1 with a cup immediately, the flame that makes burner 1 is extinguished because of anoxic.Ni/SiO in cup
2/ Si substrate is arrived ambient temperature by fast cooling.In temperature-fall period, the solubleness of carbon in nickel film will reduce, and the surface that carbon atom is just liquated out nickel from nickel film inside forms respectively two Graphene retes at two faces of nickel.
Step (6): the etchant solution (CuSiO that uses a kind of preparation
4: H
2o:HCl=10g:50ml:50ml) nickel film and outer field graphene film are eroded, just obtain being attached to SiO
2the few layer graphene film of the suprabasil big area of/Si.
At room temperature, using 100 times of object lens and wavelength is 514nm, and the laser source that power is 0.4mW adopts Raman spectrum to analyze the characteristic of few layer graphene film of growth.
Two flame method are based on non-equilibrium surperficial liquate process and carburizing/decarburization mechanism.This growth mechanism is similar to the mechanism of CVD method growing graphene.The solubleness of carbon in nickel film is relevant with the temperature of nickel film.In cementation process, carbon diffuses in nickel film, and in temperature-fall period, because the reduction of the solubility with temperature of carbon in nickel diminishes, has carbon from nickel film, to precipitate into nickel film surface.Here, at outside surface, nickel and the SiO of nickel
2between layer, all find that there is the graphene layer of generation.
3.1 at the epontic Graphene of different base
Fig. 2 (a) is the Raman spectrum of the Graphene on three different base surfaces that obtains in this experiment.The D peak of the graphite Raman spectrum of growing on nickel outside surface has high strength, and the Graphene of meaning growth is containing more defect, and G peak and 2D peak intensity ratio be about 2, this illustrates that this graphene film is few layer graphene.
Similarly, at another side (nickel and the SiO of nickel film
2between) Graphene quality also lower.The D peak of its Raman spectrum and 2D peak are weak and wide.These Raman traits show the quality that it is bad.This is SiO because the most carbon atom in nickel film is emanated
2surface, the sub-fraction nickel/SiO that emanates
2surface.The SiO measuring
2the D peak of the Raman spectrum of suprabasil Graphene very a little less than, G peak and 2D peak are very strong and narrow, this shows SiO
2on surface, the Graphene of growth has very high degree of crystallinity.
Fig. 2 (b) is at SiO
2the optical photograph of the Graphene of growth in situ on surface.
With etchant solution (CuSiO
4: H
2o:HCl=10g:50ml:50ml), after nickel erosion is fallen, use opticmicroscope at SiO
2many bending things are seen on surface.The shape of these bending things is corresponding with the size of initial nickel film.In heat-processed, nickel film meeting recrystallize, meanwhile, carbon atom dissolves in nickel film, and gathers at nickel crystal boundary.In temperature-fall period, the solubleness of carbon in nickel film starts to reduce, and carbon is just separated out from nickel film, with the shape of nickel crystal boundary at SiO
2surface deposition becomes graphene layer.
Several layer graphenes of growing in 3.2 silicon base
Fig. 3 (a) be one at SiO
2the optical microscope image of growth in situ Graphene sample in substrate.This Graphene be at evaporation the SiO of the thick nickel film of 300nm
2in substrate, grow.Select the square region of sample 40 μ m * 40 μ m to carry out point by point scanning Raman image, confirmed the existence of Graphene, and carried out quality characterization.The G peak of Graphene and the Raman image at 2D peak are respectively as shown in Fig. 3 (b) and Fig. 3 (c).
From Fig. 3 (b) and Fig. 3 (c), find out, 40 μ m * 40 μ m square region of Raman scanning imagery are red everywhere, and this shows that this region is covered by Graphene entirely.
What in Fig. 3 (d), three Raman scattering light spectral lines from the bottom up provided respectively is the Raman spectrum at A point, B point and C point place in Fig. 3 (b) and Fig. 3 (c).From Fig. 3 (d), can find out, the G peak of graphite Raman spectrum and the strength ratio IG/I2D at 2D peak are approximately 0.6 or 1.1, and this shows that the Graphene sample of growth is double-deck or few layer (in 4 layers) Graphene.This and the employing CVD method of reporting in the past, on nickel film or copper film, the result of growing graphene is similar.Generally speaking, on 40 μ m * 40 μ m areas, covering with continuous graphene layer is easily to realize. in the region of Raman spectroscopy scans, except important G band and 2D band, also found a D band that intensity is very weak.
The strength ratio ID/IG at D peak and G peak is approximately 0.1.High-quality graphite material there will not be D peak.This shows, the Graphene that present method obtains not as the quality of the Graphene that mechanically peel highly oriented pyrolytic graphite obtains good.
The impact of nickel film thickness on Graphene in 3.3 silicon base
Fig. 4 (a) is to adopting the Raman spectrum of Graphene of the nickel film growth of different thickness to contrast, and result shows, nickel film thickness is 25nm, 50nm, and between from 100nm to 700nm, Graphene can grow out.G and the 2D peak of Raman spectrum of Graphene of nickel film growth that with thickness is 25nm and 50nm is all very small and weak, and the Graphene of growth second-rate is described when nickel film thickness is 25nm and 50nm.That is that nickel film can evaporate or recrystallize because in heat-processed, when nickel film thickness is thinner, causes forming the white space without nickel.When nickel film thickness is increased to over 100nm, the Raman spectrum of Graphene all has very strong 2D peak.This explanation, the thickness of nickel film is limited to the growth effect of Graphene.
Fig. 4 (b) has shown that ID/IG and IG/I2D ratio are with the changing conditions of nickel film thickness.By Fig. 4 (b), found out, the size of the G peak of the Graphene of growth and the intensity rate IG/I2D at 2D peak is between 0.8～1.8, and this shows that the Graphene of growth comprises double-deck and few layer graphene.
Although above-mentioned, by reference to the accompanying drawings the specific embodiment of the present invention is described; but be not limiting the scope of the invention; one of ordinary skill in the art should be understood that; on the basis of technical scheme of the present invention, those skilled in the art do not need to pay various modifications that creative work can make or distortion still in protection scope of the present invention.
Claims (10)
1. the method for the lower pair flame method of atmospheric environment growth in situ Graphene in dielectric base, it is characterized in that, nickel deposited film in dielectric base in advance, then under atmospheric environment, and then utilize carburizing/decarburization mechanism and the non-equilibrium surface segregation process of nickel film, utilize two flame method in dielectric base, to form graphene film; Upper and lower surfaces at nickel film all can grow graphene film, then nickel film and the outer field Graphene of nickel film are got rid of, thereby in dielectric base, are directly obtained the graphene film of growth in situ.
2. the method for the lower pair flame method of atmospheric environment as claimed in claim 1 growth in situ Graphene in dielectric base, is characterized in that, described in advance in dielectric base the step of nickel deposited film be: the nickel film that evaporation thickness is 100nm～700nm in dielectric base.
3. the method for the lower pair flame method of atmospheric environment as claimed in claim 2 growth in situ Graphene in dielectric base, is characterized in that, the described nickel film that evaporation thickness is 100nm～700nm in dielectric base is used thermal evaporation.
4. the method for the lower pair flame method of atmospheric environment as claimed in claim 1 growth in situ Graphene in dielectric base, is characterized in that, the step that the two flame method of described employing form graphene film in dielectric base is:
Step (1): preprocessing process: the dielectric base after plated nickel film is put into first burner that can the produce cold flame setting-up time that burns;
Step (2): cementation process: the flame of the first burner is overlapped with the flame that can produce the second burner of thermal-flame, after flame overlaps, dielectric base enters the flame of the second burner under the state of the hypoxia protection of the flame of the first burner, the flame of the second burner is by the heating and continuous setting-up time of dielectric base, and carbon seed is diffused in whole nickel film;
Step (3): in the cementation process of step (2), the flame that can produce the first burner of cold flame keeps overlapping with the flame that can produce the second burner of thermal-flame;
Step (4): first turn off the flame of the second burner, after setting-up time, then turn off the flame of the first burner, need to adopt anaerobic environment in the process of turning off the first burner; Dielectric base in anaerobic environment is cooled to ambient temperature; In temperature-fall period, the solubleness of carbon in nickel film reduces, and the surface that carbon atom is just liquated out nickel from nickel film inside, forms respectively two Graphene retes in the upper and lower surfaces of nickel.
5. the method for the lower pair flame method of atmospheric environment as claimed in claim 1 growth in situ Graphene in dielectric base, is characterized in that, the step that nickel film and the outer field Graphene of nickel film are got rid of is:
Use the etchant solution of preparation that nickel film and the outer field graphene film of nickel film are eroded, just obtain being attached to the few layer graphene film of big area in dielectric base.
6. the method for the lower pair flame method of atmospheric environment as claimed in claim 4 growth in situ Graphene in dielectric base, is characterized in that, the setting-up time of described step (2) is 20 seconds; The flame of described the second burner is 950 ℃.
7. the method for the lower pair flame method of atmospheric environment as claimed in claim 4 growth in situ Graphene in dielectric base, is characterized in that, the setting-up time of described step (4) is 50 seconds to 60 seconds.
8. the method for the lower pair flame method of atmospheric environment as claimed in claim 5 growth in situ Graphene in dielectric base, is characterized in that, the etchant solution of described preparation is CuSiO
4: H
2o:HCl=10g:50ml:50ml.
9. the method for the lower pair flame method of atmospheric environment as claimed in claim 4 growth in situ Graphene in dielectric base, it is characterized in that, described the first burner is the burner that spirit lamp, acetylene lamp, methyl alcohol lamp maybe can produce cold flame and chemistry of fuel composition carbon elements.
10. the method for the lower pair flame method of atmospheric environment as claimed in claim 4 growth in situ Graphene in dielectric base, it is characterized in that, described the second burner is the burner that alcohol blast burner, methyl alcohol blowtorch, acetylene burner, methane blowtorch maybe can produce thermal-flame and chemistry of fuel composition carbon elements.
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|---|---|---|---|---|
| CN110132935A (en) * | 2019-05-20 | 2019-08-16 | 大连理工大学 | A kind of preparation method enhancing surface-enhanced raman scattering substrate |
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| KR20120020250A (en) * | 2010-08-29 | 2012-03-08 | 이장훈 | Apparatus and method for forming graphene-ball by spray pyrolysis |
| CN103101908A (en) * | 2013-01-24 | 2013-05-15 | 东南大学 | Method for preparing graphene film |
| CN103213970A (en) * | 2012-01-18 | 2013-07-24 | 中国科学院上海硅酸盐研究所 | Method for preparing graphene powder and graphene transparent conductive film by oxyhydrogen flame method |
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| KR20120020250A (en) * | 2010-08-29 | 2012-03-08 | 이장훈 | Apparatus and method for forming graphene-ball by spray pyrolysis |
| CN102070141A (en) * | 2011-03-10 | 2011-05-25 | 武汉大学 | Method for preparing graphene |
| CN103213970A (en) * | 2012-01-18 | 2013-07-24 | 中国科学院上海硅酸盐研究所 | Method for preparing graphene powder and graphene transparent conductive film by oxyhydrogen flame method |
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| CN110132935B (en) * | 2019-05-20 | 2021-05-07 | 大连理工大学 | Preparation method of enhanced surface Raman scattering substrate |
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