CN102502606A - Method for preparing graphene nano holes - Google Patents

Method for preparing graphene nano holes Download PDF

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Publication number
CN102502606A
CN102502606A CN2011103532158A CN201110353215A CN102502606A CN 102502606 A CN102502606 A CN 102502606A CN 2011103532158 A CN2011103532158 A CN 2011103532158A CN 201110353215 A CN201110353215 A CN 201110353215A CN 102502606 A CN102502606 A CN 102502606A
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China
Prior art keywords
graphene
nanometers
graphene nano
nano holes
hole
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Pending
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CN2011103532158A
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Chinese (zh)
Inventor
尹奎波
徐涛
孙立涛
徐峰
贺龙兵
谢骁
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Southeast University
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Southeast University
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Publication date
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Priority to CN2011103532158A priority Critical patent/CN102502606A/en
Publication of CN102502606A publication Critical patent/CN102502606A/en
Pending legal-status Critical Current

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Abstract

The invention discloses a method for preparing graphene nano holes. The method comprises the following steps of: bombarding the surface of graphene by adopting high-energy convergent electron beams to obtain nano holes with large size, heating the graphene nano holes to the temperature of between 200 and 1,300 DEG C in a certain atmosphere under certain pressure, preserving the heat for 10 to 500 minutes, and thus reducing the aperture of the nano holes to be below 5 nanometers. By the method, the graphene holes of below 5 nanometers can be conveniently prepared, the preparation success rate can be greatly improved, and the preparation cost is reduced.

Description

The preparation method in a kind of graphene nano hole
Technical field:
Patent of the present invention relates to the preparation method in a kind of graphene nano hole, belongs to nano-device and makes the field.
Background technology:
Graphene is a kind of new carbon with bi-dimensional cellular shape structure that is formed by the monolayer carbon atom packing; Have excellent mechanical property, electric property; Can be used for preparing the carbon crystal pipe, simultaneously, Graphene has high specific surface area; Can be used as the solid support material of catalyzer, thereby have broad application prospects.
The fluid device of receiving based on the solid nano hole is considered to the basis of third generation dna sequencing; The antetype device of fluidic transmitter received is used to detect the single DNA base pair; Its principle of work is to adopt nanoporous dielectric to connect two fluid pool unit, applies voltage along the nanoporous length direction and produces ion(ic)current, when dna molecular through nanoporous the time; Because the obstruction of dna molecular will cause the faint variation of electric current; Through measuring the numerical value of electric current, can judge position and the space structure of dna molecular at passage, this antetype device can be used for dna sequencing and drug screening.
Graphene is owing to have thin thickness, high physical strength, and very compound dna sequencing is with the requirement of nanoporous.For guaranteeing high order-checking accuracy, the diameter of nanoporous requires less than 5 nanometers, but present technology of preparing and imperfection about the graphene nano hole.Applied Physics Letters 93,113107 (2008) discloses the preparation method in a kind of graphene nano hole, in transmission electron microscope, utilizes high energy to assemble the beam bombardment Graphene and has obtained the graphene nano hole; Pore size is by the decision of beam spot diameter, and nanoporous machines its aperture, back and can't dwindle, if the diameter of initial nanoporous surpasses 5 nanometers; The resolving power of so whole antetype device can descend a lot; If prepare a duct again less than 5 nanometers, need antetype device be handled, spread a new graphene film again; Operation is loaded down with trivial details, and wastes huge.
Summary of the invention:
In order to solve the adjusting problem of graphene nano hole dimension, the invention provides the preparation method in a kind of graphene nano hole, to obtain the graphene nano hole dimension adjustable.
The preparation method in a kind of graphene nano hole, concrete steps are:
The first step places on the carrier platform Graphene is unsettled, then the carrier platform is positioned in the transmission electron microscope;
Second step, 0-1300 ℃, be incubated 10-500 minute, originally the hole greater than 5 nanometers is contracted in 5 nanometers.
Described protection gas is any one in air, argon gas, nitrogen, hydrogen, methane, acetylene, the ethanol.
Beneficial effect:
Can the nanoporous greater than 5 nanometers be narrowed down to the aperture, thereby satisfy the requirement of high precision dna sequencing, increase substantially the power that is prepared into of antetype device less than 5 nanometers.
Description of drawings
Fig. 1 is the transmission electron microscope figure in the graphene nano hole of aperture 10 nanometers that obtain of the present invention;
Fig. 2 is the transmission electron microscope in the graphene nano hole of later aperture 2 nanometers of the shrinkage cavity that obtains of the present invention.
Embodiment
The preparation method in a kind of graphene nano hole, concrete steps are:
The first step places on the carrier platform Graphene is unsettled, owing to be empty in the middle of the carrier platform, Graphene is a slice film, so this sheet film is covered the empty zone of carrier platform, has just formed unsettledly, then the carrier platform is positioned in the transmission electron microscope; The surface of described carrier platform can be SiN or Cu grid.
In second step, utilize and assemble high-power electron beam obtains the 5-20 nanometer in the bombardment of Graphene surface nanoporous;
In the 3rd step, the graphene nano hole is being protected under the gas shiled 1 * 10 5-1 * 10 -6Under the pressure of Pa sample temperature is elevated to 200-1300 ℃, is incubated 10-500 minute, originally the hole greater than 5 nanometers is contracted in 5 nanometers.
Described protection gas is any one in air, argon gas, nitrogen, hydrogen, methane, acetylene, the ethanol.
Embodiment 1.
The unsettled Cu of carrier platform that places is online with Graphene, then the carrier platform is positioned in the transmission electron microscope;
Utilize under the room temperature and assemble high-power electron beam obtains 10 nanometers in the bombardment of Graphene surface nanoporous;
With the graphene nano hole 10 -6Be heated to 500 ℃ in the Pa vacuum, be incubated the graphene nano hole that obtains aperture 2 nanometers after 30 minutes.Correlated results is seen Fig. 1 and the Fig. 2 in the accompanying drawing.
Fig. 1 is the transmission electron microscope figure in the graphene nano hole of aperture 10 nanometers that obtain under the original state;
Fig. 2 is the transmission electron microscope figure in the graphene nano hole of aperture 2 nanometers that obtain after the thermal treatment.
Embodiment 2.
Place on the carrier platform SiN substrate Graphene is unsettled, then the carrier platform is positioned in the transmission electron microscope;
At 400 ℃ of nanoporouss that utilize the convergence high-power electron beam to obtain 6 nanometers in the bombardment of Graphene surface down;
With the graphene nano hole in hydrogen atmosphere 10 5Be heated to 1300 ℃ under the Pa air pressure, be incubated the graphene nano hole that obtains aperture 3.2 nanometers after 100 minutes.
Embodiment 3.
Place on the Cu substrate Graphene is unsettled, then carrier is positioned in the transmission electron microscope;
Utilize under the room temperature and assemble high-power electron beam obtains 20 nanometers in the bombardment of Graphene surface nanoporous;
The graphene nano hole is heated to 200 ℃ under the 1Pa air pressure in methane atmosphere, is incubated the graphene nano hole that obtains aperture 4.3 nanometers after 500 minutes.

Claims (2)

1. the preparation method in a graphene nano hole is characterized in that, concrete steps are:
The first step places on the carrier platform Graphene is unsettled, then the carrier platform is positioned in the transmission electron microscope;
In second step, utilize and assemble high-power electron beam obtains the 5-20 nanometer in the bombardment of Graphene surface nanoporous;
In the 3rd step, the graphene nano hole is being protected under the gas shiled 1 * 10 5-1 * 10 -6Under the pressure of Pa sample temperature is elevated to 200-1300 ℃, is incubated 10-500 minute, originally the hole greater than 5 nanometers is contracted in 5 nanometers.
2. the preparation method in a kind of graphene nano as claimed in claim 1 hole is characterized in that, described protection gas is any one in air, argon gas, nitrogen, hydrogen, methane, acetylene, the ethanol.
CN2011103532158A 2011-11-10 2011-11-10 Method for preparing graphene nano holes Pending CN102502606A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103224232A (en) * 2013-04-23 2013-07-31 北京大学 Preparation method of graphite nanometer hole
CN106517174A (en) * 2016-11-25 2017-03-22 西安交通大学 Quick heating method for graphene and deep processing method based on same
CN109811046A (en) * 2019-01-18 2019-05-28 广东工业大学 A kind of three layers of nano-pore structure and the preparation method and application thereof that size is controllable
CN111153380A (en) * 2019-12-23 2020-05-15 华东师范大学 Preparation method of metal type chromium ditelluride nano-pores with controllable pore size
CN113198840A (en) * 2021-04-22 2021-08-03 武汉大学 Method for preparing graphene from carbon nano tube and application of graphene

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102115069A (en) * 2010-12-20 2011-07-06 中国石油大学(北京) Graphene with porous structure and preparation method of graphene
CN102169105A (en) * 2010-12-22 2011-08-31 东南大学 Graphene-based nano-pore monomolecular sensor and medium identification method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102115069A (en) * 2010-12-20 2011-07-06 中国石油大学(北京) Graphene with porous structure and preparation method of graphene
CN102169105A (en) * 2010-12-22 2011-08-31 东南大学 Graphene-based nano-pore monomolecular sensor and medium identification method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
BO SONG ET AL: "Atomic-Scale Electron-Beam Sculpting of Near-Defect-Free Graphene Nanostructures", 《NANO LETTERS》 *

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103224232A (en) * 2013-04-23 2013-07-31 北京大学 Preparation method of graphite nanometer hole
CN103224232B (en) * 2013-04-23 2015-02-11 北京大学 Preparation method of graphite nanometer hole
CN106517174A (en) * 2016-11-25 2017-03-22 西安交通大学 Quick heating method for graphene and deep processing method based on same
CN106517174B (en) * 2016-11-25 2019-04-12 西安交通大学 A kind of quick heating means of graphene and the deep working method based on it
CN109811046A (en) * 2019-01-18 2019-05-28 广东工业大学 A kind of three layers of nano-pore structure and the preparation method and application thereof that size is controllable
CN111153380A (en) * 2019-12-23 2020-05-15 华东师范大学 Preparation method of metal type chromium ditelluride nano-pores with controllable pore size
CN113198840A (en) * 2021-04-22 2021-08-03 武汉大学 Method for preparing graphene from carbon nano tube and application of graphene

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Application publication date: 20120620