CN103523770A - Preparation method of graphene - Google Patents
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Abstract
The invention provides a preparation method of graphene. The preparation method of the graphene at least comprises the following steps: firstly, providing a SiC substrate; then, injecting Ge in the SiC substrate by adopting an ion injecting technology; and finally, carrying out annealing treatment onto the formed structure, wherein Si and C in the SiC are forced to break very easily in an annealing process of the injected Ge, the bond-broken Si and the injected Ge form SiGe, and the bond-broken C is recombined on the surface of the SiGe to form graphene. According to the invention, the graphene can be prepared by only needing normal pressure or low pressure as well as low temperature, requirements to a preparation apparatus are low; moreover, energy resources are saved and cost is reduced, and therefore, the preparation method is suitable for industrial production.
Description
Technical field
The present invention relates to semiconductor applications, particularly relate to a kind of preparation method of Graphene.
Background technology
Two scientists of 2004 Nian， Univ Manchester UKs use the method that micromechanics is peeled off to find Graphene, and have obtained Nobel Prize in physics in 2010.Graphene, the monoatomic layer of graphite, is that carbon atom is by the two-dirnentional structure of honeycomb arrangement.After Graphene is found, because its excellent performance and huge application prospect have caused the research boom in the fields such as physics and Materials science.Graphene is also very extensive in the application in optical, electrical field, comprises lithium ion battery, solar cell, gas detector and some devices etc. based on Graphene.Graphene is all on the basis of the graphene film controlled based on big area, the number of plies in the application in optical, electrical field.But controlledly synthesis has the grapheme material problem of specific morphology not still to be resolved.Based on this, the research of Graphene still rests on fundamental research field, and the large-scale application of distance still has a segment distance.
The method of preparing at present Graphene mainly contains that micromechanics is peeled off, chemical vapor deposition and graphite oxide reduction method, SiC subliming method.Micromechanics stripping method can be prepared high-quality Graphene, but the Graphene area that at present prepared by this method is less than 1mm * 1mm, can only be for Basic Experiment Study.Although CVD (Chemical Vapor Deposition) method can be prepared large-area graphene film, but the controllability of the graphene film thickness that this method obtains is poor, if CVD legal system on Cu is for Graphene (Xuesong Li, Weiwei Cai, Jinho An, Ruoff et al, Large-Area Synthesis of High-Quality and Uniform Graphene Films on Copper Foils, Science, 2009, 324, 1312) be a kind of self-limit growth mechanism of surface catalysis, when the first layer Graphene covers Cu surface 95%, the catalytic effect on Cu surface will weaken even inefficacy, so the Graphene of preparing on Cu is individual layer and a small amount of bilayer, on Ni, CVD legal system is for Graphene (Qingkai Yu, Jie Lian, Sujitra Siriponglert, et al, Graphene segregated on Ni surfaces and transferred to insulators, APPLIED PHYSICS LETTERS, 2008,93,113103) be that a kind of dissolving precipitation mechanism is prepared Graphene, the stage of Graphene growth occurs in temperature-fall period, and the number of plies is subject to the impact of rate of temperature fall, so the Graphene of preparation is multilayer film in uneven thickness.And graphite oxide reduction method can a large amount of Graphene sample of chemical preparation, meets to a certain extent industrial application requirement, yet due to the introducing of oxygenant, destroyed the conjugated structure of Graphene.Although chemical reduction and high-temperature heat treatment can be recovered the conjugated structure of Graphene to a certain extent, yet the intrinsic electric property of Graphene reduces greatly.
It is one of preparation method of current comparatively main flow that SiC subliming method is prepared Graphene, can obtain the controlled graphene film of large-area high-quality and thickness, but conventional SiC subliming method need to be at high temperature, preparation (T=1550 ℃ under ultrahigh vacuum(HHV), P=1bar), instrument is had to very high requirement, cost increases, stoped its suitability for industrialized production (Konstantin V.Emtsev et al.Towards wafer-size graphene layers by atmospheric pressure graphitization of silicon carbide.Nature Materials, 8, 203-207 (2009)).
Shortcoming in view of above-mentioned graphene preparation method, the present invention proposes and a kind ofly can under normal pressure, lesser temps, prepare the method for Graphene, can obtain the controlled graphene film of large-area high-quality and thickness, save energy, reduce cost, be applicable to suitability for industrialized production.
Summary of the invention
The shortcoming of prior art in view of the above, the object of the present invention is to provide a kind of preparation method of Graphene, for solving prior art SiC subliming method, prepares Graphene and need under high temperature, ultrahigh vacuum(HHV), cause being difficult for the problem of suitability for industrialized production.
For achieving the above object and other relevant objects, the invention provides a kind of preparation method of Graphene, described graphene preparation method at least comprises:
1) provide a SiC substrate;
2) adopt ion implantation technique to inject Ge in described SiC substrate;
3) to step 2) structure that forms carries out anneal, and the Ge of injection can force very easily scission of link of the Si of described SiC and C in annealing process, and the Si after scission of link and the Ge of injection form SiGe, and the C after scission of link forms Graphene in described SiGe surface restructuring.
Preferably, described step 2) in, the Implantation Energy scope of Ge is 5～30keV, and the dosage range of injection is 1E15～1E20atoms/cm
2.
Preferably, in described step 3), the temperature range of anneal is 800～1000 ℃, and the time range of anneal is 10～100min, and annealing adopts Ar gas as shielding gas.
Preferably, the flow range of described Ar gas is 1～1000sccm.
Preferably, under normal pressure or low pressure, carry out anneal; The scope of described low pressure is 1E-1～1E-5mbar.
Preferably, the thickness range of formation SiGe is 1-3nm.
Preferably, the Graphene forming in described step 3) is individual layer, bilayer or multilayer.
Preferably, the thickness range of formation Graphene is 0.34～1nm.
Preferably, in described step 1), also comprise the step of described SiC substrate being carried out to surface cleaning.
Preferably, the crystal formation of described SiC substrate adopts 4H-SiC, 6H-SiC or 3C-SiC.
As mentioned above, the preparation method of Graphene of the present invention, comprises step: first, provide a SiC substrate; Then, adopt ion implantation technique to inject Ge in described SiC substrate; Finally, the structure of above-mentioned formation is carried out anneal, and the Ge of injection can force very easily scission of link of the Si of described SiC and C in annealing process, and the Si after scission of link and the Ge of injection form SiGe, and the C after scission of link forms Graphene in described SiGe surface restructuring.The present invention only needs normal pressure and low temperature just can prepare Graphene, lower to the requirement of apparatus for preparation, and save energy, reduces cost, is applicable to suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is the preparation method's of Graphene of the present invention process flow sheet.
The structural representation of the SiC substrate providing in the preparation method that Fig. 2 is Graphene of the present invention.
Fig. 3 adopts ion implantation technique in SiC substrate, to inject the structural representation of Ge in the preparation method of Graphene of the present invention.
Fig. 4 is the SiGe that forms after annealing in the preparation method of Graphene of the present invention and the structural representation of Graphene.
The Raman comparison diagram of SiC in the preparation method that Fig. 5 is Graphene of the present invention after the original SiC providing and injection Ge annealing.
Element numbers explanation
S1～S3 step
1 Si atom
2 C atoms
3 Ge atoms
4 SiGe
5 Graphenes
Embodiment
Below, by specific specific examples explanation embodiments of the present invention, those skilled in the art can understand other advantages of the present invention and effect easily by the disclosed content of this specification sheets.The present invention can also be implemented or be applied by other different embodiment, and the every details in this specification sheets also can be based on different viewpoints and application, carries out various modifications or change not deviating under spirit of the present invention.
Refer to accompanying drawing 1 to Fig. 5.It should be noted that, the diagram providing in the present embodiment only illustrates basic conception of the present invention in a schematic way, satisfy and only show with assembly relevant in the present invention in graphic but not component count, shape and size drafting while implementing according to reality, during its actual enforcement, kenel, quantity and the ratio of each assembly can be a kind of random change, and its assembly layout kenel also may be more complicated.
The invention provides a kind of preparation method of Graphene, as shown in Figure 1, the preparation method of described Graphene at least comprises the following steps:
First perform step S1, as shown in Figure 2, provide a SiC substrate, described SiC substrate is comprised of some Si atoms 1 and C atom 2.
Preferably, before carrying out subsequent technique, described SiC substrate is carried out to surface cleaning.Be specially: SiC substrate is carried out to sonic oscillation 10 minutes to remove its surperficial organism such as grease with acetone, ethanol and deionized water respectively according to sequencing, afterwards SiC substrate is dried up.Wherein, the crystal formation of described SiC substrate can adopt 4H-SiC, 6H-SiC or 3C-SiC etc.In the present embodiment, described SiC substrate adopts 6H-SiC.
Then perform step S2, as shown in Figure 3, adopt ion implantation technique to inject Ge atom 3 in described SiC substrate.
Wherein, the ion implantation Implantation Energy that adopts can be within the scope of 5～30keV, preferably, ion implantation Implantation Energy is 5～20keV.Particularly, in the present embodiment, the energy that adopts ion implantation technique to inject Ge is 10keV.The energy injecting due to Ge is low, and therefore, Ge is only infused in the top layer of described SiC substrate, injects the degree of depth and is about 1～10nm.The implantation dosage scope of described Ge can be at 1E15～1E20atoms/cm
2interior selection, preferably, the implantation dosage of described Ge is 1E15～1E16atoms/cm
2.Particularly, in the present embodiment, the implantation dosage of described Ge is 1E15atoms/cm
2.As can be seen from Figure 3, the Ge atom 3 of injection is embedded between Si atom 1 and C atom 2.
Finally perform step S3, as shown in Figure 4, the structure that step S2 is formed is carried out anneal, the Ge atom 3 injecting can force very easily scission of link of the Si atom 1 of described SiC and C atom 2 in annealing process, Si after scission of link and the Ge of injection form SiGe4, and the C after scission of link forms Graphene 5 in described SiGe4 surface restructuring.
The temperature of carrying out anneal can complete within the scope of 800～1000 ℃, and annealing time is 10～100 minutes.In the present embodiment, the temperature of carrying out anneal is 800 ℃, and the set of time of processing is 10 minutes.
Preferably; while carrying out anneal; can in annealing device, pass into Ar gas as protective gas; be used for preventing that the Graphene of follow-up generation is oxidized; but in the present invention, be not limited to Ar gas as shielding gas, also can adopt other rare gas element or a kind of and combination in inactive gas.In the present embodiment, adopt Ar gas as shielding gas.The flow range of the Ar gas passing into is 1～1000sccm(per minute standard milliliter), preferably, Ar airshed is 200～800sccm.In the present embodiment, the shielding gas of the Ar gas that passes into 500sccm during as annealing.
Anneal can be carried out at atmospheric or low pressure, and the present embodiment is preferably and under low pressure carries out anneal and prepare Graphene.Concrete, the air pressure range under low pressure is 1E-1～1E-5mbar.In the present embodiment, in the low pressure environment that is 1E-2mbar at air pressure, carry out anneal.
In annealing process, the Ge atom 3 of injection can force very easily scission of link of Si atom 1 and C atom 2 under annealing process, and the thickness range of the SiGe4 of formation is 1～3nm.In the present embodiment, the thickness of the SiGe4 of formation is 2nm.After Si atom 1 and 2 bond ruptures of C atom, 2, remaining C atom is separated out and is reassembled into core and grows up and form Graphene 5 on SiGe4 surface.The thickness range of the Graphene 5 forming is 0.34～1nm.In the present embodiment, the thickness of the Graphene of formation is 0.34nm.The dosage injecting according to Ge, the Graphene 5 of formation can be individual layer, bilayer or multilayer.In the present embodiment, the implantation dosage of Ge is 1E15atoms/cm
2, the Graphene 5 of formation is individual layer.
Compare traditional SiC distillation and prepare the method for Graphene, adopt preparation temperature in graphene preparation method provided by the invention obviously to reduce (800～1000 ℃), its reason is: on the one hand may be relevant with ion implantation technology, implantation membership causes SiC lattice damage, contributes to the atomic bond of Si atom 1 in SiC substrate and C atom 2 to disconnect; On the other hand, after ion implantation Ge, Ge very easily becomes key to form SiGe4 in this temperature range with Si atom, and this has also impelled the disconnection of Si and C atomic bond indirectly.
Adopt Raman spectroscopy to characterize process results, to confirm having prepared Graphene in SiC substrate.As example, refer to Fig. 5, Raman figure (curve below) and Ge that the original SiC substrate providing in the preparation method of Graphene of the present invention is provided inject the Raman figure (curve above) after SiC annealing.Concrete technology parameter is: ion implantation energy is that 10keV, Ge implantation dosage are 1E15atoms/cm
2, annealing temperature is that 900 ℃, annealing time are 30min, and air pressure is 1E-3mbar, and the flow of Ar gas is 200sccm.As can be seen from Figure 5, in the Raman spectrum of SiC substrate, do not have the characteristic peak of Graphene, and SiC injects Ge and carries out after anneal, has occurred the characteristic feature peak of Graphene: G peak and 2D peak in Raman spectrum through top layer.Wherein, G peak is in 1570cm
-1near, 2D peak is in 2700cm
-1near, this shows, adopts graphene preparation method of the present invention successfully to prepare Graphene, and it is low compared with the technological temperature of traditional technology to prepare the technological temperature of Graphene.It should be noted that, in the present embodiment, only shown one group of Graphene prepared by processing parameter, in fact, change the position that the processing parameter prepare Graphene can't change G and 2D characteristic peak in Raman spectrum, and be only the change of relative intensity, in the present invention, show no longer one by one the Raman spectrum utilize Graphene prepared by other processing parameters.
In sum, the invention provides a kind of preparation method of Graphene, the preparation method of this Graphene at least comprises: first, provide a SiC substrate; Then, adopt ion implantation technique to inject Ge in described SiC substrate; Finally, the structure of above-mentioned formation is carried out anneal, and the Ge of injection can force very easily scission of link of the Si of described SiC and C in annealing process, and the Si after scission of link and the Ge of injection form SiGe, and the C after scission of link forms Graphene in described SiGe surface restructuring.The present invention only needs low pressure and low temperature just can prepare Graphene, lower to the requirement of apparatus for preparation, and save energy, reduces cost, is applicable to suitability for industrialized production.
So the present invention has effectively overcome various shortcoming of the prior art and tool high industrial utilization.
Above-described embodiment is illustrative principle of the present invention and effect thereof only, but not for limiting the present invention.Any person skilled in the art scholar all can, under spirit of the present invention and category, modify or change above-described embodiment.Therefore, such as in affiliated technical field, have and conventionally know that the knowledgeable, not departing from all equivalence modifications that complete under disclosed spirit and technological thought or changing, must be contained by claim of the present invention.
Claims (10)
1. a graphene preparation method, is characterized in that, described graphene preparation method at least comprises:
1) provide a SiC substrate;
2) adopt ion implantation technique to inject Ge in described SiC substrate;
3) to step 2) structure that forms carries out anneal, and the Ge of injection can force very easily scission of link of the Si of described SiC and C in annealing process, and the Si after scission of link and the Ge of injection form SiGe, and the C after scission of link forms Graphene in described SiGe surface restructuring.
2. graphene preparation method according to claim 1, is characterized in that: described step 2), the Implantation Energy scope of Ge is 5～30keV, and the dosage range of injection is 1E15～1E20atoms/cm
2.
3. graphene preparation method according to claim 1, is characterized in that: in described step 3), the temperature range of anneal is 800～1000 ℃, and the time range of anneal is 10～100min, adopts Ar gas as shielding gas during anneal.
4. graphene preparation method according to claim 3, is characterized in that: the flow range of described Ar gas is 1～1000sccm.
5. graphene preparation method according to claim 1, is characterized in that: under normal pressure or low pressure, carry out anneal; Air pressure range under described low pressure is 1E-1～1E-5mbar.
6. graphene preparation method according to claim 1, is characterized in that: the thickness range that forms SiGe in described step 3) is 1～3nm.
7. graphene preparation method according to claim 1, is characterized in that: the Graphene forming in described step 3) is individual layer, bilayer or multilayer.
8. graphene preparation method according to claim 7, is characterized in that: the thickness range that forms Graphene is 0.34～1nm.
9. graphene preparation method according to claim 1, is characterized in that: in described step 1), also comprise the step of described SiC substrate being carried out to surface cleaning.
10. graphene preparation method according to claim 9, is characterized in that: the crystal formation of described SiC substrate adopts 4H-SiC, 6H-SiC or 3C-SiC.
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| CN107653446A (en) * | 2016-07-26 | 2018-02-02 | 中国科学院上海微系统与信息技术研究所 | A kind of graphene growth method for improving graphene nucleation density |
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| CN109879275A (en) * | 2019-01-30 | 2019-06-14 | 宁波大学 | A kind of method that the concentration of combination germanium prepares graphene with ion implantation technique |
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