CN106185897B - A method of the controllable preparation graphene nanobelt in a variety of substrates - Google Patents
A method of the controllable preparation graphene nanobelt in a variety of substrates Download PDFInfo
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Abstract
The invention discloses a kind of methods of controllable preparation graphene nanobelt in a variety of substrates.This method comprises: dry linear micro-nano monocrystalline is heat-treated, the graphene nanobelt is obtained.The present invention discloses a kind of method for preparing graphene nanobelt by the organic micro-nano monocrystalline heat treatment of aromatic molecules for the first time；It is disclosed for the first time by changing the pattern for preparing organic micro-nano monocrystalline come controllable preparation graphene nanobelt；This method enormously simplifies the preparation process of graphene nanobelt compared with traditional method, and significantly reduces the preparation cost of graphene nanobelt.This method can use the ordered arrangement that the method for simply controlling linear micro-nano monocrystalline arrangement realizes graphene nanobelt, and it is the method for greatly reducing cost that this, which prepares graphene nanobelt to current realization ordered arrangement,.
Description
Technical field
The invention belongs to graphene nanobelt preparation fields, are related to one kind controllable preparation graphene nano in a variety of substrates
The method of band.
Background technique
Graphene has the properties such as high carrier mobility, excellent thermal conductivity, is the reason in future electronic device
Think material (K.S.Novoselov, A.K.Geim, Science 2004,306,666.).However zero band gap properties pole of graphene
The earth limits its application in microelectronic component.The band gap for how opening and controlling graphene becomes graphene electronics
One key scientific problems of application.It is a kind of ideal opening graphite that two-dimensional graphene, which is cut into quasi-one-dimensional nanoribbons,
The method of alkene band gap.Extensive theoretical and experimental study has been carried out to this novel one-dimensional c-based nanomaterial of standard, has found it
With excellent physical and chemical performance, it is expected to obtain wide application ((a) Son, Y.-W. on nanoelectronics device；
Cohen,M.L.；Louie,S.G.Phys.Rev.Lett.2006,97,216803.(b)Wang,X.；Dai,
H.Nat.Chem.2010,2,661.).Structurally, graphene nanobelt (GNRs) and carbon nanotube (CNTs) close phase
It closes, is all quasi- one-dimentional structure, therefore be similar to the classification of CNTs, the different topology shape having according to the edge GNRs carbon atom
Shape can also be classified as armchair graphene nanobelt (AGNRs) and sawtooth pattern graphene nanobelt (ZGNRs).According to stone
The item number of carbon atom chain can define width Na (Fujita, the M. of nanobelt in black alkene nanobelt；Wakabayashi,K.；
Nakada,K.；Kusakabe,K.J.Phys.Soc.Jpn.1996,65,1920.).GNRs is by its special edge effect and width
The influence of degree, and there are flexible electrical properties, the origin of the band gap of the GNRs of different boundary is entirely different, the band gap of AGNRs
Width originating from quantum confinement and dependence nanobelt.The band gap of ZGNRs is derived from the localization edge potential that edge magneticization generates.Band
The opening of gap makes it be expected to have a wide range of applications in terms of quantum device.Research shows that the energy gap of GNRs can be with
The variation of nanometer bandwidth and change, wherein there is band gap in Na=20AGNRs, shows semiconductor property, and same wide
The ZGNRs of degree is the metal of zero band gap, and its marginality for occurring local at fermi level.When GNRs band gap open,
Biggish room temperature switch ratio may be implemented, so as to prepare the field effect transistor of high mobility and on-off ratio.Due to stone
Black alkene and its tempting physical property and the potential application value in nanoelectronics of derivative, to study low dimensional physics phenomenon
Provide a good opportunity.
The preparation method of GNRs can be mainly divided into two major classes according to forming types, respectively from bottom to top and from upper and
Under.Prepare from top to bottom GNRs typically refer to using raw material as graphene or carbon nanotube by photoetching process, micromechanics stripping method,
The methods of etching method, oxidizing process obtain.Usual preparation process is more complicated and the controllability on boundary is lower, obtained GNRs knot
Structure is also and inhomogenous, greatly influences to obtain the electric property of GNRs.Therefore, many seminars begin one's study from bottom to top recently
Method, generally include chemical vapour deposition technique, solution is combined to, metal surface assist synthesis etc..And chemical vapor deposition side
Method is difficult to prepare one-dimensional GNRs, needs to introduce some templates or metal kind since substrate has isotropism
Son, obtained graphene nanobelt is of low quality or is limited to the structure of template ((a) Sokolov, A.N.；Yap,F.L.；
Liu,N.；Kim,K.；Ci,L.；Johnson,O.B.；Wang,H.；Vosgueritchian,M.；Koh,A.L.；Chen,J.；
Park,J.；Bao,Z.Nat.Commun.2013,4,e2402.(b)Liu,N.；Kim,K.；Hsu,P.-C.；Sokolov,
A.N.；Yap,F.L.；Yuan,H.；Xie,Y.；Yan,H.；Cui,Y.；Hwang,H.Y.；Bao,
Z.J.Am.Chem.Soc.2014,136,17284.).Now from bottom to top organic synthesis method (including solution be combined to and gold
Metal surface assists synthesis) gradually get growing concern for, atomic level can achieve to the controllability of edge and width.
But the nanobelt size that the synthesis of solution phase obtains is extremely limited, often size is smaller.And metal surface is assisted
Synthesis needs to carry out ((a) Zhang, H. on monocrystalline noble metal；Lin,H.；Sun,K.；Chen,L.；Zagranyarski,Y.；
Aghdassi,N.；Duhm,S.；Li,Q.；Zhong,D.；Li,Y.；Müllen,K.；Fuchs,H.；Chi,
L.J.Am.Chem.Soc.2015,137,4022.(b)Basagni,A.；Sedona,F.；Pignedoli,C.A.；
Cattelan,M.；Nicolas,L.；Casarin,M.；Sambi, M.J.Am.Chem.Soc.2015,137,1802.), preparation
Condition it is harsher, and need in later period application process to prepare the device of graphene nanobelt by shifting.It is this
Method is more complicated by process, and the requirement of instrument needed for narrow GNRs is relatively high in order to obtain, has pole for industrialized utilization
Big difficulty.It is still a greatly challenge that graphene is directly prepared in a variety of and/or dielectric base, and inexpensive at present
And be hopeful industrialize graphene nanobelt preparation method still also need to explore.
Summary of the invention
The object of the present invention is to provide a kind of methods of controllable preparation graphene nanobelt in a variety of substrates.
The method provided by the invention for preparing graphene nanobelt includes the following steps: the linear micro-nano monocrystalline that will be dried
It is heat-treated, obtains the graphene nanobelt.
The heat treatment of the above method includes: that the linear micro-nano monocrystalline of the drying is placed in substrate, in inert conditions
Heating.
In the heating stepses, the final temperature of heating is 300-1000 DEG C or 800 DEG C；Soaking time be 3-120min or
8min。
The inert conditions are argon gas or nitrogen atmosphere；
The flow velocity of inert gas is 50-300sccm or 100sccm.
In this step, the relevant parameter of the length, thickness and width of graphene nanobelt and the linear micro-nano monocrystalline of gained
It is closely related, and structure is also closely related with the temperature and time of heat treatment, by the growth conditions for changing linear micro-nano monocrystalline
The controllable preparation of graphene nanobelt may be implemented with the condition of heat treatment.
The linear micro-nano monocrystalline of the drying by polycyclic fragrant organic molecule, Pyromellitic Acid, 1 containing carboxyl functional group,
4,5,8- naphthalenetetracarbacidic acidic or 3,4,9,10- tetracarboxylic acid are made；
Or, the linear micro-nano monocrystalline of the drying is by with polycyclic fragrant organic molecule, equal benzene tetramethyl containing carboxyl functional group
Acid, Isosorbide-5-Nitrae, 5,8- naphthalenetetracarbacidic acidics or 3,4,9,10- tetracarboxylic acids are solute, are molten at least one of water, ethyl alcohol and methanol
The solution of agent composition is made.
It in this step, in a solvent can be with self assembly as the polycyclic fragrant organic molecule containing carboxyl functional group of solute
Form linear micro-nano monocrystalline；Length, the width and thickness of the linear micro-nano monocrystalline can pass through solution concentration and growth time control
System；
More specifically, the linear micro-nano monocrystalline of the drying is made as follows (1) or (2):
The method (1) includes: that the growth of monocrystalline is carried out in solution, and growth, which finishes, is cooled to room temperature, is obtained containing wired
Property micro-nano monocrystalline liquid system, then the liquid system containing linear micro-nano monocrystalline is placed in substrate, is dried；
The method (2) includes: that substrate is placed in solution to the growth for carrying out monocrystalline, and growth, which finishes, is cooled to room temperature, is dried
It is dry.
In the method (1) and method (2), the concentration of the solution is 2-50g.ml-1Or 10g.ml-1Or 6 μ g.ml-1Or
13μg.ml-1；
In the growth step of the monocrystalline, temperature is 35-50 DEG C or 40 DEG C；Time is 1-48h or 5h or 10h or 5-10h.
The method also includes making the graphene nanobelt ordered arrangement, also i.e. by the linear micro-nano monocrystalline
The step of carrying out ordered arrangement；
The step of making linear micro-nano monocrystalline ordered arrangement following steps a, step b or step c.
Specifically, the liquid system containing linear micro-nano monocrystalline is placed in substrate by the step a in the method (1)
After step, before the baking step；
The step a is to flow the liquid system containing linear micro-nano monocrystalline in the same direction on the substrate
It is dynamic；
Liquid system containing linear micro-nano monocrystalline is being placed in step in substrate in the method (1) by the step b
Before；
The step b is to be surface-treated to the substrate；
The step c is in the method (2) before the growth step of monocrystalline；
The step c is to be surface-treated to the substrate.
Various common surface treatment methods are applicable in, and such as can refer to Review literature Controlled Deposition of
Crystalline Organic Semiconductors for Field-Effect-Transistor Applications。
Specifically, the surface treatment can be in the orderly groove of substrate surface setting.
In the above method, substrate used does not dissolve in solvent for use；Be chosen in particular from metal, dielectric base, plastics, glass or
Mica.It more specifically can be SiO2/ Si substrate or SERS substrate.Again concretely with a thickness of 300nm/500 μm of SiO2/ Si substrate.Institute
The thickness for stating substrate is arbitrarily adjustable.For metallic substrates, can also according to routine operation by its elder generation in reducibility gas such as hydrogen
Annealing.
In addition, the graphene nanobelt being prepared according to the method described above, also belongs to protection scope of the present invention；Wherein,
The width of the graphene nanobelt is specially 20-300nm, more specifically can be 80-100nm.
The method provided by the invention for preparing graphene nanobelt, the method pass through self assembly shape using polycyclic aromatic molecules
Then linear micro-nano monocrystalline makes linear micro-nano single crystal transition graphene nanobelt by heat treatment.It is received relative to carbon is cut open
The method that mitron or graphene prepare graphene nanobelt, method of the invention are a kind of simple operating process, low cost and can
It is embodied directly in the method that graphene nanobelt is grown on a variety of substrates.This method has following feature and advantage:
1, the present invention discloses one kind for the first time and prepares graphene nano by the organic micro-nano monocrystalline heat treatment of aromatic molecules
The method of band；
2, the present invention discloses for the first time is received by the pattern that change prepares organic micro-nano monocrystalline come controllable preparation graphene
Rice band；
3, method disclosed by the invention enormously simplifies the preparation process of graphene nanobelt compared with traditional method,
And significantly reduce the preparation cost of graphene nanobelt.
4, method disclosed by the invention can use the method for simply controlling linear micro-nano monocrystalline arrangement and realize graphene
The ordered arrangement of nanobelt, it is the method for greatly reducing cost that this, which prepares graphene nanobelt to current realization ordered arrangement,.
Detailed description of the invention
Fig. 1 is the flow chart for preparing graphene nanobelt used in the present invention.
A) the scanning electron microscope diagram for the graphene nanobelt that Fig. 2 is prepared for embodiment 1 and b) Raman figure.
Fig. 3 is the transmission electron microscope figure of graphene nanobelt prepared by embodiment 1, a) is low power transmission electron microscopy
Mirror figure, b) be high resolution transmission electron microscopy, c) it is selective electron diffraction figure.
The scanning electron microscope diagram of the graphene nanobelt grown in the different base that Fig. 4 is prepared for embodiment 2, it is a) golden
Belong to the substrate of silver foil, b) glass substrate, c) mica substrate.
Fig. 5 is the optical microscope of the graphene nanobelt of ordered arrangement in the same direction prepared by embodiment 3.
Fig. 6 is that the concentration in embodiment 4 in 3,4,9,10- tetracarboxylic acid is 6g.ml-1And 13g.ml-1Lower crystal growth 5
The AFM figure of the graphene nanobelt obtained after hour heat treatment.
Fig. 7 is that the concentration in embodiment 4 in 3,4,9,10- tetracarboxylic acid is 6g.ml-1And 13g.ml-1Lower crystal growth 10
The AFM figure of the graphene nanobelt obtained after hour heat treatment.
Specific embodiment
The present invention is further elaborated combined with specific embodiments below, but the present invention is not limited to following embodiments.Institute
State method is conventional method unless otherwise instructed.The raw material can obtain unless otherwise instructed from public commercial source.
The structure of annealing device as used in the following examples is conventional levels tube furnace.
The preparation process of graphene nanobelt is as shown in Figure 1 in the present invention.
Embodiment 1, directly in dielectric base SiO2Graphene nanobelt is prepared on/Si
1) dielectric base SiO is cleaned2/ Si:
It will be with a thickness of 300nm/500 μm of SiO2/ Si substrate successively with volume ratio be 1:20 dish washing liquid solution, acetone,
Ethyl alcohol is respectively cleaned by ultrasonic 3 minutes, is dried with nitrogen；
2) aqueous solution of 3,4,9,10- tetracarboxylic acids of fresh configuration, concentration are 10 μ g.ml-1；
It 3) will be by the clean SiO of step 1) processing2/ Si substrate is placed in the configured solution of step 2), heating
Solution stands growth 5 hours for carrying out monocrystalline, i.e., obtains linear micro-nano monocrystalline in substrate to 40 DEG C；
4) substrate for growing linear micro-nano monocrystalline is taken out, is dried at room temperature；
5) substrate dried in step 4) is put into horizontal pipe furnace, by the central temperature of substrate alignment Electric stove
Area is passed through 100sccm argon gas, after twenty minutes, begins to warm up, and when the temperature in center of electric furnace region reaches 800 DEG C, carries out hot place
Reason 8 minutes；
6) stop heating, maintain the flow velocity of argon gas, horizontal pipe furnace is cooled to room temperature, obtains graphene provided by the invention
Nanobelt.
SEM characterization and Raman characterization difference are as shown in figures 2 a and 2b.Fig. 3 a is to shift the graphene nanobelt in substrate
To the transmission electron microscope picture of micro-grid, Fig. 3 b is the High-Resolution Map of graphene nano belt edge, and Fig. 3 c is the constituency of graphene nanobelt
Electron diffraction diagram.
As seen from the figure, gained graphene nanobelt is the smaller graphene nanobelt composition of multilayer, has polycrystalline structure；
The width of the graphene nanobelt is 80-100nm.
Embodiment 2 prepares graphene nanobelt in a variety of substrates
According to the identical method of embodiment 1, the substrate in step 1) is only become into metallic silver, glass or mica.
Fig. 4 is the electron scanning micrograph for the graphene nanobelt being prepared in three kinds of different bases.
As seen from the figure, graphene nanobelt can be grown on the substrate of multiple performance very different.The graphene is received
The width of rice band is 20-300nm.
Embodiment 3, the graphene nanobelt for preparing ordered arrangement in the same direction
1) aqueous solution of 3,4,9,10- tetracarboxylic acids is configured, concentration is 10 μ g.ml-1；
2) by the configured Solutions Solution of step 1) to 40 DEG C, after standing growth 5 hours that carry out monocrystalline, that is, contained
The liquid system of linear micro-nano monocrystalline；
The liquid system containing linear micro-nano monocrystalline is placed in a clean SiO2In/Si substrate, it is sprawled, controlled
The liquid system is flowed towards same direction, and line can be realized using the active force of monocrystalline and substrate surface in the flow process
Property micro-nano crystal formation ordered arrangement in the same direction.
3) growth obtained by step 2) there is the substrate of the linear micro-nano monocrystalline of ordered arrangement in the same direction to dry in room temperature；
4) substrate for having dried step 3) is put into horizontal pipe furnace, and substrate is aligned to the central temperature area of Electric stove,
It is passed through 100sccm argon gas, after twenty minutes, is begun to warm up, when the temperature in center of electric furnace region reaches 800 DEG C, carries out heat treatment 8
Minute；
5) stop heating, maintain the flow velocity of argon gas, horizontal pipe furnace is cooled to room temperature, obtains graphene provided by the invention
Nanobelt.
Fig. 5 is the photo that the graphene nanobelt of ordered arrangement in the same direction is prepared.
As seen from the figure, the graphene nanobelt of Orienting ordered arrangement may be implemented using the method for the surface treatment.
The time of embodiment 4, the solution concentration by changing crystal growth and crystal growth prepares controllable width and thickness
Graphene nanobelt
According to the identical method of embodiment 1, only the solution concentration of in step 2) 3,4,9,10- tetracarboxylic acids is replaced
It is changed to 6 μ g.ml-1With 13 μ g.ml-1；Replacement step 3) in growth time be 10 hours.
Fig. 6 is 6 μ g.ml for the concentration in 3,4,9,10- tetracarboxylic acid-1With 13 μ g.ml-1Lower crystal growth passes through for 5 hours again
The AFM of the graphene nanobelt obtained after Overheating Treatment schemes.
Fig. 7 is 6 μ g.ml for the concentration in 3,4,9,10- tetracarboxylic acid-1With 13 μ g.ml-1Lower crystal growth 10 hours is again
The AFM of the graphene nanobelt obtained after Overheating Treatment schemes.
As seen from the figure, it can realize that controllable preparation graphene is received by controlling the growth conditions of presoma monocrystal nanowire
Rice band.
Claims (12)
1. a kind of method for preparing graphene nanobelt includes the following steps: that the linear micro-nano monocrystalline that will be dried is heat-treated,
Obtain the graphene nanobelt；
The linear micro-nano monocrystalline of the drying is made by the polycyclic fragrant organic molecule containing carboxyl functional group；
Or, the linear micro-nano monocrystalline of the drying is by with the polycyclic fragrant organic molecule solute containing carboxyl functional group, with water, ethyl alcohol
Solution at least one of methanol for solvent composition is made.
2. according to the method described in claim 1, it is characterized by: the heat treatment includes: by the linear micro-nano of the drying
Monocrystalline is placed in substrate, is heated in inert conditions.
3. according to the method described in claim 2, it is characterized by: the final temperature of heating is 300-1000 in the heating stepses
℃；Soaking time is 3-120min.
4. according to the method described in claim 3, it is characterized by: the final temperature of heating is 800 DEG C in the heating stepses；It protects
The warm time is 8min.
5. according to the method described in claim 2, it is characterized by: the inert conditions are argon gas or nitrogen atmosphere；
The flow velocity of inert gas is 50-300sccm.
6. according to the method described in claim 5, it is characterized by: the flow velocity of inert gas is 100sccm.
7. any method in -6 according to claim 1, it is characterised in that: the linear micro-nano monocrystalline of the drying is by equal benzene
Tetracarboxylic acid, 1,4,5,8 naphthalenetetracarboxylic acid or 3,4,9,10- tetracarboxylic acid are made；
Or, the linear micro-nano monocrystalline of the drying is by with Pyromellitic Acid, Isosorbide-5-Nitrae, 5,8- naphthalenetetracarbacidic acidics or 3,4,9,10- tetramethyls
Acid is solute, is that the solution that solvent forms is made at least one of water, ethyl alcohol and methanol.
8. according to the method described in claim 7, it is characterized by: the linear micro-nano monocrystalline of the drying as follows
(1) or (2) are made:
The method (1) includes: that the growth of monocrystalline is carried out in solution, and growth, which finishes, is cooled to room temperature, is obtained containing linear micro-
It receives the liquid system of monocrystalline, then the liquid system containing linear micro-nano monocrystalline is placed in substrate, dry；
The method (2) includes: that substrate is placed in solution to the growth for carrying out monocrystalline, and growth, which finishes, is cooled to room temperature, is dried.
9. according to the method described in claim 8, it is characterized by: in the method (1) and method (2), the solution it is dense
Degree is 2-50g/ml；
In the growth step of the monocrystalline, temperature is 35-50 DEG C；Time is 1-48h.
10. according to the method described in claim 9, it is characterized by: in the method (1) and method (2), the solution it is dense
Degree is 10g/ml or 6 μ g/ml or 13 μ g/ml；
In the growth step of the monocrystalline, temperature is 40 DEG C；Time is 5-10h.
11. according to the method described in claim 1, it is characterized by: the method also includes having the graphene nano
The step of sequence arranges also is the step of the linear micro-nano monocrystalline is carried out ordered arrangement.
12. according to the method described in claim 8, it is characterized by: the linear micro-nano monocrystalline to be carried out to the step of ordered arrangement
Suddenly it is step a, step b or step c:
Liquid system containing linear micro-nano monocrystalline is placed in substrate after step by the step a in the method (1), institute
Before stating baking step；
The step a is to flow the liquid system containing linear micro-nano monocrystalline in the same direction on the substrate；
Liquid system containing linear micro-nano monocrystalline is being placed in substrate before step by the step b in the method (1)；
The step b is to carry out surface treatment to the substrate or orderly groove is arranged in the substrate surface；
The step c is in the method (2) before the growth step of monocrystalline；
The step c is to carry out surface treatment to the substrate or orderly groove is arranged in the substrate surface.
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| CN103910353A (en) * | 2013-01-08 | 2014-07-09 | 海洋王照明科技股份有限公司 | Preparation method of graphene nanobelts |
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| CN103910353A (en) * | 2013-01-08 | 2014-07-09 | 海洋王照明科技股份有限公司 | Preparation method of graphene nanobelts |
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