CN105668503A - Preparation method of metal-assisted two-dimensional material nanoribbon - Google Patents

Preparation method of metal-assisted two-dimensional material nanoribbon Download PDF

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CN105668503A
CN105668503A CN201610137385.5A CN201610137385A CN105668503A CN 105668503 A CN105668503 A CN 105668503A CN 201610137385 A CN201610137385 A CN 201610137385A CN 105668503 A CN105668503 A CN 105668503A
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metal
dimensional material
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CN105668503B (en
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王紫东
傅云义
贾越辉
龚欣
彭沛
田仲政
任黎明
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Peking University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B81MICROSTRUCTURAL TECHNOLOGY
    • B81BMICROSTRUCTURAL DEVICES OR SYSTEMS, e.g. MICROMECHANICAL DEVICES
    • B81B7/00Microstructural systems; Auxiliary parts of microstructural devices or systems
    • B81B7/02Microstructural systems; Auxiliary parts of microstructural devices or systems containing distinct electrical or optical devices of particular relevance for their function, e.g. microelectro-mechanical systems [MEMS]
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B81MICROSTRUCTURAL TECHNOLOGY
    • B81CPROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
    • B81C1/00Manufacture or treatment of devices or systems in or on a substrate
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B81MICROSTRUCTURAL TECHNOLOGY
    • B81CPROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
    • B81C1/00Manufacture or treatment of devices or systems in or on a substrate
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B81MICROSTRUCTURAL TECHNOLOGY
    • B81CPROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
    • B81C1/00Manufacture or treatment of devices or systems in or on a substrate
    • B81C1/00388Etch mask forming
    • B81C1/00404Mask characterised by its size, orientation or shape
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B81MICROSTRUCTURAL TECHNOLOGY
    • B81CPROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
    • B81C1/00Manufacture or treatment of devices or systems in or on a substrate
    • B81C1/00436Shaping materials, i.e. techniques for structuring the substrate or the layers on the substrate
    • B81C1/00523Etching material
    • B81C1/00531Dry etching
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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    • B81C2201/01Manufacture or treatment of microstructural devices or systems in or on a substrate
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B81MICROSTRUCTURAL TECHNOLOGY
    • B81CPROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
    • B81C2201/00Manufacture or treatment of microstructural devices or systems
    • B81C2201/01Manufacture or treatment of microstructural devices or systems in or on a substrate
    • B81C2201/0198Manufacture or treatment of microstructural devices or systems in or on a substrate for making a masking layer

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Abstract

The invention discloses a preparation method of a metal-assisted two-dimensional material nanoribbon. According to the method, the rectangular metal-two-dimensional material double-layer nanostructure is prepared with the help of metal, and therefore nano rolls of the metal-two-dimensional material are formed at the edges of the nanostructure; the width of the nano rolls can be generally 100 nm or below, and the two-dimensional material nanoribbon with the width of 30-80 nm can be finally prepared by repeatedly using the methods of plasma etching and wet metal dissolving. Compared with other techniques for preparing the two-dimensional material nanoribbon, the preparation method has the advantages that a high-precision electron beam exposure machine does not need to be used, and the prepared two-dimensional material nanoribbon is controllable in position.

Description

A kind of preparation method of the two-dimensional material nano belt assisted by metal
Technical field
The invention belongs to micro/nano-scale device arts, the preparation method being specifically related to a kind of two-dimensional material nano belt assisted by metal.
Background technology
Two-dimensional material (2DM), because possessing the performance of some excellences, has a wide range of applications in radio frequency electronics, logic electronics device, photoelectricity or the field such as luminescent device, flexible circuit. For being etched to the two-dimensional material of definite shape, if applying stress in its edge, then its edge often tends to form the less stable space form of energy, i.e. frizz. The width of these frizzs can be low to moderate below 100nm, and this width is suitable with the width of two-dimensional material nano belt. Two-dimensional material nano belt has the character different from large-area two-dimensional material, as: large area single-layer graphene is absent from energy band band gap, and its nano belt then can have certain band gap. At present, the method preparing two-dimensional material nano belt mainly has: E-beam lithography, ultrasonic centrifuging, Chemical self-assembly method, CNT slide fastener method etc.
Summary of the invention
It is an object of the invention to the preparation method proposing a kind of two-dimensional material nano belt assisted by metal.
The preparation method of the two-dimensional material nano belt that the present invention proposes, the key step comprised is as follows:
1) select suitable substrate, in its superficial growth two-dimensional material, two-dimensional material is transferred in dielectric substrate.
Substrate owing to growing needed for different two-dimensional material is different, so needing the transfer method adopted also different:
A) substrate for wet etching method can be used to dissolve, uses wet method transfer method to transfer them in dielectric substrate, it may be assumed that use the organic polymer being soluble in acetone and other organic solvent as support membrane, two-dimensional material is transferred to insulated substrate surface;
B) substrate for wet etching method cannot be used to dissolve, dry method transfer method then can only be used to shift, that is: use there is certain degree of hardness, be not susceptible to too large deformation, the organic polymer that is soluble in acetone and other organic solvent is as support membrane, two-dimensional material is taken off from former substrate, and transfers to insulated substrate surface; The dielectric substrate used can be integral insulation material, it is also possible to simply have insulating barrier at substrate surface.
2) in above-mentioned two-dimensional material, select suitable position, be etched into rectangle two-dimensional material.Can be prepared by focused ion bundle, it is also possible to utilize the method for common photoetching and etching to obtain. Subsequently at sample surfaces spin coating photoresist, using the method for photoetching to be removed by the photoresist of the surface on two-dimensional material surface, the figure of the photoresist window of formation and size and rectangle two-dimensional material are completely the same, such as Fig. 1. Use thermal evaporation at the sample surfaces relatively thin metal (2~8nm) of deposit, then obtain metal/2DM double-layer nanostructured of rectangle. After thermal evaporation, the short side edge double-layer nanostructured for metal/2DM of rectangle will form the nanometer roll of metal/2DM. Finally, whole sample is soaked in acetone, and use stripping technology to be removed by the excess metal above photoresist. To the nano-band array that production site is controlled, then need to make the double-layer nanostructured array of corresponding rectangular metal/2DM, such as Fig. 2.
The reason of the formation of the nanometer roll of metal/2DM is as follows: photoresist be exposed after edge tool present structure wide at the top and narrow at the bottom, the metal then deposited can in photoresist edge natural separation, then metal/the 2DM defining rectangle is double-layer nanostructured. After thermal evaporation, cavity inner temperature declines, and there is larger difference in the thermal coefficient of expansion of two-dimensional material and metal, then bigger shrinkage stress is produced in edge, the last double-layer nanostructured edge of metal/2DM is by forming curling release stress, form the nanometer roll of metal/2DM, and spatially present 2DM/ metal/2DM ... and the structure spaced apart of metal/2DM, such as Fig. 3.
The length of long sides of rectangle is designated as a, and length of short sides is designated as b, in order to ensure that in subsequent step, the nanometer roll of metal/2DM is formed relatively easily, and the nanometer roll of this metal/2DM always minor face place formed, this rectangle need to meet following condition: b≤4 μm andIf the rectangle length of side is relatively big, then the shrinkage stress that metal produces in contraction process is then not enough so that the double-layer nanostructured edge of metal/2DM occurs curling; If the long limit of rectangle and minor face are more or less the same, then cannot ensure that the nanometer roll of metal/2DM is always formed at short side edge place, with regard to the position that uncontrollable metal/2DM nanometer roll produces.
The metal used should have bigger thermal coefficient of expansion, it is possible to is ferrum, nickel, palladium, gold, copper, silver, antimony, aluminum, bismuth, magnesium or zinc etc.
3) use plasma fully to etch and be positioned at outermost two-dimensional material, then outermost material become virgin metal/2DM double-layer nanostructured in metal:
Suitable plasma should be selected according to two-dimensional material kind, generally use O2Plasma but it also may be CHF3、XeF2、Cl2, the gas such as Ar plasma.
Due to metal/2DM double-layer nanostructured in metal relatively thin, do not damage metal to effectively etch two-dimensional material, the relevant parameter that plasma etching uses should control in suitable scope: RIE power PRIERange for 5~100W; ICP power PICPRange for 10~150W; Scope 5~the 120s of etch period t.
4) select suitable solution by outermost dissolving metal, then use deionized water clean and make sample drying:
The solution dissolving metal need to select according to metal species, and can not react with two-dimensional material or two-dimensional material is damaged, and introduces, without at substrate surface, the pollutant that subsequent step cannot remove.
Using deionized water to clean is to remove the solution dissolving metal that substrate surface speckles with, and the correlative resultant etc. after dissolving metal.
The method making sample drying can be that natural air drying, heating or nitrogen gun dry up.
5) now substrate surface whether only remaining two-dimensional material is determined; If also having 2DM/ metal/2DM ... the structure of metal/2DM exists, then return to step 3) again sample is processed, until substrate surface only remaining two-dimensional material. Step 3) to 5) processing procedure illustrate such as Fig. 4. After these processes, metal/2DM double-layer nanostructured in not curling part also can be completely removed, at this moment just obtain the nano belt of two-dimensional material in insulated substrate surface:
Determine that whether only the method for substrate surface remaining two-dimensional material has: x-ray photoelectron spectroscopy (XPS), x-ray power spectrum (EDS), x-ray fluorescence spectrum (XRF), energy dispersive type x-ray fluorescence spectrum (EDX), Auger electron spectroscopy (AES), transmission electron microscope (TEM), scanning transmission microscope (STEM), PSTM (STM), atomic force microscope (AFM), Raman spectrum etc.
Being masked as accordingly of substrate surface only remaining two-dimensional material nano belt: for XPS, EDS, XRF, EDX, AES, in the measurement result of substrate surface, the measurement result before the metal line strength ratio used is decreased obviously; For TEM, STEM, STM, at former nanometer roll place it is observed that pure two-dimensional material lattice; For AFM, highly consistent corresponding with respective two-dimensional material of height that double-layer nanometer volume place records; For Raman spectrum, when hot spot is beaten at nanometer roll place, do not observe the lifting effect of metal pair Raman spectrum.
Above-mentioned two-dimensional material refers to Graphene (graphene), silene (silicene), germanium alkene (germanene), black phosphorus (BP), boron nitride (BN), Transition-metal dichalcogenide (TMDC), metal carbides or metal nitride (MXene), topological insulator (Bi2Se3、Bi2Te3、Sb2Te3) etc.
The substrate of above-mentioned growth two-dimensional material can be various metal simple-substance, metal alloy, metal-oxide, silicon, germanium, sige alloy, silicon oxide, metal silicide, carborundum, metal carbides, glass, quartz, Muscovitum, various Organic substance, metallorganic, high molecular polymer etc.
The above-mentioned acid solution for dissolving metal can be various acid solution, mixed acid solution, saline solution, and other has the solution etc. of oxidisability.
The technical characterstic of the present invention: the present invention is susceptible to this phenomenon curling based on two-dimensional material edge, by the auxiliary of metal, prepares metal/two-dimensional material double-layer nanostructured of rectangle, thus form the nanometer roll of metal/two-dimensional material at its edge. The width of this frizz generally at below 100nm, by the method to its Reusability plasma etching and wet etching metal, can may finally prepare the two-dimensional material nano belt that width is 30~80nm. Preparing the technology of two-dimensional material nano belt relative to other, the present invention need not use high-precision electron beam exposure apparatus, and prepared two-dimensional material nano belt position is controlled.
Accompanying drawing explanation
Fig. 1 is rectangle two-dimensional material and the schematic diagram with the on all four photoresist window of its size;
Fig. 2 is the schematic diagram of the double-layer nanostructured array of rectangular metal/2DM;
Metal/2DM nanometer roll schematic diagram that the short side edge place that Fig. 3 is double-layer nanostructured for rectangular metal/2DM is formed;
Fig. 4 is the schematic diagram being prepared two-dimensional material nano belt by metal/2DM nanometer roll, and wherein (a) fully etches outermost two-dimensional material; B () is fully dissolve outermost metal; C () is for, after being repeatedly performed the etching of two-dimensional material and the dissolving of metal, being only left the 2DM/ metal/2DM of bottom ... the structure of metal/2DM;D () is two-dimensional material nano belt;
In figure, 1 metal/2DM is double-layer nanostructured; 2 metals/2DM nanometer roll; 3 metals; 4 two-dimensional material; 5 dielectric substrate; 6 photoresists.
Detailed description of the invention
Below by example, the present invention will be further described. It should be noted that the purpose publicizing and implementing example is in that help is further appreciated by the present invention, but it will be appreciated by those skilled in the art that: in the spirit and scope without departing from the present invention and claims, various substitutions and modifications are all possible. Therefore, the present invention should not be limited to embodiment disclosure of that, and the scope that the scope of protection of present invention defines with claims is as the criterion.
Example 1: the preparation of three layers graphene nanobelt.
1) use CVD, grow three layer graphenes at copper foil surface, then three layer graphenes are transferred to SiO2On/Si substrate:
To the mixing gas of copper foil surface ventilating methane, hydrogen and argon under the growth temperature of 1000 DEG C, then grow the three layers continuous film of Graphene at copper foil surface. Subsequently, at three layers graphenic surface spin coating PMMA as support membrane (under the rotating speed of 2500rpm spin coating 60s), ferric chloride (FeCl then it is placed on3) middle immersion, until Copper Foil is corroded completely. It is transferred to SiO by there being PMMA three layer graphenes supported2On/Si substrate. Finally use acetone PMMA film to be dissolved, through cleaning post-drying, obtain being coated with the SiO of three layer graphenes2/ Si substrate slice.
2) in the position that this unabroken regional choice of three layer graphenes is suitable, it is etched into three layer graphenes of rectangle:
With the rotating speed of 4000rpm, at sample surfaces spin coating negativity ultraviolet photoresist (AR-N4340). Using ultraviolet photolithographic at the three unabroken correct positions of layer graphene, exposure length of long sides is a=8 μm, and length of short sides is the rectangle of b=3 μm, uses O after development2Plasma three unnecessary layer graphenes are etched away (etching power be: PRIE=30W; PICP=25W; Etch period is t=40s). Finally will at SiO2/ Si substrate surface leaves three layer graphenes of rectangle.
3) at substrate surface spin coating AR-P5350 photoresist, directly over rectangle three layer graphene, expose rectangular light photoresist window on all four with its figure and size.
4) use thermal evaporation to deposit the thick palladium (Pd) of 3nm at sample surfaces, then obtain Pd/ Graphene double-layer nanostructured of rectangle. Rapidly after cooling, the double-layer nanostructured middle minor face place of this rectangle Pd/ Graphene will occur curling, form the nanometer roll of Pd/ Graphene. Finally, whole sample is soaked in acetone, and uses stripping technology to be peeled off by the unnecessary Pd in other place.
5) O is used2The outermost Graphene of plasma etching:
Use O2The outermost Graphene of plasma etching, the power of etching is: PRIE=30W; PICP=25W; Etch period is t=40s. After etching, outermost layer Graphene will be completely removed, and outermost layer becomes metal Pd.
6) use dust technology fully to dissolve Pd, then sample soaked in deionized water, then with hot plate, sample is dried:
Use dust technology (concentration 25%), when heating, fully dissolve Pd. Then whole substrate is soaked in deionized water, to clean the metal ion of sample surfaces the nitric acid molecule speckled with and the Pd being dissolved in nitric acid. Finally, sample is dried at 80 DEG C with hot plate.
7) dissolve Pd every time, and after clean drying substrate, all use XRF that the Pd content of sample surfaces is measured, if the more last measurement of Pd content significantly decreases, then illustrate that substrate surface has left behind the nano belt of three layer graphenes:
If using the XRF more last measurement of Pd content measured not to be decreased obviously, then illustrate that substrate surface still has the nanometer roll of Pd/ Graphene, it is therefore desirable to then through O2Plasma etching and nitric acid dissolve Pd, until the more last measurement of Pd content significantly decreases.
Example 2: monolayer molybdenum bisuphide (MoS2) preparation of nano belt.
1) CVD is used, at SiO2/ Si superficial growth monolayer MoS2, then by monolayer MoS2It is transferred to another sheet SiO2On/Si substrate:
MoO is utilized at the temperature of 750 DEG C2Powder and sulfur powder are at SiO2/ Si superficial growth goes out monolayer MoS2Continuous film. At this monolayer MoS2Surface is coated with polydimethylsiloxane (PDMS) thin film (thickness is about 3mm), then slowly by it from SiO2/ Si substrate surface is taken off, at this moment, and monolayer MoS2To stick on PDMS. Monolayer MoS will be stained with2PDMS film press lightly at a piece of new SiO2On/Si substrate. Finally use acetone to be dissolved by PDMS film, through cleaning post-drying, obtain being coated with monolayer MoS2SiO2/ Si substrate slice.
2) at this monolayer MoS2The position that unabroken regional choice is suitable, is etched into the monolayer MoS of rectangle2:
With the rotating speed of 4000rpm, at monolayer MoS2Surface spin coating negativity ultraviolet photoresist (AR-N4340). Use ultraviolet photolithographic at monolayer MoS2Unabroken correct position, exposure length of long sides is a=8 μm, and length of short sides is the rectangle of b=4 μm, uses O after development2Plasma is by unnecessary monolayer MoS2Etch away (etching power be: PRIE=60W; PICP=80W; Etch period is t=45s). Finally will at SiO2/ Si substrate surface leaves the monolayer MoS of rectangle2
3) at substrate surface spin coating AR-P5350 photoresist, at rectangle monolayer MoS2Surface exposes rectangular light photoresist window on all four with its figure and size.
4) use thermal evaporation to deposit the thick Al of 2nm at sample surfaces, then obtain the Al/MoS of rectangle2Double-layer nanostructured. Rapidly after cooling, this rectangle Al/MoS2Double-layer nanostructured middle minor face place will occur curling, formed Al/MoS2Nanometer roll. Finally, whole sample is soaked in acetone, and uses stripping technology to be peeled off by the unnecessary Al in other place.
5) O is used2The outermost MoS of plasma etching2:
Use O2Plasma etching outermost layer MoS2, the power of etching is: PRIE=60W; PICP=80W; Etch period is t=45s. After etching, outermost layer MoS2To completely remove, outermost layer becomes metal Al.
6) use dilute hydrochloric acid fully to dissolve Al, then sample soaked in deionized water, then with hot plate, sample is dried:
Dilute hydrochloric acid (mass fraction is 7.5%) is used fully to dissolve Al. Then whole sample is soaked in deionized water, to clean the HCl molecule that sample surfaces speckles with and the Al being dissolved in hydrochloric acid3+. Finally, sample is dried at 80 DEG C with hot plate.
7) dissolve Al every time, and after clean drying substrate, all use EDS that the Al content of sample surfaces is measured, if the more last measurement of Al content significantly decreases, then illustrate that substrate surface has left behind monolayer MoS2Nano belt:
If using the EDS more last measurement of Al content measured not to be decreased obviously, then illustrate that substrate surface still has Al/MoS2Nanometer roll, it is therefore desirable to then through O2Plasma etching and dissolving with hydrochloric acid Al, until the more last measurement of Al content is decreased obviously.
Example 3: monolayer tungsten disulfide (WS2) preparation of nano belt.
1) CVD is used, at native gold superficial growth monolayer WS2, then by monolayer WS2It is transferred to SiO2On/Si substrate:
Use WO3Powder and sulfur powder are at 800 DEG C, it is possible to go out monolayer WS in native gold superficial growth2Continuous film. Subsequently, at WS2Spin coating PMMA in surface, as support membrane (under the rotating speed of 2500rpm spin coating 60s), is then placed in chloroazotic acid and soaks, until native gold is corroded completely.The monolayer WS that PMMA will be had to support2It is transferred to SiO2On/Si substrate. Finally use acetone PMMA film to be dissolved, through cleaning post-drying, obtain being coated with monolayer WS2SiO2/ Si substrate slice.
2) at this monolayer WS2The position that unabroken regional choice is suitable, is etched into the monolayer WS of rectangle2:
With the rotating speed of 4000rpm, at sample surfaces spin coating negativity ultraviolet photoresist (AR-N7520.18). Use ultraviolet photolithographic at monolayer WS2Unabroken correct position, exposure length of long sides is a=8 μm, and length of short sides is the rectangle of b=3 μm, uses O after development2Plasma is by unnecessary monolayer WS2Etch away (etching power be: PRIE=70W; PICP=90W; Etch period is t=50s). Finally will at SiO2/ Si substrate surface leaves the monolayer WS of rectangle2
3) at substrate surface spin coating AR-P5350 photoresist, at rectangle monolayer WS2Surface exposes rectangular light photoresist window on all four with its figure and size.
4) use thermal evaporation to deposit the thick nickel (Ni) of 3nm at sample surfaces, then obtain the Ni/WS of rectangle2Double-layer nanostructured. Rapidly after cooling, this rectangle Ni/WS2Double-layer nanostructured middle minor face place will occur curling, formed Ni/WS2Nanometer roll. Finally, whole sample is soaked in acetone, and uses stripping technology to be peeled off by the unnecessary Ni in other place.
5) O is used2The outermost WS of plasma etching2:
Use O2The outermost WS of plasma etching2, the power of etching is: PRIE=70W; PICP=90W; Etch period is t=50s. After etching, outermost WS2To be completely removed, outermost layer becomes W metal.
6) use dust technology fully to dissolve Ni, then sample soaked in deionized water, then with hot plate, sample is dried:
Use dust technology (mass fraction is 25%), fully dissolve Ni when heating. Then whole sample is soaked in deionized water, clean the ion of sample surfaces the nitric acid molecule speckled with and the Ni being dissolved in nitric acid. Finally, hot plate is used to be dried by sample at 80 DEG C.
7) dissolve Ni every time, and after clean drying substrate, all use AFM to former Ni/WS2The position of nanometer roll carries out elevation carrection, if final height is less than 1nm, then illustrates that substrate surface has left behind monolayer WS2Nano belt:
If using the AFM height measured more than 1nm, then illustrate that substrate surface still has Ni/WS2Nanometer roll, it is therefore desirable to then through O2Plasma etching and nitric acid dissolve Ni, until being highly down to below 1nm.
Example 4: the preparation of single-layer graphene nano belt.
1) use CVD, grow single-layer graphene at copper foil surface, then single-layer graphene is transferred to SiO2On/Si substrate:
Under the growth temperature of 1000 DEG C, pass into the mixing gas of methane, hydrogen and argon to copper foil surface, then grow the continuous film of single-layer graphene at copper foil surface. Subsequently, at single-layer graphene surface spin coating PMMA as support membrane (under the rotating speed of 2500rpm spin coating 60s), FeCl then it is placed on3Solution soaks, until Copper Foil is corroded completely. It is transferred to SiO by there being the PMMA single-layer graphene supported2On/Si substrate. Finally use acetone PMMA film to be dissolved, through cleaning post-drying, obtain being coated with the SiO of single-layer graphene2/ Si substrate slice.
2) in the position that the unabroken regional choice of this single-layer graphene is suitable, it is etched into the single-layer graphene of rectangle:
With the rotating speed of 4000rpm, in single-layer graphene surface spin coating negativity ultraviolet photoresist (AR-N7520.18).Using ultraviolet photolithographic at the unabroken correct position of single-layer graphene, exposure length of long sides is a=8 μm, and length of short sides is the rectangle of b=4 μm, uses O after development2Plasma unnecessary single-layer graphene is etched away (etching power be: PRIE=25W; PICP=20W; Etch period is t=30s). Finally will at SiO2/ Si substrate surface leaves the single-layer graphene of rectangle.
3) at substrate surface spin coating AR-P5350 photoresist, directly over rectangle single-layer graphene, expose rectangular light photoresist window on all four with its figure and size.
4) use thermal evaporation to deposit the thick Al of 2.5nm at sample surfaces, then obtain Al/ Graphene double-layer nanostructured of rectangle. Rapidly after cooling, the double-layer nanostructured middle minor face place of this rectangle Al/ Graphene will occur curling, form the nanometer roll of Al/ Graphene. Finally, whole sample is soaked in acetone, and uses stripping technology to be peeled off by the unnecessary Al in other place.
5) O is used2The outermost Graphene of plasma etching:
Use O2The outermost Graphene of plasma etching, the power of etching is: PRIE=25W; PICP=20W; Etch period is t=30s. After etching, outermost Graphene will be completely removed, and outermost layer becomes metal Al.
6) use dilute hydrochloric acid fully to dissolve Al, then sample soaked in deionized water, then with hot plate, sample is dried:
Dilute hydrochloric acid (mass fraction is 7.5%) is used fully to dissolve Al. Then whole sample is soaked in deionized water, clean the HCl molecule that sample surfaces speckles with and the Al being dissolved in hydrochloric acid3+. Finally, hot plate is used to be dried by sample at 80 DEG C.
7) dissolve Al every time, and after clean drying substrate, all use the AFM position that former Al/ graphene nano is rolled up to carry out elevation carrection, if final height is lower than 1nm, then illustrate that substrate surface has left behind the nano belt of single-layer graphene:
If using the AFM height measured more than 1nm, then illustrate that substrate surface still has the double-layer nanostructured frizz of Al/ Graphene, it is therefore desirable to then through O2Plasma etching and dissolving with hydrochloric acid Al, until being highly down to below 1nm.
Although the present invention discloses as above with preferred embodiment, but is not limited to the present invention. Any those of ordinary skill in the art, without departing under technical solution of the present invention ambit, all may utilize the method for the disclosure above and technology contents and technical solution of the present invention is made many possible variations and modification, or be revised as the Equivalent embodiments of equivalent variations. Therefore, every content without departing from technical solution of the present invention, the technical spirit of the foundation present invention, to any simple modification made for any of the above embodiments, equivalent variations and modification, all still falls within the scope of technical solution of the present invention protection.

Claims (10)

1. a preparation method for two-dimensional material nano belt, comprises the steps of:
1) grow two-dimensional material at substrate surface, then two-dimensional material is transferred in dielectric substrate;
2) etch described two-dimensional material rectangular, at this rectangle two-dimensional material surface spin coating photoresist, make and the on all four rectangular light photoresist window of above-mentioned rectangle two-dimensional material size; Using thermal evaporation deposit layer of metal to be formed double-layer nanostructured, after cooling, described double-layer nanostructured edge curls into double-layer nanometer volume, is fallen by the metal-stripping in other region;
3) double-layer nanometer volume described in plasma etching is used to be positioned at outermost two-dimensional material, until outermost material becomes metal;
4) by outermost dissolving metal, then clean with deionized water and dry;
5) step 3 is repeatedly repeated) and 4), until the two-dimensional material in double-layer nanometer volume is all etched to two-dimensional material nano belt.
2. preparation method as claimed in claim 1, it is characterised in that described two-dimensional material is Graphene, silene, germanium alkene, black phosphorus, boron nitride, Transition-metal dichalcogenide, metal carbides or metal nitride or topological insulator.
3. preparation method as claimed in claim 1, it is characterized in that, the substrate of described growth two-dimensional material is various metal simple-substance, metal alloy, metal-oxide, silicon, germanium, sige alloy, silicon oxide, metal silicide, carborundum, metal carbides, glass, quartz, Muscovitum, various Organic substance, metallorganic or high molecular polymer.
4. preparation method as claimed in claim 1, it is characterised in that the thickness range of described metal is 2~8nm.
5. preparation method as claimed in claim 1, it is characterised in that described metal is ferrum, nickel, palladium, gold, copper, silver, antimony, aluminum, bismuth, magnesium or zinc etc.
6. preparation method as claimed in claim 1, it is characterised in that step 2) described in the condition that meets of the size of rectangular double-layer nanostructured be: length of short sides less than or equal to 4 μm, and long limit with length of short sides ratio more than or equal to 1.5.
7. preparation method as claimed in claim 1, it is characterised in that step 3) described in plasma refer to O2、CHF3、XeF2、Cl2, the gas such as Ar plasma.
8. preparation method as claimed in claim 1, it is characterised in that step 3) described in the technological parameter of plasma etching be: RIE power is 5W~100W, and ICP power is 10W~150W, and etch period is 5s~120s.
9. preparation method as claimed in claim 1, it is characterised in that step 4) described in dissolve the solution of metal and refer to various acid solution, mixed acid solution, saline solution, and other has the solution of oxidisability.
10. preparation method as claimed in claim 1, it is characterized in that, step 5) in judge that the two-dimensional material in double-layer nanometer volume is all etched to the method for two-dimensional material nano belt when being respectively as follows: XPS, EDS, XRF, EDX, AES metal content measure technology of employing, the measurement result before metal line strength ratio measured by substrate surface is decreased obviously; Or when adopting TEM, STEM, STM, structure characterization technique, at former nanometer of frizz place it is observed that pure two-dimensional material lattice; Or when adopting AFM height measurement technique, highly consistent corresponding with respective two-dimensional material of height that double-layer nanometer frizz place records; Or when adopting Raman spectroscopy, when hot spot is beaten at double-layer nanometer frizz place, do not observe the lifting effect of metal pair Raman spectrum.
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