CN103935956B - A kind of graphene nanobelt border method of modifying based on Tip-Enhanced Raman Spectroscopy - Google Patents
A kind of graphene nanobelt border method of modifying based on Tip-Enhanced Raman Spectroscopy Download PDFInfo
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- CN103935956B CN103935956B CN201410148684.XA CN201410148684A CN103935956B CN 103935956 B CN103935956 B CN 103935956B CN 201410148684 A CN201410148684 A CN 201410148684A CN 103935956 B CN103935956 B CN 103935956B
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Abstract
The present invention discloses a kind of graphene nanobelt border method of modifying based on Tip-Enhanced Raman Spectroscopy, first graphene nanobelt to be finished for border is transferred on substrate, silicon nitride cantilevers conducting probe is contacted with graphene nanobelt, will electric probe be added directly be pressed in the top of graphene nanobelt; Silicon nitride cantilevers conducting probe is connected with the mains, and is connect and adds electric probe and on graphene nanobelt, apply bias voltage to form loop, allow electric current pass graphene nanobelt by silicon nitride cantilevers conducting probe; Scan with the border of silicon nitride cantilevers conducting probe to graphene nanobelt, gated sweep speed is 10-30 μm/s, and the carbon atom on border is subject to energy excitation and spontaneously carries out atom reconstruct, and graphene edge generates the graphene nanobelt of the atom level of crystalline state; Other defect can not be introduced to graphene nanobelt in the basis that the border of graphene nanobelt is reconstructed, easy to operate, and in operating process, be convenient to monitoring.
Description
Technical field
The invention belongs to field of nanometer technology, be specifically related to a kind of graphene nanobelt border method of modifying based on Tip-Enhanced Raman Spectroscopy (Tip-enhancedRamanspectroscopy, TERS) system.
Background technology
Graphene is a kind of by the former molecular material of monolayer carbon, and have numerous very special physical characteristic, under room temperature, the migration velocity of electronics in grapheme material is 200 times of silicon conductor.Research is before this verified, and CNT (cylindrical structure curling by Graphene) has fabulous electric conductivity, but the comparatively complicated CNT of structure is difficult to be arranged on electronic chip inside.Along with deepening continuously of studying Graphene, Graphene is applied in traditional field-effect transistor and becomes a kind of trend, become study hotspot based on the microelectronic component preparation of Graphene and the electrology characteristic of Graphene.Usually, the field-effect transistor used in digital circuit needs higher on-off ratio, to having response speed faster to the gate source voltage of change, therefore needs to possess less grid and the higher conducting channel of electron mobility.And Graphene is a kind of semi-metallic of zero band gap, therefore only open the band gap of Graphene, the on-off ratio of grapheme transistor could be improved.Research finds, bilayer graphene is added to vertical electric field or carries out adulterating to Graphene and can open the band gap of Graphene, and another method conveniently opening Graphene band gap prepares graphene nanobelt exactly, and the width of its band gap width and nanobelt and be with the shape on border relevant.
Graphene nanobelt has two kinds of border structures: armchair and zigzag.Border structure is very important in the rare nanostructured of graphite, wherein armchair graphene nanobelt shows as semiconductor property, sawtooth pattern graphene nanobelt then shows metalline, the probability that carrier penetrates Schottky barrier not with size and length change and change.The boundary condition of graphene nanobelt and the impact of width on graphene nanobelt field-effect transistor character most important.Due to the restriction of nanobelt boundary condition and width, the preparation of graphene nanobelt faces huge challenge.The conventional preparation method of the rare nanobelt of graphite, as CNT cutting-out method, nanowire mask etching method and photoetching process etc., do not possess the ability on the rare border of controlled working graphite, what obtain is all unordered border structures, uncontrollablely determines the rare nanobelt structure of the graphite on border.At present, by the anisotropic etching effect in conjunction with traditional micro-processing technology and Graphene, accurately can prepare smooth sawtooth pattern (atom level) border structure, but, high oxide residual on the graphene nanobelt that ion cutting obtains and the removal problem of surface impurity propose higher requirement to graphene nanobelt (Graphenenanoribbon, GNR) preparation.Carbon atom during graphite is rare is SP
2configuration, if carried out cutting, its border atomic structure will inevitably be destroyed and occur dangling bonds, introduces defect in Graphene, reduces the mobility of carrier in graphene-channel.Therefore, the rare nanobelt of graphite prepared for conventional method can carry out border modification by prior art.Different borders is modified, and has different impacts to the Electronic Transport Properties of the rare nanobelt of graphite.
The impact of boundary condition on the electric property of device of Graphene also can not be ignored, therefore seems particularly important to the selection on GNR border and the restructuring of defect internal carbon.Existing researcher is by the integrated system (TEM-STM) based on transmission electron microscope and PSTM, utilize Joule heat that the carbon atom of graphene edge is at high temperature evaporated, nanobelt border re-constructs, and effectively form crystalline state specific border continuously.
Tip-Enhanced Raman Spectroscopy technology based near field optic principle and SPM technology is a kind of new technology that developed recently gets up.Tip-Enhanced Raman Spectroscopy combine with technique SPM scanning technique and needle point strengthen optical detector technology.Needle point strengthens the raman spectral signal that optical technology can strengthen nanometer local greatly, further raising signal to noise ratio, when beam of laser is radiated at distance sample surfaces nanometer separations in a suitable manner, when radius of curvature is on the needle point of the gold-plated or platinum plating of the SPM of tens nanometers (atomic force microscope or PSTM STM needle point), due to optical antenna resonance enhancement, near needle point, electromagnetic field is greatly strengthened, thus enhance the Raman signal of nanometer local near needle point, there is SPM technology and the Tip-Enhanced Raman Spectroscopy combine with technique of nano-space resolution ratio, bias voltage can be applied to modify sample surfaces at conducting probe and sample.This technology has been applied to the sign of semi-conducting material, DNA molecular and biomolecule etc.
Summary of the invention
The object of the invention is in order to overcome above-mentioned conventional graphite alkene nanobelt border comparatively coarse, had a strong impact on its electric conductivity, be the problem of the large obstacle hindering graphene nanobelt electric transmission, provide a kind of completely newly based on the graphene nanobelt border method of modifying of Tip-Enhanced Raman Spectroscopy (TERS) system, consistent, the periodically rare nanobelt structure of graphite can be processed.
The present invention realizes foregoing invention object by following means: Tip-Enhanced Raman Spectroscopy system is made up of FT-Raman and confocal Raman system and atomic force microscopy system, atomic force microscopy system adopts silicon nitride cantilevers conducting probe, first graphene nanobelt to be finished for border is transferred on substrate, silicon nitride cantilevers conducting probe is contacted with limit graphene nanobelt, will electric probe be added directly be pressed in the top of border graphene nanobelt to be finished; Silicon nitride cantilevers conducting probe is connected with the mains, is connect by silicon nitride cantilevers conducting probe and add electric probe and on graphene nanobelt, apply bias voltage to form loop, allowing electric current pass graphene nanobelt; Scan with the border of silicon nitride cantilevers conducting probe to graphene nanobelt, gated sweep speed is 10-30 μm/s, and the carbon atom on border is subject to energy excitation and spontaneously carries out atom reconstruct, and graphene edge generates the graphene nanobelt of the atom level of crystalline state.
The beneficial effect that the present invention has after adopting technique scheme is: the graphene nanobelt that the present invention can be unordered to the border of being prepared by conventional method carries out border restructuring modification, other defect can not be introduced to graphene nanobelt in the basis that the border of graphene nanobelt is reconstructed, realize in the Raman spectrum system that the boundary types reconstruct of graphene nanobelt and modifying process use needle point to strengthen, the Raman spectroscopy that needle point strengthens can to the monitoring that the situation of carrying out of reconstruct is carried out constantly while being reconstructed the border of graphene nanobelt, whether monitoring reaches expection requirement.The present invention is easy to operate, and is convenient to monitoring in operating process, has huge progradation to the preparation of graphene nanobelt field-effect transistor and popularization.
Accompanying drawing explanation
Fig. 1 is the armchair border schematic diagram of graphene nanobelt;
Fig. 2 is the sawtooth pattern border schematic diagram of graphene nanobelt;
Fig. 3 carries out processing the enforcement schematic diagram reconstructed to graphene nanobelt border prepared by conventional method for utilizing Tip-Enhanced Raman Spectroscopy (TERS) system;
Fig. 4 is irregular and passes through the Raman spectrogram on the sawtooth pattern graphene nanobelt border modified, first figure is the Raman spectrogram on irregular sawtooth pattern graphene nanobelt border, second figure is the Raman spectrogram through the sawtooth pattern graphene nanobelt border modified, and illustration is wherein Lorentz lorentz's fitted figure picture of each G characteristic peak.
Description of reference numerals is as follows:
1-armchair graphene nanobelt; 2-sawtooth pattern graphene nanobelt; 3-substrate; The graphene nanobelt that 4-border is to be finished; 5-Raman spectrum system; 6-silicon nitride cantilevers conducting probe; 7-add electric probe.
Detailed description of the invention
Below in conjunction with accompanying drawing, the present invention is described further, but protection scope of the present invention is not limited thereto.
Fig. 1 and the two kinds of border structure types that Figure 2 shows that Graphene of the present invention: armchair graphene nanobelt 1 and sawtooth pattern graphene nanobelt 2.
Figure 3 shows that the enforcement schematic diagram that the graphene nanobelt border based on Tip-Enhanced Raman Spectroscopy (TERS) system reconstructs.Unordered border, the border of conventional method being prepared graphene nanobelt 4 to be finished is transferred in the target substrate 3 with traditional cmos process compatibility, transfer to the graphene nanobelt 4 that border on substrate 3 is to be finished, before carrying out border modification, first dry up with nitrogen with after acetone, absolute ethyl alcohol, each ultrasonic 3-5 of deionized water minute.
Tip-Enhanced Raman Spectroscopy system is made up of FT-Raman and confocal Raman system 5 and atomic force microscopy (AFM) system.Atomic force microscopy system adopts silicon nitride cantilevers conducting probe 6, and silicon nitride cantilevers conducting probe 6 is coated with 10-50nm platinum, to meet probe electric conductivity.The elastic constant of silicon nitride cantilevers conducting probe 6 is 0.06-0.58N/m, and resonant frequency is 18-65KHz.Silicon nitride cantilevers conducting probe 6 uses carbon nano-tube point or all-metal silk needle point, and its radius of curvature is 5-20nm.
In TERS system, silicon nitride cantilevers conducting probe 6 is connected with the mains, and will add electric probe 7 and be directly pressed in a top of border graphene nanobelt to be finished 4.During AFM employing contact mode, silicon nitride cantilevers conducting probe 6 graphene nanobelt 4 also to be finished with border contacts, by to silicon nitride cantilevers conducting probe 6 with add electric probe 7 and on the graphene nanobelt 4 that border is to be finished, apply bias voltage to form loop, allow electric current pass border graphene nanobelt to be finished 4.
Under AFM system contacts pattern, utilize graphene nanobelt 4 border to be finished, silicon nitride cantilevers conducting probe 6 pairs of borders to scan, gated sweep speed is 10-30 μm/s.Due to the joule heating effect that electric current causes, energy will be dissipated in the Nodes on graphene nanobelt to be finished 4 border, border, cause the carbon atom on border be subject to energy excitation and spontaneously carry out atom reconstruct, thus graphene nanobelt 4 border of impelling border to be finished obtain atom level structural remodeling.Simultaneously due to the evaporation of part carbon atom and other foreign ions, defective graphene edge generates the nanobelt of crystalline state, forms the perfect graphene nanobelt of atom level.While the graphene nanobelt 4 that AFM system is to be finished to border carries out modification, the change of the Raman spectrum strengthened by needle point, sawtooth pattern and handrail type Graphene can be made a distinction, thus realize the preparation of the graphene nanobelt of evenly regular specific border (armchair and the sawtooth pattern) structure in border, as shown in Figure 4, the appearance of sawtooth pattern nanobelt can cause and is positioned at 1593cm
-1the splitting of neighbouring G feature peak-to-peak.
In the border restructuring procedure of border graphene nanobelt 4 to be finished, carry out under nitrogen or ar gas environment, the border reconstruct situation of the Raman spectrum system 5 in TERS system to graphene nanobelt 4 to be finished is utilized to detect whether reach expection requirement, the restructuring situation on graphene nanobelt border can be monitored by the change constantly of Raman spectrum, by the orthoplasy and the carbon atom restructuring that regulate the sweep speed of bias voltage and silicon nitride cantilevers conducting probe 6 to realize graphene nanobelt border, Tip-Enhanced Raman Spectroscopy system uses the optical maser wavelength of 532nm, the Raman light of laser energy 2mW is monitored.
Claims (6)
1. the graphene nanobelt border method of modifying based on Tip-Enhanced Raman Spectroscopy, Tip-Enhanced Raman Spectroscopy system is made up of FT-Raman and confocal Raman system and atomic force microscopy system, atomic force microscopy system adopts silicon nitride cantilevers conducting probe, it is characterized in that:
(1) first graphene nanobelt to be finished for border is transferred on substrate, described silicon nitride cantilevers conducting probe is contacted with graphene nanobelt, will electric probe be added directly be pressed in the top of described graphene nanobelt,
(2) silicon nitride cantilevers conducting probe is connected with the mains, by silicon nitride cantilevers conducting probe with add electric probe and on graphene nanobelt, apply bias voltage to form loop, allow electric current pass graphene nanobelt;
(3) scan with the border of silicon nitride cantilevers conducting probe to graphene nanobelt, gated sweep speed is 10-30 μm/s, the carbon atom on border is subject to energy excitation and spontaneously carries out atom reconstruct, and graphene edge generates the graphene nanobelt of the atom level of crystalline state.
2. according to claim 1 based on the graphene nanobelt border method of modifying of Tip-Enhanced Raman Spectroscopy, it is characterized in that: step (3) is carried out under nitrogen or ar gas environment.
3., according to claim 1 based on the graphene nanobelt border method of modifying of Tip-Enhanced Raman Spectroscopy, it is characterized in that:
Silicon nitride cantilevers conducting probe is coated with 10-50nm platinum, and the elastic constant of silicon nitride cantilevers conducting probe is 0.06-0.58N/m, and resonant frequency is 18-65kHz.
4. according to claim 1 based on the graphene nanobelt border method of modifying of Tip-Enhanced Raman Spectroscopy, it is characterized in that: the needle point of silicon nitride cantilevers conducting probe is carbon nano-tube point or all-metal silk needle point, and the radius of curvature of needle point is 5-20nm.
5. according to claim 1 based on the graphene nanobelt border method of modifying of Tip-Enhanced Raman Spectroscopy, it is characterized in that: use optical maser wavelength 532nm, the border reconstruct situation of Raman light to graphene nanobelt of laser energy 2mW detects.
6. according to claim 1 based on the graphene nanobelt border method of modifying of Tip-Enhanced Raman Spectroscopy, it is characterized in that: in step (1), the graphene nanobelt transferred on substrate is first dried up with nitrogen with after acetone, absolute ethyl alcohol, each ultrasonic 3-5 of deionized water minute.
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| CN106985213B (en) * | 2017-04-28 | 2019-01-29 | 沈阳工业大学 | Utilize the method and apparatus of the accurate controllable cutting graphite alkene band of photocatalytic oxidation |
| CN110117780B (en) * | 2019-03-19 | 2021-03-12 | 中国科学院上海微***与信息技术研究所 | Two-dimensional material layer and preparation method thereof |
| CN110342504B (en) * | 2019-06-28 | 2021-05-28 | 西安交通大学 | Preparation method of graphene nanoribbon |
| CN110311010B (en) * | 2019-06-28 | 2022-06-07 | 西安交通大学 | Infrared wide spectrum detector based on graphene nanoribbons |
| CN111505345B (en) * | 2020-05-15 | 2021-08-10 | 大连理工大学 | Atomic force microscope probe modification method based on scanning electron microscope micro-control system |
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| CN102285631A (en) * | 2011-06-09 | 2011-12-21 | 北京大学 | Method for processing nanoscale pattern on graphite or graphene surface |
| CN102502605A (en) * | 2011-11-09 | 2012-06-20 | 复旦大学 | Electrically-induced reduction method for degraded graphene oxide |
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