CN106698408B - A kind of concave structure single crystal graphene and preparation method thereof - Google Patents
A kind of concave structure single crystal graphene and preparation method thereof Download PDFInfo
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- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
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- 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
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
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- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
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Abstract
The present invention discloses a kind of preparation method of concave structure single crystal graphene the following steps are included: 1) using acetic acid and acetone ultrasonic cleaning copper foil substrate, then carries out pre-anneal treatment；2) pre-oxidation treatment is carried out to the copper foil substrate after annealing；3) chemical gas deposition is carried out on the copper foil after step 2) pre-oxidation treatment using chemical vapour deposition technique, it is cooling up to the concave structure single crystal graphene.Preparation process of the present invention is simple and convenient to operate, favorable repeatability, by controlling reaction atmosphere, prepare the single crystal graphene with spill (internal single layer periphery is double-deck) structure, and the cost being related to is low, reproducible, has a good application prospect in fields such as optics, microwave diode and sensors.
Description
Technical field
The present invention relates to a kind of concave structure single crystal graphene and preparation method thereof more particularly to a kind of middle part single layer peripheries
The controllable preparation of the single crystal graphene of double-layer structure.
Background technique
Since two thousand four, people achieve huge breakthrough to the research of graphene property and application, are corresponding to it
Graphene technology of preparing also in rapid progress, search out a kind of quickly cheap mode is to prepare high-quality graphene
All graphene researcher focus of attention.So far, people have been developed that mechanical stripping method, silicon carbide epitaxy method,
Liquid phase stripping method, oxidation-reduction method, the preparation methods such as chemical vapour deposition technique and from bottom to top synthetic method.These methods respectively have excellent
Gesture, suitable for different occasions, wherein chemical vapour deposition technique is considered as the preparation method of most prospect.
With the further investigation to graphene, people have obtained a series of graphene of special constructions, their special knots
Structure and performance can satisfy the demand of many special industries, obtain there are mainly two types of the methods of the graphene of these special constructions:
Photoetching and chemical vapor deposition.Wherein, it is needed by the graphene that photoetching process obtains object construction by spin coating, production mask
Plate, photoetching and except glue, cost is very high.The present invention is made by methane partial pressure, depositing temperature and the collaboration of pre-oxidation
It is low in cost with having obtained the graphene of " recessed " shape structure, it is reproducible.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of concave structure single crystal graphene, the present invention passes through methane point
The mono-crystalline structures that graphene made from pressure, depositing temperature and the synergistic effect of pre-oxidation has middle part single layer, periphery double-deck, and relate to
And it is reproducible, to graphene monocrystalline research have important progradation.
To achieve the above object, the technical solution adopted by the present invention are as follows:
A kind of preparation method of concave structure single crystal graphene, includes the following steps:
1) it is cleaned by ultrasonic copper foil substrate using acetic acid and acetone, then carries out pre-anneal treatment；
2) gained copper foil substrate will be handled through step 1) carry out pre-oxidation treatment；
3) chemical vapor deposition is carried out on the copper foil after step 2) pre-oxidation treatment using chemical vapour deposition technique, it is cold
But up to the concave structure single crystal graphene.
In above scheme, the ultrasonic cleaning step are as follows: method for suppersonic cleaning is used, with acetic acid (purity 99.5wt%)
20~40min is cleaned to copper foil respectively with acetone (purity 99.5wt%).Wherein acetic acid can wash the oxidation of copper foil surface
Layer makes copper atom be exposed to most surface layer, promotes catalytic performance.Acetone can wash the residual organic impurities of copper foil surface, have
Conducive to graphene nucleation density is reduced, make cleaning more thorough by way of ultrasonic cleaning, guarantees graphene growth environment
Cleaning.
In above scheme, the pre-anneal treatment uses normal pressure annealing process, the specific steps are as follows: pass first into 500~
The Ar gas of 1000sccm drains air, is then passed through the H of 50~100sccm simultaneously2Gas is again heated to 1050~1080 DEG C, moves back
90~120min of fire closes H2Gas.The present invention can further remove the impurity of copper foil surface using annealing process, can also make
Copper domain is grown up, and the surface of atomically flating is obtained, and is conducive to the nucleation for controlling graphene.
In above scheme, the pre-oxidation treatment technique are as follows: keep Ar gas be passed through flow be 500~1000sccm side by side
H to the greatest extent2Gas, then it is passed through the O of 3~5sccm simultaneously2Gas, oxidizing temperature are 1050~1080 DEG C, and oxidization time is 5~10min, are closed
O2Gas.The present invention is passivated copper foil using pre-oxidation treatment technique, so that oxygen atom is occupied the nucleation site of graphene, further decreases
Graphene nucleation density is conducive to growing up for graphene monocrystalline.
In above scheme, the chemistry gas deposition step are as follows: the flow that is passed through of Ar gas is kept to be 500~1000sccm and lead to
Enter the H of 300~500sccm2, while being passed through the CH of 1~1.5sccm4, depositing temperature is 1050~1080 DEG C, sedimentation time 60
~90min.Internal single layer periphery double-layer structure can be obtained by the synergistic effect of pre-oxidation, atmosphere and depositing temperature in this step
Single crystal graphene, it is low in cost, it is reproducible.
The flow that is passed through that Ar gas is kept in above scheme, in cooling step described in step 3) is 500~1000sccm, is closed
Close CH4, and adjust H2Flow is 50~100sccm's, is down to 100 DEG C hereinafter, closing Ar, H to temperature2.This step is passed through 500
The H of the Ar and 50~100sccm of~1000sccm2, so that gained graphene film is stablized cooling under protective atmosphere, ensure that institute
The quality for obtaining graphene film, obtaining single crystal graphene is double-deck structure (concave structure single crystal graphene) in middle part single layer periphery.
According to concave structure single crystal graphene prepared by above scheme, its laminated structure double-deck in middle part single layer periphery
(middle part is single-layer graphene, and periphery is bilayer graphene, forms concave structure of the middle part to lower recess), single crystal graphene etc.
Imitating diameter is 10~80 μm.Wherein, the single-layer graphene at middle part has semimetallic characteristic, peripheral bilayer graphene structure tool
There is the characteristic of semiconductor, schottky junction can be formed in the two interface, can be applied to the fields such as microwave diode.
The present invention has obtained novel concave structure by methane partial pressure, depositing temperature and the synergistic effect of pre-oxidation for the first time
Single crystal graphene.Field effect transistor, which is fabricated to, using this single crystal graphene is desired to have excellent performance；Additionally due to
Inhomogeneities of the concave structure single crystal graphene in number of plies distribution, can be applied to microwave diode and sensor etc.,
It has broad application prospects.
The invention has the benefit that preparation method of the present invention is simple, and it is easy to operate, in methane partial pressure, deposition
At temperature and the synergistic effect of pre-oxidation, the sheet concave structure single crystal graphite of middle part single layer, peripheral double-layer structure can be obtained
Alkene, it is low in cost, it is reproducible, and inhomogeneities of the products therefrom in number of plies distribution, in optics, microwave diode and sensing
The fields such as device have a good application prospect.
Detailed description of the invention
Fig. 1 is that the SEM of 1 products therefrom of the embodiment of the present invention schemes；
Fig. 2 is 1 products therefrom of the embodiment of the present invention in SiO2(a) Raman test result and (b) optics on/Si substrate is aobvious
Structure chart under micro mirror；
Fig. 3 is the SAED figure of the double layer area of 1 products therefrom of the embodiment of the present invention.
Fig. 4 is that the SEM of comparative example products therefrom of the present invention schemes.
Specific embodiment
To make the objectives, technical solutions, and advantages of the present invention more comprehensible, with reference to embodiments, to the present invention into
Row is further described.It should be appreciated that described herein, specific examples are only used to explain the present invention, is not used to limit
The present invention.
Embodiment 1
A kind of concave structure single crystal graphene, preparation method include the following steps:
1) copper foil that area is 2cm × 2cm is cut, successively using acetic acid (purity 99.5wt%) and acetone, (concentration is
99.5wt%) by copper foil ultrasonic cleaning 20min；Copper foil after cleaning is put into quartz ampoule, quartz tube 6cm, it is long
Degree is 100cm, is passed through the Ar of 500sccm, keeps 30min, it is ensured that drains the air in quartz ampoule, then is passed through 50sccm's simultaneously
H2, 1050 DEG C are risen to the speed of 15 DEG C/min, is kept 90min (annealing), H is closed2；
2) the Ar throughput in step 1) is kept to drain H in quartz ampoule2, then it is passed through the O of 3sccm2Pre-oxidation treatment is carried out,
5min is kept, oxidizing temperature is 1050 DEG C, closes O2；Keep the flow of Ar in step 2) constant, H2Flow increase to
300sccm, and it is passed through the CH of 1sccm4, chemical vapor deposition is carried out at a temperature of 1050 DEG C, growth is kept the temperature on copper foil
60min；
3) it keeps the flow of Ar in step 2) constant, closes CH4, H2Flow is decreased to 50sccm, is down to 100 DEG C to temperature
Hereinafter, closing Ar, H2, sample is taken out to get the concave structure single crystal graphene.
Fig. 1 is the SEM structure chart of the present embodiment products therefrom, and products therefrom diameter is 10~80 μm；Fig. 2 is embodiment institute
Product is obtained in SiO2Structure chart under (a) optical microscopy and (b) Raman test result on/Si substrate, wherein No. 1 region
I2D: IG> 2, i.e. No. 1 region is single layer region, the I in No. 2 regions2D: IG< 1, i.e., No. 2 regions are double layer area, illustrate products therefrom
In double-deck concave structure in internal single layer, periphery.Fig. 3 is the SAED figure of the double layer area of embodiment products therefrom, I in figure1-210:
I1-100> 2, i.e. shooting area is double layer area.
The present embodiment products therefrom is applied to prepare microwave diode, shows good service performance.
Embodiment 2
A kind of concave structure single crystal graphene, preparation method include the following steps:
1) copper foil that area is 2cm × 2cm is cut, successively using acetic acid (purity 99.5wt%) and acetone, (concentration is
99.5wt%) by copper foil ultrasonic cleaning 30min；Copper foil after cleaning is put into quartz ampoule, quartz tube 6cm, it is long
Degree is 100cm, is passed through the Ar of 750sccm, keeps 30min, it is ensured that drains the air in quartz ampoule, then is passed through 75sccm's simultaneously
H2, 1065 DEG C are risen to the speed of 15 DEG C/min, keeps 100min, closes H2(annealing)；
2) Ar throughput in step 1) is kept to drain H in quartz ampoule2, then it is passed through the O of 4sccm2, keep 7min, oxidizing temperature
1065 DEG C, close O2；Keep the flow of Ar in step 2) constant, H2Flow increase to 400sccm, and be passed through 1.2sccm's
CH4, chemical vapor deposition is carried out at a temperature of 1065 DEG C, the heat preservation growth 70min on copper foil；
4) it keeps the flow of Ar in step 3) constant, closes CH4, H2Flow is decreased to 75sccm, is down to 100 DEG C to temperature
Hereinafter, closing Ar, H2, sample is taken out to get the concave structure single crystal graphene.
The present embodiment products therefrom is applied to prepare microwave diode, shows good service performance.
Embodiment 3
A kind of concave structure single crystal graphene, preparation method include the following steps:
1) copper foil that area is 2cm × 2cm is cut, successively using acetic acid (purity 99.5wt%) and acetone, (concentration is
99.5wt%) by copper foil ultrasonic cleaning 40min；Copper foil after cleaning is put into quartz ampoule, quartz tube 6cm, it is long
Degree is 100cm, is passed through the Ar of 1000sccm, keeps 30min, it is ensured that drains the air in quartz ampoule, then is passed through 100sccm simultaneously
H2, 1080 DEG C are risen to the speed of 15 DEG C/min, is kept 120min (annealing), H is closed2；
2) Ar throughput in step 1) is kept to drain H in quartz ampoule2, then it is passed through the O of 5sccm2Pre-oxidation treatment is carried out, is protected
10min is held, oxidizing temperature is 1080 DEG C, closes O2；Keep the flow of Ar in step 2) constant, H2Flow increase to
500sccm, and it is passed through the CH of 1.5sccm4, chemical vapor deposition is carried out at a temperature of 1080 DEG C, heat preservation growth is (heavy on copper foil
Product) 90min；
3) it keeps the flow of Ar in step 2) constant, closes CH4, H2Flow is decreased to 100sccm, is down to 100 DEG C to temperature
Hereinafter, closing Ar, H2, sample is taken out to get the concave structure single crystal graphene.
The present embodiment products therefrom is applied to prepare microwave diode, shows good service performance.
Comparative example
A kind of single crystal graphene, preparation method include the following steps:
1) copper foil that area is 2cm × 2cm is cut, successively using acetic acid (purity 99.5wt%) and acetone, (concentration is
99.5wt%) by copper foil ultrasonic cleaning 40min；Copper foil after cleaning is put into quartz ampoule, quartz tube 6cm, it is long
Degree is 100cm, is passed through the Ar of 1000sccm, keeps 30min, it is ensured that drain the air in quartz ampoule, then be passed through 100sccm's
H2, 1080 DEG C are risen to the speed of 15 DEG C/min, keeps 120min, closes H2；
2) Ar throughput in step 1) is kept to drain H in quartz ampoule2, then it is passed through the O of 5sccm2, keep 10min, oxidation temperature
Degree is 1080 DEG C, closes O2；Keep the flow of Ar in step 2) constant, H2Flow reduce to 50sccm, and be passed through 1sccm's
CH4, chemical vapor deposition is carried out at a temperature of 1080 DEG C, the heat preservation growth 60min on copper foil；
3) it keeps the flow of Ar in step 2) constant, closes CH4, H2Flow increases to 100sccm, is down to 100 DEG C to temperature
Hereinafter, closing Ar, H2, take out sample.Gained sample is no longer concave structure single crystal graphene.
Fig. 4 is the SEM structure chart of this comparative example products therefrom, and gained graphene monocrystalline is in uniform laminated structure.
Above-described embodiment is just for the sake of clearly demonstrating the present invention, not to the limitation of embodiment, while here without
It needs also be exhaustive all embodiments.For those of ordinary skill in the art, the present invention is not being departed from
Under the premise of concept, amplified it is obvious it is several improvement and variation still in the invention protection scope it
It is interior.
Claims (5)
1. a kind of preparation method of concave structure single crystal graphene, which comprises the steps of:
1) it is cleaned by ultrasonic copper foil substrate using acetic acid and acetone, then carries out pre-anneal treatment；
2) gained copper foil substrate will be handled through step 1) carry out pre-oxidation treatment；
3) chemical gas deposition is carried out on the copper foil after step 2) pre-oxidation treatment using chemical vapour deposition technique, cooling to obtain the final product
The concave structure single crystal graphene；Its laminated structure double-deck in middle part single layer periphery, middle part is single-layer graphene, and periphery is
Bilayer graphene；
The pre-oxidation treatment technique are as follows: the flow that is passed through of Ar gas is kept to be 500~1000sccm and drain H2Gas, then lead to simultaneously
Enter the O of 3~5sccm2Gas, oxidizing temperature are 1050~1080 DEG C, and oxidization time is 5~10min, close O2Gas；
The chemistry gas deposition step are as follows: the flow that is passed through of Ar gas is kept to be 500~1000sccm and be passed through 300~500sccm
H2, while being passed through the CH of 1~1.5sccm4, depositing temperature is 1050~1080 DEG C, and sedimentation time is 60~90min.
2. preparation method according to claim 1, which is characterized in that the ultrasonic cleaning step are as follows: clear using ultrasonic wave
Washing method successively cleans 20~40min to copper foil respectively with acetic acid and acetone.
3. preparation method according to claim 1, which is characterized in that the pre-anneal treatment uses normal pressure annealing process,
Specific step is as follows: the Ar gas for passing first into 500~1000sccm drains air, is then passed through the H of 50~100sccm simultaneously2
Gas is again heated to 1050~1080 DEG C, and anneal 90~120min, and annealing is completed to close H2Gas.
4. preparation method according to claim 1, which is characterized in that keep Ar gas in cooling step described in step 3)
Being passed through flow is 500~1000sccm, closes CH4, and adjust H2Flow is 50~100sccm, to temperature be down to 100 DEG C with
Under, close Ar, H2。
5. concave structure single crystal graphene made from any one of Claims 1 to 4 preparation method, which is characterized in that described recessed
The shape structure single crystal graphene laminated structure double-deck in middle part single layer, periphery, the equivalent diameter of single crystal graphene is 10~80 μm.
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