CN106185897A - A kind of controlled method preparing graphene nanobelt in multiple substrate - Google Patents
A kind of controlled method preparing graphene nanobelt in multiple substrate Download PDFInfo
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Abstract
The invention discloses a kind of controlled method preparing graphene nanobelt in multiple substrate.The method includes: dry linear micro-nano monocrystalline is carried out heat treatment, obtains described graphene nanobelt.The present invention discloses a kind of method preparing graphene nanobelt by aromatic molecules organic micro-nano monocrystalline heat treatment for the first time；Disclose for the first time by changing that pattern prepare organic micro-nano monocrystalline is controlled prepares graphene nanobelt；The method, compared with traditional method, enormously simplify the preparation process of graphene nanobelt, and significantly reduces the preparation cost of graphene nanobelt.The method can utilize the simple method controlling the arrangement of linear micro-nano monocrystalline to realize the ordered arrangement of graphene nanobelt, and this is the method greatly reducing cost to realize ordered arrangement at present preparing graphene nanobelt.
Description
Technical field
The invention belongs to graphene nanobelt preparation field, relate to a kind of controlled in multiple substrate preparing graphene nano
The method of band.
Background technology
Graphene has the character 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.).But zero band gap properties pole of Graphene
The earth limits its application in microelectronic component.How to open and control the band gap of Graphene and become Graphene electronics
One key scientific problems of application.It is that one preferably opens graphite that two-dimensional graphene is cut into quasi-one-dimensional nanoribbons
The method of alkene band gap.This one-dimensional c-based nanomaterial of novel standard is carried out theoretical widely and experimentation, has found it
There is the physical and chemical performance of excellence, be expected on nanoelectronics device, obtain wide application ((a) Son, Y.-W.；
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 CNT (CNTs) phase closely
Close, be all quasi-one-dimentional structure, be therefore similar to the classification of CNTs, the different topology shape having according to GNRs edge carbon atom
Shape, it is possible to be classified as armchair graphene nanobelt (AGNRs) and sawtooth pattern graphene nanobelt (ZGNRs).According to stone
In ink alkene nano belt, the bar number of carbon atom chain can define width Na (Fujita, the M. of nano belt；Wakabayashi,K.；
Nakada,K.；Kusakabe,K.J.Phys.Soc.Jpn.1996,65,1920.).GNRs is by its special edge effect and width
The impact of degree, and there is electrical properties flexibly, the origin of the band gap of the GNRs of different boundary is entirely different, the band gap of AGNRs
Originate from quantum confinement and rely on the width of nano belt.The band gap of ZGNRs comes from the localization edge electromotive force that edge magneticization produces.Band
The opening of gap makes it be expected at aspects such as quantum device transistors will to have a wide range of applications.Research shows that the energy gap of GNRs can be with
The change of nano belt width and change, wherein Na=20AGNRs occurs in that band gap, demonstrates semiconductor property, and the widest
The metal that ZGNRs is zero band gap of degree, and it occurs in that the marginality of local at fermi level.When the band gap of GNRs is opened,
Bigger room temperature switch ratio can be realized, such that it is able to prepare the field-effect transistor of high mobility and on-off ratio.Due to stone
Ink alkene and the tempting physical property of derivant thereof and using value potential in nanoelectronics, for research low dimensional physics phenomenon
Provide a good opportunity.
The preparation method of GNRs can be largely classified into two big classes according to forming types, is respectively the most from bottom to top and from upper
Under.Prepare from top to bottom GNRs typically refer to raw material as Graphene or CNT by photoetching process, micromechanics stripping method,
The method such as etching method, oxidizing process obtains.Usual preparation process is more complicated and the controllability on border is relatively low, the GNRs knot obtained
Structure is also and heterogeneity, greatly impact obtain the electric property of GNRs.Therefore, the most many seminars begin one's study from bottom to top
Method, generally include chemical vapour deposition technique, solution is combined to, synthesis etc. is assisted in metal surface.And chemical gaseous phase deposition side
Method has isotropism due to substrate, is therefore difficult to prepare one-dimensional GNRs, needs to introduce some templates or metal kind
Son, the graphene nanobelt obtained is of low quality or is limited to structure ((a) Sokolov, the A.N. of template；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.).Organic synthesis method the most from bottom to top (includes that solution is combined to and gold
Metal surface assists synthesis) gradually get growing concern for, it can reach atomic level to the controllability of edge and width.
But the nano belt size that the synthesis of solution phase obtains is extremely limited, and often size is smaller.And metal surface is assisted
Synthesis needs to carry out on monocrystalline noble metal ((a) Zhang, H.；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 harsher, and need to prepare the device of graphene nanobelt by transfer in later stage application process.This
Method is more complicated by process, in order to the requirement of instrument is higher needed for obtaining narrow GNRs, has pole for industrialized utilization
Big difficulty.Multiple and/or dielectric base is directly prepared Graphene and is still a great challenge, and low cost at present
And be hopeful industrialization graphene nanobelt preparation method the most also need explore.
Summary of the invention
It is an object of the invention to provide a kind of controlled method preparing graphene nanobelt in multiple substrate.
The method preparing graphene nanobelt that the present invention provides, comprises the steps: dry linear micro-nano monocrystalline
Carry out heat treatment, obtain described graphene nanobelt.
The heat treatment of said method includes: be placed in substrate, in inert conditions by described dry linear micro-nano monocrystalline
Heating.
In described heating steps, the final temperature of heating is 300-1000 DEG C or 800 DEG C；Temperature retention time be 3-120min or
8min。
Described inert conditions is argon or nitrogen atmosphere；
The flow velocity of noble gas is 50-300sccm or 100sccm.
In this step, the length of graphene nanobelt, thickness and width and the relevant parameter of gained linear micro-nano monocrystalline
It is closely related, and structure also temperature and time with heat treatment is closely related, by changing the growth conditions of linear micro-nano monocrystalline
With the controlled preparation that the condition of heat treatment can realize graphene nanobelt.
Described dry linear micro-nano monocrystalline by containing carboxyl functional group multi-ring fragrance organic molecule, Pyromellitic Acid, 1,
4,5,8-naphthalenetetracarbacidic acidic or 3,4,9,10-tetracarboxylic acid prepare；
Or, described dry linear micro-nano monocrystalline is by with multi-ring fragrance organic molecule, the equal benzene tetramethyl containing carboxyl functional group
Acid, Isosorbide-5-Nitrae, 5,8-naphthalenetetracarbacidic acidics or 3,4,9,10-tetracarboxylic acids are solute, with at least one in water, ethanol and methanol for molten
The solution of agent composition prepares.
In this step, the multi-ring fragrance organic molecule containing carboxyl functional group as solute in a solvent can be with self assembly
Form linear micro-nano monocrystalline；Length, width and the thickness of this linear micro-nano monocrystalline can pass through solution concentration and growth time control
System；
More specifically, described dry linear micro-nano monocrystalline (1) as follows or (2) prepare:
Described method (1) including: carries out the growth of monocrystalline in solution, grows and complete is cooled to room temperature, obtains containing wired
Property micro-nano monocrystalline liquid system, the more described liquid system containing linear micro-nano monocrystalline is placed in substrate, dries；
Described method (2) including: substrate is placed in solution the growth carrying out monocrystalline, grows the complete room temperature that is cooled to, and dries
Dry.
In described method (1) and method (2), the concentration of described solution is 2-50g.ml-1Or 10g.ml-1Or 6 μ g.ml-1Or
13μg.ml-1；
In the growth step of described monocrystalline, temperature is 35-50 DEG C or 40 DEG C；Time is 1-48h or 5h or 10h or 5-10h.
Described method also includes the step making described graphene nanobelt ordered arrangement, also will described linear micro-nano monocrystalline
Carry out the step of ordered arrangement；
The described step making linear micro-nano monocrystalline ordered arrangement is following steps a, step b or step c.
Concrete, described step a will be placed in substrate containing the liquid system of linear micro-nano monocrystalline in described method (1)
After step, before described baking step；
Described step a is to make the described liquid system containing linear micro-nano monocrystalline flow the most in the same direction
Dynamic；
Described step b will be placed in step in substrate containing the liquid system of linear micro-nano monocrystalline in described method (1)
Before；
Described step b is for carry out surface process to described substrate；
Described step c is in described method (2) before the growth step of monocrystalline；
Described step c is for carry out surface process to described substrate.
Various conventional surface treatment methods are the most applicable, as referred to Review literature Controlled Deposition of
Crystalline Organic Semiconductors for Field-Effect-Transistor Applications。
Concrete, it can be to arrange orderly groove at described substrate surface that described surface processes.
In said method, substrate used is all insoluble in solvent for use；Be chosen in particular from metal, dielectric base, plastics, glass or
Muscovitum.Can be more specifically SiO2/ Si substrate or SERS substrate.The most concretely thickness is the SiO of 300nm/500 μm2/ Si substrate.Institute
The thickness stating substrate is the most adjustable.For metallic substrates, also can be first in reducibility gas is such as hydrogen by it according to routine operation
Annealing.
It addition, the graphene nanobelt prepared according to the method described above, fall within protection scope of the present invention；Wherein,
The width of described graphene nanobelt is specially 20-300nm, can be more specifically 80-100nm.
The method preparing graphene nanobelt that the present invention provides, the method utilizes multi-ring aromatic molecules by self assembly shape
Linear micro-nano monocrystalline, then makes linear micro-nano single crystal transition be graphene nanobelt by heat treatment.Receive relative to cutting open carbon
Mitron or Graphene prepare the method for graphene nanobelt, and the method for the present invention is that a kind of operating process is simple, low cost and can
The method being embodied directly in multiple Grown graphene nanobelt.The method has following feature and advantage:
1, the present invention discloses for the first time and a kind of prepares graphene nano by aromatic molecules organic micro-nano monocrystalline heat treatment
The method of band；
2, the present invention discloses for the first time and receives by changing the controlled Graphene of preparing of pattern prepare organic micro-nano monocrystalline
Rice band；
3, method disclosed by the invention, compared with traditional method, enormously simplify the preparation process of graphene nanobelt,
And significantly reduce the preparation cost of graphene nanobelt.
4, method disclosed by the invention, it is possible to use the simple method controlling the arrangement of linear micro-nano monocrystalline realizes Graphene
The ordered arrangement of nano belt, this is the method greatly reducing cost to realize ordered arrangement at present preparing graphene nanobelt.
Accompanying drawing explanation
Fig. 1 is the flow chart preparing graphene nanobelt used by the present invention.
Fig. 2 is a) scanning electron microscope diagram of graphene nanobelt and b) the Raman figure of embodiment 1 preparation.
Fig. 3 is the transmission electron microscope figure of the graphene nanobelt of embodiment 1 preparation, a) is low power transmission electron microscopy
Mirror figure, b) is high resolution transmission electron microscopy, c) is SEAD figure.
Fig. 4 is the scanning electron microscope diagram of the graphene nanobelt of growth in the different base of embodiment 2 preparation, a) gold
Belong to the substrate of native silver, b) glass substrate, c) mica substrate.
Fig. 5 is the optical microscope of the graphene nanobelt of the ordered arrangement in the same direction of embodiment 3 preparation.
Fig. 6 be the concentration in embodiment 4 at 3,4,9,10-tetracarboxylic acid be 6g.ml-1And 13g.ml-1Lower crystal growth 5
The AFM figure of the graphene nanobelt obtained after hour heat treatment.
Fig. 7 be the concentration in embodiment 4 at 3,4,9,10-tetracarboxylic acid be 6g.ml-1And 13g.ml-1Lower crystal growth 10
The AFM figure of the graphene nanobelt obtained after hour heat treatment.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is further elaborated, but the present invention is not limited to following example.Institute
Method of stating is conventional method if no special instructions.Described raw material the most all can be either commercially available from open.
The structure of annealing device used in following embodiment is conventional levels tube furnace.
In the present invention, the preparation process of graphene nanobelt is as shown in Figure 1.
Embodiment 1, directly in dielectric base SiO2Graphene nanobelt is prepared on/Si
1) dielectric base SiO is cleaned2/ Si:
By the SiO that thickness is 300nm/500 μm2/ Si substrate successively with the liquid detergent solution that volume ratio is 1:20, acetone,
The each ultrasonic cleaning of ethanol 3 minutes, nitrogen dries up；
2) fresh configuration 3,4,9,10-tetramethyl aqueous acid, concentration is 10 μ g.ml-1；
3) will be through step 1) the clean SiO that processes2/ Si substrate is placed on step 2) in the solution that configured, heating
Solution, to 40 DEG C, stands the growth 5 hours carrying out monocrystalline, i.e. obtains linear micro-nano monocrystalline in substrate；
4) take out the substrate of the linear micro-nano monocrystalline of growth, dry at ambient temperature；
5) by step 4) in the substrate dried put in horizontal pipe furnace, substrate is directed at the central temperature of Electric stove
District, is passed through 100sccm argon, after 20 minutes, begins to warm up, and when the temperature in center of electric furnace region reaches 800 DEG C, carries out at heat
Manage 8 minutes；
6) stopping heating, maintain the flow velocity of argon, horizontal pipe furnace is cooled to room temperature, obtains the Graphene that the present invention provides
Nano belt.
SEM characterizes and Raman characterizes the most as shown in figures 2 a and 2b.Fig. 3 a is for shift suprabasil graphene nanobelt
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
Electronogram.
As seen from the figure, gained graphene nanobelt is the graphene nanobelt composition that multilamellar is less, has the structure of polycrystalline；
The width of this graphene nanobelt is 80-100nm.
Embodiment 2, in multiple substrate, prepare graphene nanobelt
According to method identical with embodiment 1, only by step 1) in substrate become argent, glass or Muscovitum.
Fig. 4 is the electron scanning micrograph preparing the graphene nanobelt in three kinds of different base.
As seen from the figure, the substrate of multiple performance very different can grow graphene nanobelt.This Graphene is received
The width of rice band is 20-300nm.
Embodiment 3, prepare the graphene nanobelt of ordered arrangement in the same direction
1) configuration 3,4,9,10-tetramethyl aqueous acids, concentration is 10 μ g.ml-1；
2) by step 1) Solutions Solution that configured to 40 DEG C, after standing the growth 5 hours carrying out monocrystalline, i.e. obtain and contain
The liquid system of linear micro-nano monocrystalline；
This liquid system containing linear micro-nano monocrystalline is placed in the SiO of a cleaning2In/Si substrate so that it is sprawl, control
This liquid system flows towards same direction, utilizes monocrystalline can realize line with the active force of substrate surface in this flow process
Property micro-nano crystal formation ordered arrangement in the same direction.
3) by step 2) gained growth has the substrate of the linear micro-nano monocrystalline of ordered arrangement in the same direction to dry in room temperature；
4) by step 3) substrate dried puts in horizontal pipe furnace, and substrate is directed at the central temperature district of Electric stove,
It is passed through 100sccm argon, after 20 minutes, begins to warm up, when the temperature in center of electric furnace region reaches 800 DEG C, carry out heat treatment 8
Minute；
5) stopping heating, maintain the flow velocity of argon, horizontal pipe furnace is cooled to room temperature, obtains the Graphene that the present invention provides
Nano belt.
Fig. 5 is the photo preparing the graphene nanobelt of ordered arrangement in the same direction.
As seen from the figure, the method utilizing this surface to process can realize the graphene nanobelt of Orienting ordered arrangement.
Embodiment 4, prepare controllable width and thickness by changing the time of the solution concentration of crystal growth and crystal growth
Graphene nanobelt
According to method identical with embodiment 1, only by step 2) in the solution concentration of 3,4,9,10-tetracarboxylic acids replace
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 to be 6 μ g.ml in the concentration of 3,4,9,10-tetracarboxylic acid-1With 13 μ g.ml-1Lower crystal growth 5 hours warp again
The AFM figure of the graphene nanobelt obtained after Overheating Treatment.
Fig. 7 is to be 6 μ g.ml in the concentration of 3,4,9,10-tetracarboxylic acid-1With 13 μ g.ml-1Lower crystal growth 10 hours is again
The AFM figure of the graphene nanobelt obtained after Overheating Treatment.
As seen from the figure, controlled Graphene of preparing can be realized by the growth conditions of control presoma monocrystal nanowire to receive
Rice band.
Claims (10)
1. the method preparing graphene nanobelt, comprises the steps: dry linear micro-nano monocrystalline is carried out heat treatment,
Obtain described graphene nanobelt.
Method the most according to claim 1, it is characterised in that: described heat treatment includes: by described dry linear micro-nano
Monocrystalline is placed in substrate, heats in inert conditions.
Method the most according to claim 2, it is characterised in that: in described heating steps, the final temperature of heating is 300-1000
DEG C or 800 DEG C；Temperature retention time is 3-120min or 8min.
The most according to the method in claim 2 or 3, it is characterised in that: described inert conditions is argon or nitrogen atmosphere；
The flow velocity of noble gas is 50-300sccm or 100sccm.
5. according to described method arbitrary in claim 1-4, it is characterised in that: described dry linear micro-nano monocrystalline is by containing carboxylic
Multi-ring fragrance organic molecule, Pyromellitic Acid, 1,4,5,8 naphthalenetetracarboxylic acid or the 3,4,9,10-tetramethyl processed with acid of base functional group
?；
Or, described dry linear micro-nano monocrystalline by with containing carboxyl functional group multi-ring fragrance organic molecule, Pyromellitic Acid, 1,
4,5,8-naphthalenetetracarbacidic acidics or 3,4,9,10-tetracarboxylic acids are solute, form with at least one in water, ethanol and methanol for solvent
Solution prepare.
Method the most according to claim 5, it is characterised in that: described dry linear micro-nano monocrystalline is as follows
(1) or (2) prepare:
Described method (1) including: carries out the growth of monocrystalline in solution, grows and complete is cooled to room temperature, obtains containing linear micro-
Receive the liquid system of monocrystalline, the more described liquid system containing linear micro-nano monocrystalline is placed in substrate, dry；
Described method (2) including: substrate is placed in solution the growth carrying out monocrystalline, grows the complete room temperature that is cooled to, and dries.
Method the most according to claim 6, it is characterised in that: in described method (1) and method (2), described solution dense
Degree is 2-50g.ml-1Or 10g.ml-1Or 6 μ g.ml-1Or 13 μ g.ml-1；
In the growth step of described monocrystalline, temperature is 35-50 DEG C or 40 DEG C；Time is 1-48h or 5h or 10h or 5-10h.
8. according to described method arbitrary in claim 1-7, it is characterised in that: described method also includes making described Graphene receive
The step of rice band ordered arrangement, also will carry out the step of ordered arrangement by described linear micro-nano monocrystalline.
Method the most according to claim 8, it is characterised in that: described linear micro-nano monocrystalline is carried out the step of ordered arrangement
For step a, step b or step c:
Described step a will be placed in substrate after step containing the liquid system of linear micro-nano monocrystalline in described method (1), institute
Before stating baking step；
Described step a is to make the described liquid system containing linear micro-nano monocrystalline flow the most in the same direction；
Liquid system containing linear micro-nano monocrystalline is being placed in substrate before step in described method (1) by described step b；
Described step b for carrying out surface process or arranging orderly groove at described substrate surface to described substrate；
Described step c is in described method (2) before the growth step of monocrystalline；
Described step c for carrying out surface process or arranging orderly groove at described substrate surface to described substrate.
10. the graphene nanobelt that the arbitrary described method of claim 1-9 prepares；
The width of described graphene nanobelt is specially 20-300nm.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112694084A (en) * | 2020-12-11 | 2021-04-23 | 上海交通大学 | Graphene nanoribbon device array and preparation system and preparation method thereof |
| CN113104843A (en) * | 2021-04-20 | 2021-07-13 | 雷索新材料(苏州)有限公司 | Graphene and preparation method thereof |
| WO2023045453A1 (en) * | 2021-09-22 | 2023-03-30 | 广东墨睿科技有限公司 | Method for high clean and non-destructive transfer of graphene nanoribbon |
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