CN106698408A - Concave structure monocrystalline graphene and preparation method thereof - Google Patents
Concave structure monocrystalline graphene and preparation method thereof Download PDFInfo
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- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
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Abstract
The invention discloses a preparation method of concave structure monocrystalline graphene. The method comprises the following steps: 1, carrying out ultrasonic cleaning on a copper foil substrate by using acetic acid and acetone, and carrying out pre-annealing treatment; 2, pre-oxidizing the annealed copper foil substrate; and 3, carrying out chemical vapor deposition on the pre-oxidized copper foil through adopting a chemical vapor deposition technology, and cooling the deposited copper foil to obtain the concave structure monocrystalline graphene. The preparation method has the advantages of simplicity, convenience in operation, good repeatability, reparation of the concave (internal single layer and external double layers) structure monocrystalline graphene through controlling reaction atmosphere and low cost, and the concave structure monocrystalline graphene has very good application prospect in the fields of optical and microwave diodes 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 individual layer periphery
The controllable preparation of the single crystal graphene of double-decker.
Background technology
Since two thousand four, research of the people to Graphene property and application achieves huge breakthrough, corresponds to therewith
Graphene technology of preparing also in rapid progressive, searching out a kind of quick cheap mode preparing high-quality graphene is
All Graphene researcher focus of attention.So far, people have been developed that mechanical stripping method, silicon carbide epitaxy method,
The preparation methods such as liquid phase stripping method, oxidation-reduction method, from bottom to top chemical vapour deposition technique and synthetic method.These methods respectively have excellent
Gesture, it is adaptable to which different occasions, wherein chemical vapour deposition technique are 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 meet the demand of many special industries, and the method for obtaining the Graphene of these special constructions mainly has two kinds：
Photoetching and chemical vapor deposition.Wherein, the Graphene for obtaining object construction by photoetching process needs by spin coating, makes mask
The steps such as plate, photoetching and removing glue, cost is very high.The present invention is made by the collaboration of methane partial pressure, depositing temperature and pre-oxidation
It is with low cost with the Graphene for having obtained " recessed " shape structure, it is reproducible.
The content of the invention
It is an object of the invention to provide a kind of preparation method of concave structure single crystal graphene, the present invention is by methane point
Graphene obtained in the synergy of pressure, depositing temperature and pre-oxidation has double-deck mono-crystalline structures of middle part individual layer, periphery, and relates 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 is：
A kind of preparation method of concave structure single crystal graphene, comprises the following steps：
1) it is cleaned by ultrasonic Copper Foil substrate using acetic acid and acetone, then carries out pre-anneal treatment；
2) will be through step 1) treatment gained Copper Foil substrate carry out pre-oxidation treatment；
3) using chemical vapour deposition technique through step 2) chemical vapor deposition is carried out on Copper Foil after pre-oxidation treatment, it is cold
But the concave structure single crystal graphene is obtained final product.
In such scheme, the ultrasonic cleaning step is：Using method for suppersonic cleaning, 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 exposed to most top layer, lifts catalytic performance.Acetone can wash the residual organic impurities of copper foil surface, have
Beneficial to Graphene nucleation density is reduced, make cleaning more thorough by way of ultrasonic wave is cleaned, it is ensured that graphene growth environment
Cleaning.
In such scheme, the pre-anneal treatment uses normal pressure annealing process, comprises the following steps that：Pass first into 500~
The Ar gas of 1000sccm drains air, and the H of 50~100sccm is then passed through 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 obtains the surface of atomically flating, is conducive to controlling the nucleation of Graphene.
In such scheme, the pre-oxidation treatment technique is：Keep Ar gas be passed through flow for 500~1000sccm side by side
H to the greatest extent2Gas, then the O of 3~5sccm is passed through simultaneously2Gas, oxidizing temperature is 1050~1080 DEG C, and oxidization time is 5~10min, is closed
O2Gas.The present invention makes oxygen atom occupy the nucleation site of Graphene using pre-oxidation treatment technique passivation Copper Foil, further reduces
Graphene nucleation density, is conducive to growing up for Graphene monocrystalline.
In such scheme, the chemical gas deposition step is：Keep being passed through flow for 500~1000sccm and leading to for Ar gas
Enter the H of 300~500sccm2, while being passed through the CH of 1~1.5sccm4, depositing temperature is 1050~1080 DEG C, and sedimentation time is 60
~90min.This step is that can obtain internal individual layer periphery double-decker by the synergy of pre-oxidation, atmosphere and depositing temperature
Single crystal graphene, it is with low cost, it is reproducible.
In such scheme, step 3) described in keep Ar gas in cooling step be passed through flow for 500~1000sccm, close
Close CH4, and adjust H2Flow is 50~100sccm's, treats that temperature is down to less than 100 DEG C, closes Ar, H2.This step is passed through 500
The H of the Ar and 50~100sccm of~1000sccm2, make the stabilization cooling under protective atmosphere of gained graphene film, it is ensured that institute
The quality of graphene film is obtained, it is double-deck structure (concave structure single crystal graphene) in middle part individual layer periphery to obtain single crystal graphene.
According to concave structure single crystal graphene prepared by such scheme, it is in double-deck laminated structure in middle part individual 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.
Imitate a diameter of 10~80 μm.Wherein, the single-layer graphene at middle part has semimetallic characteristic, the bilayer graphene structure tool of periphery
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 synergy that the present invention passes through methane partial pressure, depositing temperature and pre-oxidation, has obtained novel concave structure first
Single crystal graphene.Field-effect transistor is fabricated to using this single crystal graphene be desired to have excellent performance；Additionally due to
Inhomogeneities of the concave structure single crystal graphene in number of plies distribution, can apply to the aspects such as microwave diode and sensor,
Have broad application prospects.
Beneficial effects of the present invention are：Preparation method of the present invention is simple, easy to operate, in methane partial pressure, deposition
At temperature and the synergy of pre-oxidation, you can obtain middle part individual layer, the sheet concave structure single crystal graphite of peripheral double-decker
Alkene, it is with low 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 good application prospect.
Brief description of the drawings
Fig. 1 schemes for the SEM of the products therefrom of the embodiment of the present invention 1；
Fig. 2 is the products therefrom of the embodiment of the present invention 1 in SiO2(a) Raman test result and (b) optics on/Si substrates show
Structure chart under micro mirror；
Fig. 3 is the SAED figures of the double layer area of the products therefrom of the embodiment of the present invention 1.
Fig. 4 is the SEM figures of comparative example products therefrom of the present invention.
Specific embodiment
To make the objects, technical solutions and advantages of the present invention become more apparent, with reference to embodiments, the present invention is entered
Row is further described.It should be appreciated that specific embodiment described herein is only used to explain the present invention, it is not used to limit
The present invention.
Embodiment 1
A kind of concave structure single crystal graphene, its preparation method comprises the following steps：
1) it is the Copper Foil of 2cm × 2cm to cut area, and (concentration is successively to use acetic acid (purity is 99.5wt%) and acetone
Copper Foil ultrasonic wave 99.5wt%) is cleaned into 20min；Copper Foil after cleaning is put into quartz ampoule, quartz tube is 6cm, it is long
It is 100cm to spend, and 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, 90min (annealing) is kept, close H2；
2) keep step 1) in Ar throughputs drain H in quartz ampoule2, then the O for being passed through 3sccm2Carry out pre-oxidation treatment,
5min is kept, oxidizing temperature is 1050 DEG C, closes O2；Keep step 2) in Ar flow it is 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 incubated on Copper Foil
60min；
3) keep step 2) in Ar flow it is constant, close CH4, H2Flow is decreased to 50sccm, treats that temperature is down to 100 DEG C
Hereinafter, Ar, H are closed2, sample is taken out, obtain final product the concave structure single crystal graphene.
Fig. 1 is the SEM structure charts of the present embodiment products therefrom, a diameter of 10~80 μm of products therefrom；Fig. 2 is embodiment institute
Product is obtained in SiO2Structure chart under (a) light microscope and (b) Raman test result on/Si substrates, wherein No. 1 region
I2D：IG>2, i.e., No. 1 region are individual layer region, No. 2 I in region2D：IG<1, i.e., No. 2 region are double layer area, illustrate products therefrom
In double-deck concave structure in internal individual layer, periphery.Fig. 3 is the SAED figures of the double layer area of embodiment products therefrom, I in figure1-210：
I1-100>2, i.e. shooting area are double layer area.
The present embodiment products therefrom is applied to prepare microwave diode, good performance is shown.
Embodiment 2
A kind of concave structure single crystal graphene, its preparation method comprises the following steps：
1) it is the Copper Foil of 2cm × 2cm to cut area, and (concentration is successively to use acetic acid (purity is 99.5wt%) and acetone
Copper Foil ultrasonic wave 99.5wt%) is cleaned into 30min；Copper Foil after cleaning is put into quartz ampoule, quartz tube is 6cm, it is long
It is 100cm to spend, and 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, 100min is kept, close H2(annealing)；
2) keep step 1) in Ar throughputs drain H in quartz ampoule2, then the O for being passed through 4sccm2, keep 7min, oxidizing temperature
1065 DEG C, close O2；Keep step 2) in Ar flow it is 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, growth 70min is incubated on Copper Foil；
4) keep step 3) in Ar flow it is constant, close CH4, H2Flow is decreased to 75sccm, treats that temperature is down to 100 DEG C
Hereinafter, Ar, H are closed2, sample is taken out, obtain final product the concave structure single crystal graphene.
The present embodiment products therefrom is applied to prepare microwave diode, good performance is shown.
Embodiment 3
A kind of concave structure single crystal graphene, its preparation method comprises the following steps：
1) it is the Copper Foil of 2cm × 2cm to cut area, and (concentration is successively to use acetic acid (purity is 99.5wt%) and acetone
Copper Foil ultrasonic wave 99.5wt%) is cleaned into 40min；Copper Foil after cleaning is put into quartz ampoule, quartz tube is 6cm, it is long
It is 100cm to spend, and 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, 120min (annealing) is kept, close H2；
2) keep step 1) in Ar throughputs drain H in quartz ampoule2, then the O for being passed through 5sccm2Pre-oxidation treatment is carried out, is protected
10min is held, oxidizing temperature is 1080 DEG C, closes O2；Keep step 2) in Ar flow it is 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, growth is incubated on Copper Foil (heavy
Product) 90min；
3) keep step 2) in Ar flow it is constant, close CH4, H2Flow is decreased to 100sccm, treats that temperature is down to 100 DEG C
Hereinafter, Ar, H are closed2, sample is taken out, obtain final product the concave structure single crystal graphene.
The present embodiment products therefrom is applied to prepare microwave diode, good performance is shown.
Comparative example
A kind of single crystal graphene, its preparation method comprises the following steps：
1) it is the Copper Foil of 2cm × 2cm to cut area, and (concentration is successively to use acetic acid (purity is 99.5wt%) and acetone
Copper Foil ultrasonic wave 99.5wt%) is cleaned into 40min；Copper Foil after cleaning is put into quartz ampoule, quartz tube is 6cm, it is long
It is 100cm to spend, and 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, 120min is kept, close H2；
2) keep step 1) in Ar throughputs drain H in quartz ampoule2, then the O for being passed through 5sccm2, keep 10min, oxidation temperature
It is 1080 DEG C to spend, and closes O2；Keep step 2) in Ar flow it is 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, growth 60min is incubated on Copper Foil；
3) keep step 2) in Ar flow it is constant, close CH4, H2Flow increases to 100sccm, treats that temperature is down to 100 DEG C
Hereinafter, Ar, H are closed2, take out sample.Gained sample is no longer concave structure single crystal graphene.
Fig. 4 is the SEM structure charts of this comparative example products therefrom, and gained Graphene monocrystalline is in uniform laminated structure.
Above-described embodiment just for the sake of clearly demonstrating the present invention, not to the limitation of implementation method, at the same here without
Need also be exhaustive all of implementation method.For the person of ordinary skill of the art, the present invention is not being departed from
Create design on the premise of, amplified it is obvious some improvement and change still in the invention protection domain it
It is interior.
Claims (7)
1. a kind of preparation method of concave structure single crystal graphene, it is characterised in that comprise the following steps：
1) it is cleaned by ultrasonic Copper Foil substrate using acetic acid and acetone, then carries out pre-anneal treatment；
2) will be through step 1) treatment gained Copper Foil substrate carry out pre-oxidation treatment；
3) using chemical vapour deposition technique through step 2) chemical gas deposition is carried out on Copper Foil after pre-oxidation treatment, cooling is obtained final product
The concave structure single crystal graphene.
2. preparation method according to claim 1, it is characterised in that the ultrasonic cleaning step is：It is 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, it is characterised in that the pre-anneal treatment uses normal pressure annealing process,
Comprise the following steps that：The Ar gas for passing first into 500~1000sccm drains air, and the H of 50~100sccm is then passed through simultaneously2
Gas, is again heated to 1050~1080 DEG C, and anneal 90~120min, and annealing completes to close H2Gas.
4. preparation method according to claim 1, it is characterised in that the pre-oxidation treatment technique is：Keep Ar gas
Flow is passed through for 500~1000sccm and H is drained2Gas, then the O of 3~5sccm is passed through simultaneously2Gas, oxidizing temperature be 1050~
1080 DEG C, oxidization time is 5~10min, closes O2Gas.
5. preparation method according to claim 1, it is characterised in that the chemical gas deposition step is：Keep Ar gas
Flow is passed through to be 500~1000sccm and be passed through the H of 300~500sccm2, while being passed through the CH of 1~1.5sccm4, depositing temperature
It it is 1050~1080 DEG C, sedimentation time is 60~90min.
6. preparation method according to claim 1, it is characterised in that step 3) described in keep Ar gas in cooling step
Flow is passed through for 500~1000sccm, CH is closed4, and adjust H2Flow is 50~100sccm's, treat temperature be down to 100 DEG C with
Under, close Ar, H2。
7. concave structure single crystal graphene obtained in preparation method described in any one of claim 1~6, it is characterised in that described
In double-deck laminated structure in middle part individual layer, periphery, the equivalent diameter of single crystal graphene is 10~80 μ to concave structure single crystal graphene
m。
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108423659A (en) * | 2018-05-30 | 2018-08-21 | 绍兴文理学院 | A kind of preparation method of the grade single layer single crystal graphene based on polycrystalline copper foil |
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| CN105439126A (en) * | 2014-09-01 | 2016-03-30 | 华北电力大学 | Simple preparation method of millimeter level monocrystalline graphene |
| US20160108546A1 (en) * | 2013-05-21 | 2016-04-21 | Iucf-Hyu (Industry-University Cooperation Foundation Hanyang University | Large-area single-crystal monolayer graphene film and method for producing the same |
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| US20160108546A1 (en) * | 2013-05-21 | 2016-04-21 | Iucf-Hyu (Industry-University Cooperation Foundation Hanyang University | Large-area single-crystal monolayer graphene film and method for producing the same |
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| CN104498902A (en) * | 2014-12-12 | 2015-04-08 | 中国科学院重庆绿色智能技术研究院 | Preparation method of graphene film by virtue of normal-pressure chemical vapor deposition |
| CN104975344A (en) * | 2015-07-09 | 2015-10-14 | 中国科学院上海微系统与信息技术研究所 | Low nucleation density graphene single crystal preparation method based on cuprous oxide film substrate |
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| CN108423659A (en) * | 2018-05-30 | 2018-08-21 | 绍兴文理学院 | A kind of preparation method of the grade single layer single crystal graphene based on polycrystalline copper foil |
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