CN104360107B - A kind of graphene coated atomic force microscope probe and preparation method thereof, purposes - Google Patents
A kind of graphene coated atomic force microscope probe and preparation method thereof, purposes Download PDFInfo
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- CN104360107B CN104360107B CN201410632559.6A CN201410632559A CN104360107B CN 104360107 B CN104360107 B CN 104360107B CN 201410632559 A CN201410632559 A CN 201410632559A CN 104360107 B CN104360107 B CN 104360107B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
- G01Q60/00—Particular types of SPM [Scanning Probe Microscopy] or microscopes; Essential components thereof
- G01Q60/24—AFM [Atomic Force Microscopy] or apparatus therefor, e.g. AFM probes
- G01Q60/38—Probes, their manufacture, or their related instrumentation, e.g. holders
- G01Q60/40—Conductive probes
Abstract
The invention belongs to atomic force microscope field, relate to a kind of graphene coated atomic force microscope probe and preparation method thereof, purposes, described a kind of graphene coated atomic force microscope probe, including probe base, cantilever, needle point, described cantilever and needle point are provided with metal level, needle point are additionally provided with graphene layer.The preparation method of described graphene coated atomic force microscope probe, comprise the following steps: the preparation of (1) graphene solution: 5 10 mg Graphenes are added in 1mL water, ultrasonic disperse 10 min in ultrasonic washing instrument, prepares the graphene solution that concentration is 5 10 mg/mL；(2) prepare graphene coated atomic force microscope probe: the needle point of the atomic force microscope probe that cantilever and needle point are provided with metal level immerses in the graphene solution of step (1), take out nature after mechanical agitation 30 60 s and dry.
Description
Technical field
The invention belongs to atomic force microscope field, relate to a kind of atomic force microscope probe and preparation method thereof, purposes,
Particularly relate to a kind of ruggedness graphene coated atomic force microscope probe and preparation method thereof, purposes.
Background technology
Atomic force microscope (AFM) is a kind of to have dividing for surface topography collection, electromagnetic performance of atomic resolution
The important instrument of analysis, is the important characterization tool in the field such as Surface Science, nanotechnology.Wherein, AFM probe is atomic force microscopy
Important component part in mirror, belongs to the conventional consumptive material of this high technology equipment, and its main manufacturer is distributed in Germany, auspicious
Scholar, the U.S., Japan and other countries.Common AFM probe is mainly by utilizing micro electro mechanical system (MEMS) technology means processing silicon or silicon nitride
Prepare, and conducting electricity AFM probe is that (and other improve binding force of cladding material in thick for average probe plated surface 10-50 nm metal platinum
Metal, such as titanium, chromium, platinum and iridium etc.) obtain.But, conduction AFM probe in use its conductive coating is prone to wear out,
Its electric conductivity is caused to be difficult to permanently effective holding, so the associated mechanisms of a lot of country all has high-resolution being devoted to research and development
The novel probe of more long life.At present, the new product of conduction afm tip has needle point based on CNT, diamond
Coating needle point and all-metal silk needle point etc., although these new techniques overcome the common conductive afm tip life-span to a certain extent
The shortcoming that shorter and resolution is the highest, but its preparation process is sufficiently complex, and production cost is higher.
Owing to having monoatomic layer thickness, high connductivity, heat conductivity, the excellent properties such as high mobility and be widely used in each
The Graphene of individual research field also is used for preparing conducting atomic force microscopy probe by some seminars.
1.Wen (Y. Wen, J.Chen, Y.Guo, B.Wu, G.Yu and Y.Liu, Multilayer.Graphene-
Coated atomic Force Microscopy Tips for Molecular Junctions, Adv. Mater.,
2012,24,3,482 3485) on gold-plated AFM probe, Graphene etc. is directly grown by chemical vapour deposition technique (CVD), first
Secondary obtain Graphene AFM probe.Wherein ethanol is as carbon source, gold as catalyst, hydrogen and argon gaseous mixture as current-carrying gas
Body.Ethanol is placed in low-temperature space, and gold-plated AFM probe is placed on high-temperature region (750-850 DEG C), is passed through flow velocity under mark condition and is
The gaseous mixture of 100 mL/min.After 5 minutes, form graphene layer in gold surface.
2. Martin-Olmos(C. Martin-Olmos, H. I. Rasool, B. H. Weiller and J.
K. Gimzewski, Graphene MEMS: AFM Probe Performance Improvement, ACS Nano,
2013,7 (5), 4,164 4170.) etc. on copper mold plate, stone is grown by etching-CVD by filling and etch SU-8 photoresist
Ink alkene also finally gives the AFM probe of graphene modified.The method first step sodium hydroxide selective etch silicon chip, forms heat
Oxide layer, then the substrate deposited as Graphene in its surface plated with copper；Second step, by chemical vapour deposition technique in substrate
On obtain continuous print graphene layer；3rd step, uses SU-8 photoresist to fill needle point mould, is exposed development operation；4th
Step, being passed through dry argon removing surface does not has the Graphene region of photoresist, and meanwhile, spin coating second layer SU-8 photoresist is with shape
Become the cantilever of probe.Finally, remove the silicon oxide etc. that the needle point back side is unnecessary, clean remainder, thus obtain whole AFM and visit
Pin.
3. Shim(W. Shim, K. A. Brown, X. Zhou, B. Rasina, X. Liao and C. A.
Mirkina, Multifunctional cantilever-free scanning probe arrays coated with
multilayer graphene,Proc. Natl. Acad. Sci. U. S. A., 2012, 109(45), 18312–
18317.) and Mario (M. Lanza, A. Bayerl, T. Gao, M. Porti, M. Nafria, G. Jing, Y.
Zhang, A. Liu and H. Duan, Graphene-coated Atomic Force Microscope tips for
reliable nanoscale electrical characterization,Adv. Mater., 2013, 25, 1440–
1444.) etc. directly it is transferred to the Graphene being grown in copper surface by transfer method conduct electricity on AFM probe.First at cuprio stone
One layer of PMMA of spin coating on ink alkene, rear with liquor ferri trichloridi etching copper substrate, obtain after hydrochloric acid and aqueous cleaning respectively
PMMA/ graphene layer；Conduction AFM probe is as the substrate of reception Graphene, and a period of time of drying in the air after transfer, (Graphene was attached to being dried
At detecting probe surface) after remove PMMA with acetone, finally with water clean i.e. can get Graphene cover AFM probe.
Although the Graphene AFM probe prepared by these methods improves the usability of probe to a certain extent
Can, but these preparation methoies yet suffer from bigger defect.For chemical vapour deposition technique, the carbon directly obtained on probe
Its quality of film obtains carbon film quality far below growth on Copper Foil.It is big that probe for preparing with Graphene covering copper mold exists two
Problem: 1. this preparation method needs a brand-new production and processing technology, cost is high and needs professional operation, and condition is harsh；2.
The probe tip prepared has bigger radius of curvature, affects lateral resolution.And the Graphene AFM obtained for transfer method visits
Pin, although generally Copper Foil is as the substrate of graphene growth, the graphene layer of available better quality, but the method transfer process
Complex, and PMMA is difficult to, except clean, therefore to reduce the quality of Graphene thus affect the performance of Graphene AFM probe.
Summary of the invention
The electrical characterization of nanoscale is the steps necessary analyzing many material properties in scientific research and commercial Application, at this
In field, maximally effective characterization tool is conducting atomic force microscopy, it can characterize in range of small conductor and thin absolutely
The electrical properties of edge layer material.Wherein, conducting atomic force microscopy probe is can not as the important component part of Sample Scan
Or lack, it is made up of probe base, cantilever, needle point three part.The purpose of the present invention includes the following aspects:
(1) due to normally used common conductive AFM probe be silicon detecting probe surface plating certain thickness (nanoscale) gold
Belong to, and the highest electric current and big frictional force can make the coat of metal wear and tear, and do not only result in and obtain false pattern
Image, and the quickly consumption of probe too increases the cost of research.The present invention will be greatly reduced the Fast Wearing of needle point, extend
The service life of probe.(2) current, commercially available conduction AFM probe has diamond probe, uses stable diamond coating, though
So ensure that the low abrasion degree of probe, but be the increase in the radius of probe, reduce its lateral resolution.The present invention will keep pin
The needle point radius of curvature that point is less has high-resolution with holding probe.(3) other solid metal or diamond coating are significantly
Improve the cost price of probe, the present invention uses Graphene with low cost as coating layer material, is greatly reduced and is manufactured into
This.(4) other conduction AFM probe can cause coating metallic atom penetrate into sample and introduce the pollution to sample, the present invention by
Atom bond energy strong between the impenetrability and carbon atom of Graphene alveolate texture so that metallic atom can not be to sample
Migrate, it is to avoid the pollution of sample.(5) its growth substrate is had by chemical vapour deposition technique due to the preparation of high-quality graphene
There is the strongest selectivity, and common afm tip is not at the bottom of the well behaved basis of graphene growth, prepares high-quality stone so need to explore
The new method of the afm tip of ink alkene cladding.High-quality graphene is coated on afm tip by the present invention, it is to avoid Graphene quality
Poor and the harmful effect that causes.
The purpose of the present invention can be achieved through the following technical solutions:
A kind of graphene coated atomic force microscope probe, including probe base, cantilever, needle point, described cantilever and pin
Point is provided with metal level, and needle point is additionally provided with graphene layer.
Preferably, described a kind of graphene coated atomic force microscope probe, described metal level is double-metal layer, by
Interior to outer respectively titanium and platinum；Or described metal level is single metal layer, monometallic is the alloy of platinum and iridium.
Preferably, described a kind of graphene coated atomic force microscope probe, described graphene layer is 1 to 3 layer, thick
Degree is 0.34-1 nm.
Preferably, described a kind of graphene coated atomic force microscope probe, described probe base is silicon or nitridation
Silicon.
A kind of preparation method of graphene coated atomic force microscope probe, described preparation method comprises the following steps:
(1) preparation of graphene solution: 5-10 mg Graphene is added in 1 mL water, ultrasonic in ultrasonic washing instrument
Disperse 10 min, prepare the graphene solution that concentration is 5-10 mg/mL；
(2) graphene coated atomic force microscope probe is prepared: the atomic force that cantilever and needle point are provided with metal level shown
The needle point of micro mirror probe immerses in the graphene solution of step (1), takes out nature and dry after mechanical agitation 30-60 s.
The Graphene that in the preparation method of described a kind of graphene coated atomic force microscope probe prepared by step (1) is molten
In liquid, Graphene average-size is less than 1 micron, and thickness is 1-5 layer, and every layer thickness is 0.334 nm.
The preparation method of described a kind of graphene coated atomic force microscope probe, the metal level described in preparation method
For double-metal layer, the most respectively titanium and platinum；Or described metal level is single metal layer, monometallic is the conjunction of platinum and iridium
Gold.
Described a kind of graphene coated atomic force microscope probe purposes in preparation atomic force microscope.
Graphene has the biggest specific surface area and good pliability and ductility so that it is can be by means of Van der Waals force
Effect is firmly adsorbed on detecting probe surface, thus can realize the purpose that needle point is coated with completely by graphene layer.
The technological means of subsequent treatment and effect thereof: observe Graphene attachment state on afm tip and quantity is many
Few, and with nitrogen, its probe tip is applied certain active force, so on the one hand Graphene can be made in the suction at needle point position
Attached more firm, the Graphene that on the other hand other positions of probe are unnecessary can be removed.
Compared with prior art, it has the beneficial effect that the present invention
First can reduce scientific research cost, extend the service life of probe, many experiments can be carried out, thus reduce probe
Loss.Next adds the reliability of test data, and Graphene AFM probe will not contaminated samples, using the teaching of the invention it is possible to provide real image.
Economic results in society:
Reducing the manufacturing cost of Graphene probe, preparation method is simple, fast, and low cost, and raw material can repeatedly utilize.
The most easily commercial application, preparation process is not required to manpower, can all realize automation mechanized operation, and product disclosure satisfy that supply and demand.
Graphene coated AFM probe preparation method of the present invention and prior art preparation method (CVD, etching method, transfer
Method) compared obvious advantage: 1. and this technology need not professional equipment, such as litho machine, CVD system etc.；2. need not harshness
Condition, without any restrictions to preparation condition, such as high temperature, inert ambient environment；3. it is not related to gas and poisonous process, such as nitrogen
Gas, argon, carbon monoxide, photoresist, acetone etc.；4. need not professional technique operation, such as photoetching and etching, CVD gas controls
Deng.On the whole, this technology of preparation method is simple, remarkably productive, and reduces processing cost, it is easy to industrialization.
Accompanying drawing explanation
Fig. 1 is the SEM figure of the platinum plating without graphene layer-titanium atom force microscope probe.
Fig. 2 is the SEM figure of the platinum plating-titanium atom force microscope probe of graphene coated.
Fig. 3 is the local T EM image of the platinum plating-titanium atom force microscope probe tip of graphene coated.
Fig. 4 is the current-voltage spectrum that the platinum plating without graphene layer-titanium atom force microscope probe gathers the most afterwards
Line.
Fig. 5 is the current-voltage spectrum that the platinum plating-titanium atom force microscope probe of graphene coated gathers the most afterwards
Line.
The graphene coated that Fig. 6 is the conducting atomic force microscopy probe without graphene layer and prepared by distinct methods former
Total scan area cartogram that sub-force microscope probe many experiments draws.
Fig. 7 is the schematic diagram of the graphene coated atomic force microscope probe of the present invention.
In accompanying drawing explanation, described platinum plating-titanium atom force microscope probe is and is respectively the double of titanium and platinum from the inside to the outside
The atomic force microscope probe of metal level.
Detailed description of the invention
Embodiment 1
(1) preparation of graphene solution: 5 mg Graphenes are added in 1 mL water, ultrasonic disperse in ultrasonic washing instrument
10 min, prepare the graphene solution that concentration is 5 mg/mL；
(2) graphene coated atomic force microscope probe is prepared: be that silicon, cantilever and needle point are provided with from the inside to the outside by substrate
The needle point of the atomic force microscope probe being respectively the double-metal layer of titanium and platinum immerses in the graphene solution of step (1), machinery
Take out nature after stirring 60 s to dry.In the graphene coated atomic force microscope probe being prepared into, graphene layer is 1 layer, thickness
It is 0.34 nm.
Embodiment 2
(1) preparation of graphene solution: 10 mg Graphenes are added in 1mL water, ultrasonic disperse in ultrasonic washing instrument
10 min, prepare the graphene solution that concentration is 10 mg/mL；
(2) graphene coated atomic force microscope probe is prepared: be that silicon nitride, cantilever and needle point are provided with platinoiridita by substrate
The needle point of the atomic force microscope probe of the single metal layer of alloy immerses in the graphene solution of step (1), after mechanical agitation 30s
Taking-up is dried naturally.In the graphene coated atomic force microscope probe prepared, graphene layer is 3 layers, and thickness is 1 nm.
Embodiment 3
(1) preparation of graphene solution: 7 mg Graphenes are added in 1 mL water, ultrasonic disperse in ultrasonic washing instrument
10 min, prepare the graphene solution that concentration is 7 mg/mL；
(2) graphene coated atomic force microscope probe is prepared: be that silicon, cantilever and needle point are provided with from the inside to the outside by substrate
The needle point of the atomic force microscope probe being respectively the double-metal layer of titanium and platinum immerses in the graphene solution of step (1), machinery
Take out nature after stirring 45 s to dry.In the graphene coated atomic force microscope probe prepared, graphene layer is 2 layers, thick
Degree is 0.68 nm.
Embodiment 4
(1) preparation of graphene solution: 7 mg Graphenes are added in 1 mL water, ultrasonic disperse in ultrasonic washing instrument
10 min, prepare the graphene solution that concentration is 7 mg/mL；
(2) graphene coated atomic force microscope probe is prepared: be that silicon, cantilever and needle point are provided with platinoiridita Dan Jin by substrate
The needle point of the atomic force microscope probe belonging to layer immerses in the graphene solution of step (1), takes out nature after mechanical agitation 45 s
Dry.In the graphene coated atomic force microscope probe prepared, graphene layer is 2 layers, and thickness is 0.68 nm.
Embodiment 5
CVD prepares Graphene AFM probe: ethanol is as carbon source, and gold is as catalyst, hydrogen and argon gaseous mixture conduct
Current-carrying gas.Ethanol is placed in low-temperature space, and gold-plated AFM probe is placed on high-temperature region (750-850 DEG C), is passed through in mark condition dirty
Speed is the gaseous mixture of 100 mL/min.After 5 minutes, form graphene layer in gold surface.
Embodiment 6
Etching-CVD prepares Graphene AFM probe: the method first step sodium hydroxide selective etch silicon chip, is formed
The oxide layer of heat, then the substrate deposited as Graphene in its surface plated with copper；Second step, by chemical vapour deposition technique at base
Continuous print graphene layer is obtained at the end；3rd step, uses SU-8 photoresist to fill needle point mould, is exposed development operation；The
Four steps, are passed through dry argon and remove surface and do not have a Graphene region of photoresist, meanwhile, spin coating second layer SU-8 photoresist with
Form the cantilever of probe.Finally, remove the silicon oxide etc. that the needle point back side is unnecessary, clean remainder, thus obtain whole AFM and visit
Pin.
Embodiment 7
Transfer method prepares Graphene AFM probe: first one layer of PMMA of spin coating on copper-base graphite alkene, rear ferric chloride is molten
Liquid etching copper substrate, obtains PMMA/ graphene layer with after hydrochloric acid and aqueous cleaning respectively；Conduction AFM probe is as receiving stone
The substrate of ink alkene, with acetone removes PMMA, finally after a period of time the driest (Graphene is attached to detecting probe surface) of drying in the air after transfer
Clean with water and i.e. can get the AFM probe that Graphene covers.
Characterization tool: scanning electron microscope (SEM), transmission electron microscope (TEM), conducting atomic force microscopy
(CAFM)
Characterizing method:
1) by the atomic force microscope of the double-metal layer being respectively titanium and platinum from the inside to the outside without graphene layer of preparation
Probe and graphene coated atomic force microscope probe carry out SEM and TEM morphology characterization, obtain corresponding image, therefrom can be clear
Observe that probe tip is by the contrast effect before and after graphene coated clearly.Fig. 1 and Fig. 2 finds out intuitively without graphene layer
The atomic force microscope probe tip wear degree of the double-metal layer being respectively titanium and platinum from the inside to the outside is very big, graphene coated
AFM probe tip wear degree is little.In Fig. 3, graphene sheet layer covers on needle point.
2) CAFM characterizes: cuprio single-layer graphene is as scanning sample, respectively with dividing from the inside to the outside without graphene layer
Not Wei the atomic force microscope probe of double-metal layer of titanium and platinum and the graphene coated utilizing technical measure to prepare former
Sub-force microscope probe carries out uninterrupted sweep test, under identical testing conditions, takes multiple scan until probe loses
Electric conductivity.
Can be seen that from Fig. 4 and Fig. 5 and be Ohmic contact between probe and sample, at the end of scan before scanning sample
Afterwards, between without atomic force microscope probe and the sample of double-metal layer being respectively titanium and platinum from the inside to the outside of graphene layer
Form higher Schottky barrier (tip wear degree is high), and graphene coated probe has relatively low Schottky barrier (needle point
The degree of wear is low), therefore, Graphene greatly reduces the degree of wear of probe, also can intuitively obtain this result from SEM figure.
Experimental result shows: the detectable total scan area of graphene coated AFM probe be free from graphene layer by interior
Total scan area 6-10 times that can record to the atomic force microscope probe of the outer double-metal layer being respectively titanium and platinum.Fig. 6 ratio
Compared with the atomic force microscope probe of the double-metal layer being respectively titanium and platinum from the inside to the outside without graphene layer with by not Tongfang
Total scan area cartogram that the Graphene AFM probe many experiments that method prepares draws, result shows, prepared by the technology of the present invention
The Graphene AFM probe that the electric conductivity entirety of Graphene AFM probe prepares higher than additive method and the plating without graphene layer
Graphene probe prepared by platinum-titanium atom force microscope probe and additive method, has the longest service life.
Claims (3)
1. a graphene coated atomic force microscope probe, including probe base, cantilever, needle point, it is characterised in that described
Cantilever and needle point are provided with metal level, and needle point is additionally provided with graphene layer；
Described metal level is double-metal layer, the most respectively titanium and platinum；Or described metal level is single metal layer, Dan Jin
Belong to for platinum and the alloy of iridium；
Described graphene layer is 1 to 3 layer, and thickness is 0.34-1 nm；
Described probe base is silicon or silicon nitride；
Described a kind of graphene coated atomic force microscope probe is prepared by following preparation method:
(1) preparation of graphene solution: 5-10 mg Graphene is added in 1mL water, ultrasonic disperse 10 in ultrasonic washing instrument
Min, prepares the graphene solution that concentration is 5-10 mg/mL；
(2) graphene coated atomic force microscope probe is prepared: cantilever and needle point are provided with the atomic force microscope of metal level
The needle point of probe immerses in the graphene solution of step (1), takes out nature and dry after mechanical agitation 30-60 s.
A kind of graphene coated atomic force microscope probe the most according to claim 1, it is characterised in that prepared by step (1)
Graphene solution in Graphene average-size less than 1 micron, thickness is 1-5 layer, and every layer thickness is 0.334 nanometer.
3. show in preparation atomic force according to the arbitrary described a kind of graphene coated atomic force microscope probe of claim 1 to 2
Purposes in micro mirror.
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| CN201410632559.6A CN104360107B (en) | 2014-11-12 | 2014-11-12 | A kind of graphene coated atomic force microscope probe and preparation method thereof, purposes |
| PCT/CN2014/093684 WO2016074305A1 (en) | 2014-11-12 | 2014-12-12 | Graphene-coated atomic force microscope probe and manufacturing method therefor and application thereof |
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| CN201410632559.6A CN104360107B (en) | 2014-11-12 | 2014-11-12 | A kind of graphene coated atomic force microscope probe and preparation method thereof, purposes |
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| Publication number | Publication date |
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| WO2016074305A1 (en) | 2016-05-19 |
| CN104360107A (en) | 2015-02-18 |
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