CN105483824A - Method for preparing monocrystal double-layer graphene - Google Patents
Method for preparing monocrystal double-layer graphene Download PDFInfo
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- CN105483824A CN105483824A CN201610016623.7A CN201610016623A CN105483824A CN 105483824 A CN105483824 A CN 105483824A CN 201610016623 A CN201610016623 A CN 201610016623A CN 105483824 A CN105483824 A CN 105483824A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
Abstract
The invention discloses a method for preparing monocrystal double-layer graphene. The method comprises the following steps that 1, a copper catalyst is put into a reactor, non-oxidative gas is introduced into the reactor to enable the reactor to be full of the non-oxidative gas, and monocrystal copper or polycrystalline copper or a copper film is adopted as the copper catalyst; 2, the copper catalyst is heated to the target temperature, and then the temperature is kept constant for 30-120 minutes, wherein the target temperature ranges from 1000 DEG C to 1070 DEG C; 3, the copper catalyst is cooled to enable the temperature to reach 900 DEG C-500 DEG C or be kept constant, in the cooling or constant temperature process, the non-oxidative gas carrying a carbon source is introduced into the reactor, and then the monocrystal double-layer graphene can be obtained on the surface of the copper catalyst. Accordingly, the large-size monocrystal double-layer graphene is prepared on the copper catalyst through an isothermal or non-isothermal atmospheric pressure chemical vapor deposition method, and the method is convenient to operate, simple and practicable and can be applied to high-grade electronic devices and integrated circuits.
Description
Technical field
The present invention relates to a kind of method preparing monocrystalline bilayer graphene, belong to technical field of graphene.
Background technology
At present, Graphene is as a kind of ultra-thin monatomic two-dimensional material, and the physical structure of its uniqueness, imparts the performances such as the electricity of its excellence, optics, mechanics, makes it obtain pursuing of every field scientific research personnel.The preparation of initial Graphene adopts micromechanics to peel off highly oriented pyrolytic graphite method, obtains up to 200,000V
-1s
-1the high-quality graphene of mobility.Current, adopt chemical gas-phase method to carry out the preparation of Graphene on transition metal substrate Ni or Cu surface, can obtain the individual layer of square meter level, bilayer or multi-layer graphene.
Zero band gap dispersion relation of single-layer graphene uniqueness, limits its application on logical switch and storer.In order to open Graphene band gap, people have employed various way, such as: graphene film is cut into graphene nanobelt or graphene mesh, carry out chemical doping or physical adsorption, adopt a simple stress stretching Graphene etc.Although these methods can open the band gap of Graphene, but the but havoc crystalline network of Graphene, lose the electrical properties of Graphene excellence, the particularly carrier mobility of Graphene inevitably deep fades, therefore, need to find a kind of new method to open the band gap of Graphene.Now, bilayer graphene enters the sight line of people.Bilayer graphene has the parabola shaped energy band structure of unique class, band gap can be opened like a cork under the effect of extra electric field, it is made to receive increasing concern, and obtained checking by people from theoretical modeling and experimental implementation aspect, namely by adding a highfield in the vertical direction of bilayer graphene, ~ the band gap of 250meV can just be opened.Therefore, the bilayer graphene preparing large-area high-quality becomes a large focus of current research.
Polycrystalline graphite alkene film prepared by general chemical Vapor deposition process, its monocrystalline size is approximately several microns or tens microns.The high-density crystal boundary of these polycrystalline graphite alkene films causes the characteristic electron of Graphene unstable.Although about research says that polycrystalline graphite alkene prepared by this chemical Vapor deposition process has the comparable high mobility intending to peel off Graphene, the overall transport property of polycrystal film Graphene is still subject to the impact of grain boundaries defect.Therefore, how preparing large-size monocrystal graphene is based on graphene electronic device and the integrated significant challenge of photoelectric device.
Summary of the invention
Technical problem to be solved by this invention is: overcome the deficiencies in the prior art, provides a kind of method preparing monocrystalline bilayer graphene, and the present invention, without the need to using complicated high-vacuum apparatus, can prepare monocrystalline bilayer graphene under mild conditions.
In order to solve the problems of the technologies described above, technical scheme of the present invention is a kind of method preparing monocrystalline bilayer graphene, comprises the following steps:
A) copper catalyst is put into reactor, and pass into non-oxidizing gas in reactor, make non-oxidizing gas be full of reactor, described copper catalyst is single crystal Cu or polycrystalline copper or Copper thin film;
B) copper catalyst is heated to target temperature, then keep homo(io)thermism 30-120 minute, the temperature range of described target temperature is: 1000 DEG C ~ 1070 DEG C;
C) continue to keep homo(io)thermism, the non-oxidizing gas carrying carbon source is passed in reactor, monocrystalline bilayer graphene can be obtained on copper catalyst surface.
The invention also discloses the method that another kind prepares monocrystalline bilayer graphene, comprise the following steps:
A) copper catalyst is put into reactor, and pass into non-oxidizing gas in reactor, make non-oxidizing gas be full of reactor, described copper catalyst is single crystal Cu or polycrystalline copper or Copper thin film;
B) copper catalyst is heated to target temperature, then keep homo(io)thermism 30-120 minute, the temperature range of described target temperature is: 1000 DEG C ~ 1070 DEG C;
C) then carrying out cooling to copper catalyst makes it reach 900 DEG C ~ 500 DEG C, in above-mentioned temperature-fall period, passes in reactor by the non-oxidizing gas carrying carbon source, can obtain monocrystalline bilayer graphene on copper catalyst surface.
Further, step c) described in carbon source be methane and/or acetylene and/or polystyrene and/or coronene.
Further, in step c) in, for gaseous carbon sources, gaseous carbon sources and non-oxidizing gas pass in reactor simultaneously.
Further provide a kind of method introducing solid carbon source, in step c) in, for solid carbon source, solid carbon source is placed on one end that reactor passes into air-flow, and with heating zone, position, solid carbon source place is heated, the temperature range of heating is: 200 DEG C-400 DEG C.
Further in order to obtain pure Graphene, in step c) after, also comprise steps d), first PMMA or PDMS is spin-coated on the substrate surface that growth has Graphene, and heats on warm table, then put into iron(ic) chloride or copper sulfate or ammonium persulfate solution and corrode 1-24 hour removing copper, clean with deionized water, dilute hydrochloric acid, Virahol successively afterwards, dry, transfer in target substrate, finally use hot acetone removing PMMA or PDMS layer.
After have employed technique scheme, the present invention utilizes isothermal or non-isothermal aumospheric pressure cvd method on copper catalyst, prepare large size single crystal bilayer graphene, and present method is easy to operate, simple, can be used for high-end electronic device and unicircuit; In addition, there is compared with the monocrystalline bilayer graphene that prepared by the monocrystalline bilayer graphene prepared of non-isothermal method of the present invention and isothermal method the advantage of larger size and less defect.
Accompanying drawing explanation
The schematic diagram of the reactor that Fig. 1 is carbon source of the present invention when being gaseous carbon sources;
The schematic diagram of the reactor that Fig. 2 is carbon source of the present invention when being solid carbon source;
Fig. 3 is that the scanning electronic microscope of monocrystalline bilayer graphene prepared by embodiment one is shone;
Fig. 4 is the electron scanning micrograph of monocrystalline bilayer graphene prepared by embodiment two;
Fig. 5 is the optical microscope photograph of monocrystalline bilayer graphene prepared by embodiment three;
Fig. 6 is the electron scanning micrograph of monocrystalline bilayer graphene prepared by embodiment three;
Fig. 7 be embodiment three prepare monocrystalline bilayer graphene on choose Raman spectrum corresponding to difference;
Fig. 8 is the transmission electron microscope photo of monocrystalline bilayer graphene marginal layer structure prepared by embodiment three;
Fig. 9 is the selected area electron diffraction photo of monocrystalline in Fig. 8;
The selected area electron diffraction intensity of Figure 10 corresponding to Fig. 9;
Figure 11 is the electron scanning micrograph of monocrystalline bilayer graphene prepared by embodiment four;
Figure 12 is the electron scanning micrograph of monocrystalline bilayer graphene prepared by embodiment five
In figure, 1, No. 1 inlet pipe, 2, No. 2 inlet pipe, 3, carbon source, 4, copper catalyst, 5, reactor.
Embodiment
In order to make content of the present invention more easily be clearly understood, below according to specific embodiment also by reference to the accompanying drawings, the present invention is further detailed explanation.
Embodiment one:
As shown in Figure 1, carbon source is methane, and can certainly be acetylene, copper catalyst be monocrystalline Copper Foil, and reactor is silica tube, and No. 1 pipe is tunger tube, and No. 2 pipes are hydrogen pipe, and No. 3 pipes are methane tracheae.
Prepare a method for monocrystalline bilayer graphene, comprise the following steps:
A) monocrystalline Copper Foil is placed in the middle part of clean silica tube, silica tube is vacuumized, then passes into argon gas, vacuumize, pass into hydrogen, again vacuumize, repeat three times, to remove the air in silica tube and gas circuit, then in silica tube, pass into 500-1000sccm argon hydrogen mixture;
B) to the heating of monocrystalline Copper Foil, make the central zone temperature of silica tube reach 1000 DEG C, then keep homo(io)thermism 60 minutes, anneal is carried out to monocrystalline copper foil surface;
C) continue maintenance 1000 DEG C of homo(io)thermism, pass into methane, and jointly pass in silica tube in argon hydrogen mixture, reaction starts to carry out, and carbon generates monocrystalline bilayer graphene at monocrystalline Copper Foil surface deposition.
After reaction carries out 100 minutes, stop passing into methane, raise bell simultaneously, close electric furnace, continue to pass into argon hydrogen mixture until be cooled to room temperature, can certainly furnace cooling slowly.
As shown in Figure 3, as can be seen from the figure hexagonal single crystal structure, is illustrated as Graphene.
Embodiment two:
As shown in Figure 1, carbon source is methane, and can certainly be acetylene, copper catalyst be monocrystalline Copper Foil, and reactor is silica tube, and No. 1 pipe is tunger tube, and No. 2 pipes are hydrogen pipe, and No. 3 pipes are methane tracheae.
Prepare a method for monocrystalline bilayer graphene, comprise the following steps:
A) monocrystalline Copper Foil is placed in the middle part of clean silica tube, silica tube is vacuumized, then passes into argon gas, vacuumize, pass into hydrogen, again vacuumize, repeat three times, to remove the air in silica tube and gas circuit, then in silica tube, pass into 500-1000sccm argon hydrogen mixture;
B) to the heating of monocrystalline Copper Foil, make the central zone temperature of silica tube reach 1000 DEG C, then keep homo(io)thermism 90 minutes, anneal is carried out to monocrystalline copper foil surface;
C) start slow cooling to 500 DEG C to the central zone of silica tube, in temperature-fall period, in argon hydrogen mixture, pass into methane, and jointly pass in silica tube, reaction starts to carry out, and carbon generates Graphene at monocrystalline Copper Foil surface deposition.
After reaction carries out 100 minutes, stop passing into methane, raise bell simultaneously, close electric furnace, continue to pass into argon hydrogen mixture until be cooled to room temperature, can certainly furnace cooling slowly.
As shown in Figure 4, as can be seen from the figure hexagonal single crystal structure, is illustrated as Graphene.
Embodiment three:
As shown in Figure 1, carbon source is methane, and copper catalyst is polycrystalline Copper Foil, and reactor is silica tube, and No. 1 pipe is tunger tube, and No. 2 pipes are hydrogen pipe, and No. 3 pipes are methane tracheae.
Prepare a method for monocrystalline bilayer graphene, comprise the following steps:
A) polycrystalline Copper Foil is dried up with nitrogen with after deionized water, ethanol, acetone and Virahol ultrasonic cleaning successively, put into the middle part of the silica tube of chemical gas-phase deposition system subsequently, silica tube is vacuumized, and argon gas and hydrogen is passed in silica tube, argon hydrogen mixture is made to be full of reactor, repeatedly vacuumize for three times and inner air tube is removed completely, and then pass into argon hydrogen mixture in silica tube;
B) polycrystalline Copper Foil is heated, the central zone temperature of silica tube is made to reach 1070 DEG C, when the temperature of the central zone of silica tube reaches 1070 DEG C, pass into 400sccm argon gas in silica tube while, pass into 50sccm hydrogen as reducing gas, and keep temperature now 30 minutes, anneal is carried out to polycrystalline copper foil surface;
C) then carrying out cooling to polycrystalline Copper Foil makes it reach 900 DEG C, in pipe, the temperature of central zone is reduced to the process of cooling of 900 DEG C from 1070 DEG C, in argon hydrogen mixture, pass into methane, and jointly pass into in silica tube, monocrystalline bilayer graphene can be obtained at polycrystalline copper foil surface.
In step c) after, also comprise steps d), first PMMA is spin-coated on the surface that growth has the polycrystalline Copper Foil of Graphene, and heats on warm table, then put into ferric chloride Solution corrosion 24 hours removing copper, also can be copper-bath, can also be ammonium persulfate solution, clean with deionized water, dilute hydrochloric acid, Virahol successively afterwards, dry, transfer on 300nm thick silicon dioxide/silicon substrate, finally use hot acetone removing PMMA layer.
Fig. 5 is the light micrograph of product on silicon chip, and Fig. 6 is the electron scanning micrograph of product, and the hexagonal structure of product and uniform contrast, be illustrated as single crystal graphene as can be observed from Figure.Meanwhile, the Raman spectrum of Fig. 7, the transmission electron micrograph of Fig. 8, the selected area electron diffraction photo of Fig. 9 and Figure 10 selected area electron diffraction intensity all prove that it is monocrystalline bilayer graphene.
Embodiment four:
As shown in Figure 2, carbon source is coronene, and copper catalyst is polycrystalline Copper Foil, and reactor is silica tube, and No. 1 pipe is tunger tube, and No. 2 pipes are hydrogen pipe.
Prepare a method for monocrystalline bilayer graphene, comprise the following steps:
A) clean polycrystalline Copper Foil is put into the middle part of the silica tube of chemical gas-phase deposition system, silica tube is vacuumized, and argon gas and hydrogen is passed in silica tube, argon hydrogen mixture is made to be full of reactor, repeatedly vacuumize for three times and inner air tube is removed completely, and then pass into argon hydrogen mixture in silica tube;
B) polycrystalline Copper Foil is heated, the central zone temperature of silica tube is made to reach 1050 DEG C, when the temperature of the central zone of silica tube reaches 1050 DEG C, pass into 400sccm argon gas in silica tube while, pass into 50sccm hydrogen as reducing gas, and keep temperature now 40 minutes, anneal is carried out to polycrystalline copper foil surface;
C) then carrying out cooling to polycrystalline Copper Foil makes it reach 600 DEG C, in pipe, the temperature of central zone is reduced to the process of cooling of 600 DEG C from 1050 DEG C, with heating zone, position, coronene place is heated, its temperature is made to rise to 200 DEG C, for graphene growth provides enough carbon sources, monocrystalline bilayer graphene can be obtained at polycrystalline copper foil surface.
Figure 11 is the electron scanning micrograph of product, has the two-dimensional film shape hexagonal structure of fold striped as can be observed from Figure, is illustrated as monocrystalline bilayer graphene.
Embodiment five:
As shown in Figure 2, carbon source is polystyrene, and copper catalyst is the Copper thin film be deposited on silicon chip, and reactor is silica tube, and No. 1 pipe is tunger tube, and No. 2 pipes are nitrogen tube.
Copper thin film can use fine copper target by chemical Vapor deposition process, physical vaporous deposition, vacuum thermal evaporation, magnetron sputtering method, plasma enhanced chemical vapor deposition method and print process by copper evaporation on substrate, then this substrate is put into the silica tube of chemical gas-phase deposition system.
Prepare a method for monocrystalline bilayer graphene, comprise the following steps:
A) Copper thin film be deposited on silicon chip is put into the middle part of silica tube, silica tube is vacuumized, and argon gas and nitrogen is passed in silica tube, argon hydrogen mixture is made to be full of reactor, repeatedly vacuumize for three times and inner air tube is removed completely, and then pass into argon nitrogen mixture gas in silica tube;
B) to the Copper thin film heating be deposited on silicon chip, make the central zone temperature of silica tube reach 1030 DEG C, when the temperature of the central zone of silica tube reaches 1030 DEG C, in silica tube, pass into argon gas and nitrogen, and keep temperature now 120 minutes, anneal is carried out to Copper thin film;
C) then carrying out cooling to the Copper thin film be deposited on silicon chip makes it reach 800 DEG C, in pipe, the temperature of central zone is reduced to the process of cooling of 800 DEG C from 1030 DEG C, heat with position, p-poly-phenyl ethene place, heating zone, its temperature is made to rise to 400 DEG C, for graphene growth provides enough carbon sources, monocrystalline bilayer graphene can be obtained on Copper thin film surface.
In step c) after, also comprise steps d), first PDMS is spin-coated on the Copper thin film surface that growth has Graphene, and heat on warm table, then put into copper-bath corrosion 12 hours removing copper, clean with deionized water, dilute hydrochloric acid, Virahol successively afterwards, dry, transfer in target substrate, finally use hot acetone removing PDMS layer.
Figure 12 is the electron scanning micrograph of product, has the two-dimensional film shape hexagonal structure of fold striped as can be observed from Figure, is illustrated as Graphene.
The present invention utilizes isothermal or non-isothermal aumospheric pressure cvd method on copper catalyst, prepare large size single crystal bilayer graphene, and present method is easy to operate, simple, can be used for high-end electronic device and unicircuit; In addition, there is compared with the monocrystalline bilayer graphene that prepared by the monocrystalline bilayer graphene prepared of non-isothermal method of the present invention and isothermal method the advantage of larger size and less defect.
Above-described specific embodiment; technical problem, technical scheme and beneficial effect that the present invention solves are further described; be understood that; the foregoing is only specific embodiments of the invention; be not limited to the present invention; within the spirit and principles in the present invention all, any amendment made, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (7)
1. prepare a method for monocrystalline bilayer graphene, comprise the following steps:
A) copper catalyst is put into reactor, and pass into non-oxidizing gas in reactor, make non-oxidizing gas be full of reactor, described copper catalyst is single crystal Cu or polycrystalline copper or Copper thin film;
B) copper catalyst is heated to target temperature, then keep homo(io)thermism 30-120 minute, the temperature range of described target temperature is: 1000 DEG C ~ 1070 DEG C;
C) continue to keep homo(io)thermism, the non-oxidizing gas carrying carbon source is passed in reactor, monocrystalline bilayer graphene can be obtained on copper catalyst surface.
2. prepare a method for monocrystalline bilayer graphene, comprise the following steps:
A) copper catalyst is put into reactor, and pass into non-oxidizing gas in reactor, make non-oxidizing gas be full of reactor, described copper catalyst is single crystal Cu or polycrystalline copper or Copper thin film;
B) copper catalyst is heated to target temperature, then keep homo(io)thermism 30-120 minute, the temperature range of described target temperature is: 1000 DEG C ~ 1070 DEG C;
C) then carrying out cooling to copper catalyst makes it reach 900 DEG C ~ 500 DEG C, in above-mentioned temperature-fall period, passes in reactor by the non-oxidizing gas carrying carbon source, can obtain monocrystalline bilayer graphene on copper catalyst surface.
3. the method preparing monocrystalline bilayer graphene according to claim 1 and 2, is characterized in that: step c) described in carbon source be methane and/or acetylene and/or polystyrene and/or coronene.
4. the method preparing monocrystalline bilayer graphene according to claim 3, is characterized in that: in step c) in, for gaseous carbon sources, gaseous carbon sources and non-oxidizing gas pass in reactor simultaneously.
5. the method preparing monocrystalline bilayer graphene according to claim 4, it is characterized in that: in step c) in, for solid carbon source, solid carbon source is placed on one end that reactor passes into air-flow, and with heating zone, position, solid carbon source place is heated, the temperature range of heating is: 200 DEG C-400 DEG C.
6. the method preparing monocrystalline bilayer graphene according to claim 1, it is characterized in that: in step c) after, also comprise steps d), first PMMA or PDMS is spin-coated on the substrate surface that growth has Graphene, and heat on warm table, then put into iron(ic) chloride or copper sulfate or ammonium persulfate solution and corrode 1-24 hour removing copper, clean with deionized water, dilute hydrochloric acid, Virahol successively afterwards, dry, transfer in target substrate, finally use hot acetone removing PMMA or PDMS layer.
7. the method preparing monocrystalline bilayer graphene according to claim 1 and 2, is characterized in that: described non-oxidizing gas is argon gas and/or nitrogen and/or hydrogen.
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| CN106087051A (en) * | 2016-06-02 | 2016-11-09 | 南京大学 | The preparation method of synchronous growth wafer scale AB stacking bilayer graphene and equipment thereof |
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| CN106335897A (en) * | 2016-08-26 | 2017-01-18 | 中国人民大学 | Large single crystal double layer graphene and the preparation method thereof |
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