CN108375687A - A method of the coated graphite alkene on atomic force microscope probe needle point - Google Patents
A method of the coated graphite alkene on atomic force microscope probe needle point Download PDFInfo
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- CN108375687A CN108375687A CN201810195166.1A CN201810195166A CN108375687A CN 108375687 A CN108375687 A CN 108375687A CN 201810195166 A CN201810195166 A CN 201810195166A CN 108375687 A CN108375687 A CN 108375687A
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- force microscope
- atomic force
- graphene
- needle point
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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
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Abstract
The present invention relates to a kind of methods of the coated graphite alkene on atomic force microscope probe needle point, include the following steps:Take atomic force microscope probe, submerge in poly-D-lysine aqueous solution, submerged in graphene solution again after taking-up, after taking-up dry up to get.The present invention is interacted using the anion on the polycation and graphene of poly-D-lysine, increase the active force between atomic-force microscope needle-tip and graphene, the yield rate of the atomic force microscope probe needle point of the graphene coated prepared by infusion process greatly improves, and yield rate is up to 90% or more;Method raw material provided by the invention is easy to get, easy to operate, has extremely strong practical and popularizing value.
Description
Technical field
The present invention relates to the preparation fields of atomic force microscope, and in particular to one kind is on atomic force microscope probe needle point
The method of coated graphite alkene.
Background technology
Atomic force microscope (Atomic Force Microscope, AFM) is that one kind can be used to study and exist including insulator
The analytical instrument of interior solid material surface structure.The basic principle of atomic force microscope is:It is extremely sensitive to faint power by one
Micro-cantilever one end fix, the other end has a small needle point, needle point gently to be contacted with sample surfaces, due to needle point sophisticated atomic
There are faint repulsive forces between sample surfaces atom, micro- with needle point by controlling the constant of this power in scanning
Cantilever will rise and fall in the surface direction perpendicular to sample and transport corresponding to the equipotential surface of needle point and sample surfaces interatomic force
It is dynamic.Using optical detection or tunnel current detection method, the change in location that micro-cantilever corresponds to scanning each point can be measured, so as to
To obtain the information of sample surface morphology.
AFM probe be substantially by MEMS technology process Si or Si3N4 come prepare probe tip radiuses be generally 10 to
Tens nm.Micro-cantilever is usually by general 100~500 μm long and the μ m-thicks of about 500nm~5 a silicon chip or nitridation silicon chip system
At.Typical silicon micro-cantilever is about 100 μm long, 10 μm of wide, several microns thick.Using between probe and sample it is a variety of different mutually
The power of effect and the microscope for developing various different application fields, such as AFM (model moral supernatural power), electrostatic force microscope EFM (electrostatic
Power) magnetic force microscopy MFM (magnetostatic power) lateral force microscopy LFM (the lateral deflecting force of probe) etc., therefore have corresponding variety classes
Microscopical correspondent probe.Specifically, the probe of atomic force microscope is mainly the following:(1) non-contact/tapping-mode
Needle point and contact mode probe:Most common product, high resolution, service life are general.It is constantly ground using process middle probe
Damage, resolution ratio are easy to decline.Main application is observed with surface topography.(2) conducting probe:By plating 10-50 to average probe
The Pt (and other metal for improving binding force of cladding material, such as Cr, Ti, Pt and Ir etc.) of nanometer thickness is obtained.Conducting probe is applied to
EFM, KFM, SCM etc..The probe of conducting probe resolution ratio tapping and contact pattern is poor, and conductive coating is easy when use
It falls off, electric conductivity is difficult to keep for a long time.The new product of conductive pinpoint has carbon nano-tube point, diamond coating needle point, full Buddha's warrior attendant
Lithostyle point, all-metal silk needle point, these new technologies overcome the short life of common conductive needle point and the disadvantage that resolution ratio is not high.
(3) magnetic probe:Applied to MFM, by plating the ferromagnetic layers such as Co, Fe on the probe of common tapping and contact patterns
It prepares, resolution ratio average probe is poor, and conductive coating is easy to fall off when use.(4) big L/D ratio probe:Big L/D ratio needle point is
It aims at the side for measuring deep groove and approximate vertical and designs production.Feature:Less common product, resolution ratio is very
Height, service life are general.Technical parameter:Tip height>9μm;Draw ratio 5:1;Needle type radius<10nm.(5) diamond-like-carbon
AFM probe/full diamond probe:One is one layer of diamond-like carbon film is added in the tip portion of silicon probe, another is
Full diamond is prepared (price is very high).Both diamond carbon probes have prodigious durability, reduce the mill of needle point
Damage is to increase service life.
Be currently known there are many ways to coated graphite alkene on atomic-force microscope needle-tip, the dipping of most common of which
Method is that directly afm tip is immersed into graphene solution, and taking-up is dried to obtain the final product.Such as:Patent document CN104360107A is public
A kind of graphene coated atomic force microscope probe and preparation method thereof is opened;Its disclosed graphene coated atomic force microscope
Probe includes probe base, cantilever and needle point, and the cantilever and needle point are equipped with metal layer, graphene are additionally provided on needle point
Layer;The preparation method of the probe includes the following steps:(1) preparation of graphene solution:1mL water is added in 5-10mg graphenes
In, the graphene solution of a concentration of 5-10mg/mL is prepared in the ultrasonic disperse 10min in ultrasonic washing instrument;(2) it prepares
Graphene coated atomic force microscope probe:Cantilever and needle point are equipped with to the needle point leaching of the atomic force microscope probe of metal layer
In the graphene solution for entering step (1), naturally dry is taken out after mechanical agitation 30-60s.
However, since active force, that is, Van der Waals force between atomic-force microscope needle-tip and graphene is weaker so that soaking
In the presence of that there may be the case where needle point does not coat upper graphene in stain method, cause cladding yield rate relatively low.
Invention content
It is relatively low it is an object of the invention to be directed to existing liquid phase transfer law technology cladding atomic-force microscope needle-tip yield rate
The problem of, a kind of method of the coated graphite alkene on atomic force microscope probe needle point is provided.Graphene packet can be improved in this method
Cover the clad ratio and yield rate of atomic-force microscope needle-tip.
Specifically, the method for the coated graphite alkene provided by the invention on atomic force microscope probe needle point includes as follows
Step:Atomic force microscope probe is taken, is submerged in poly-D-lysine aqueous solution, without drying after taking-up, then is placed directly on stone
Submerged in black alkene solution, after taking-up dry up to get.
Method provided by the invention is applied widely, to the material of described atomic force microscope probe delivery date substrate itself without
Particular/special requirement.
A concentration of 0.001mg/ml~0.6mg/ml of the preferably described poly-D-lysine aqueous solution of the present invention, further preferably
For 0.001mg/ml~0.005mg/ml.The time submerged in the poly-D-lysine aqueous solution is preferably 10s~60s, more
Preferably 25~35s.
The present invention in the poly-D-lysine aqueous solution of above-mentioned certain concentration by soaking atomic force microscope probe
After not, material surface can be made fully modified, to improve the active force between atomic force microscope probe needle point and graphene.
For the graphene that the present invention uses without specifically limited, the number of plies is preferably 1~5 layer, most preferably single layer.The graphite
Water, ethyl alcohol, propyl alcohol, N-Methyl pyrrolidone or dimethylformamide etc. may be used in the solvent of alkene solution can be with dispersed graphite alkene
Organic solvent, present invention preferably employs aqueous solvents.
A concentration of 0.1mg/ml~the 2mg/ml, more preferably 0.8mg/ of the further preferably described graphene solution of the present invention
Ml~1.2mg/ml.The present invention is by largely putting into practice discovery, if graphene excessive concentration, can cause to coat on afm tip
Graphene is multilayer, accordingly increases the radius of curvature of needle point, can then reduce the resolution ratio of graphene coated needle point.Described
The time submerged in graphene solution is preferably 10s~60s, more preferably 25~35s.
Drying of the present invention is preferably dried up using nitrogen.
The present invention protects the atomic force microscope probe for the coated graphite alkene being prepared using the above method simultaneously.
The present invention further protects the atomic force microscope probe of the coated graphite alkene in preparing atomic force microscope
Application.
The present invention is interacted using the anion on the polycation and graphene of poly-D-lysine, increases atom
Active force between force microscope needle point and graphene passes through the atomic force microscope probe of graphene coated prepared by infusion process
The yield rate of needle point greatly improves, and yield rate preferably can reach 95% or more up to 90% or more;Method provided by the invention is former
Material is easy to get, easy to operate, has extremely strong practical and popularizing value.
Description of the drawings
Fig. 1 is the schematic diagram of 1 the method for embodiment;In Fig. 1 (a):1 is atomic force microscope probe, and 2 rely ammonia for poly
Aqueous acid, 4 be the culture dish or beaker for filling poly-D-lysine aqueous solution;In Fig. 1 (b):3 be graphene solution, and 5 be to fill
The culture dish or beaker of graphene solution.
Specific implementation mode
The following examples are used to illustrate the present invention, but are not intended to limit the scope of the present invention..
The atomic force microscope probe used in following embodiment is purchased from producer:NANOSENSORS, type:PPP-
CONTPt, commodity lot number:Lot.No.07/201.
The poly-D-lysine used in following embodiment is purchased from producer:Beijing SolarbioScience and
Technology Co.Ltd, Lot.No.20170920;
The graphene used in following embodiment is purchased from producer:First rich nanometer, article No.:100052.
Embodiment 1
A kind of method of the coated graphite alkene on atomic force microscope probe needle point is present embodiments provided, the method is shown
It is intended to as shown in Figure 1;Specially:
(1) poly-D-lysine is modified:Take the poly-D-lysine aqueous solution 2 of a concentration of 0.001mg/ml of 10mL in culture dish 4
In, atomic force microscope probe is immersed in the Poly-L-Lysine Solution 2 30 seconds, is taken out;
(2) impregnated graphite alkene solution:Take the graphene aqueous solution 3 of a concentration of 1mg/ml of 10mL 5 in culture dish in, will be through
Step (1) processing atomic force microscope probe be immersed in 3 in 30 seconds, take out, nitrogen drying to get.
Embodiment 2
A kind of method of the coated graphite alkene on atomic force microscope probe needle point is present embodiments provided, with embodiment 1
It compares, differs only in:A concentration of 0.01mg/ml of the poly-D-lysine aqueous solution.
Embodiment 3
A kind of method of the coated graphite alkene on atomic force microscope probe needle point is present embodiments provided, with embodiment 1
It compares, differs only in:A concentration of 0.5mg/ml of the poly-D-lysine aqueous solution, the graphene solution it is a concentration of
2mg/ml。
Comparative example
The method that the embodiment 1 of referenced patent document CN104360107A provides, in original identical with the various embodiments described above
Coated graphite alkene on sub- force microscope probe tip, specific method are:
(1) preparation of graphene solution:5mg graphenes are added in 1mL water, the ultrasonic disperse in ultrasonic washing instrument
The graphene solution of a concentration of 5mg/mL is prepared in 10min;
(2) graphene coated atomic force microscope probe is prepared:The needle point of atomic force microscope probe is immersed into step (1)
Graphene solution in, take out naturally dry after mechanical agitation 60s.
After testing, the graphene coated rate and products obtained therefrom that the various embodiments described above and comparative example the method can be realized
Graphene thickness it is as shown in table 1.
Table 1:Graphene coated result
Graphene coated rate (%) | Graphene thickness (nm) | |
Embodiment 1 | 95% | 0.44 |
Embodiment 2 | 93% | 1 |
Embodiment 3 | 95% | 1 |
Comparative example | 85% | 0.34 |
As seen from the results in Table 1, scheme provided by the present application can significantly improve graphite on atomic force microscope probe needle point
The clad ratio of alkene, and it is easy to operate, there is extremely strong promotional value.
Although above having used general explanation, specific implementation mode and experiment, the present invention is made to retouch in detail
It states, but on the basis of the present invention, it can be made some modifications or improvements, this is apparent to those skilled in the art
's.Therefore, these modifications or improvements without departing from theon the basis of the spirit of the present invention, belong to claimed
Range.
Claims (10)
1. a kind of method of the coated graphite alkene on atomic force microscope probe needle point, which is characterized in that include the following steps:It takes
Atomic force microscope probe is submerged in poly-D-lysine aqueous solution, is submerged in graphene solution again after taking-up, takes out after-blow
It is dry to get.
2. according to the method described in claim 1, it is characterized in that, a concentration of 0.001mg/ of the poly-D-lysine aqueous solution
Ml~0.6mg/ml.
3. according to the method described in claim 2, it is characterized in that, a concentration of 0.001mg/ of the poly-D-lysine aqueous solution
Ml~0.005mg/ml.
4. according to the method in claim 2 or 3, which is characterized in that submerged in the poly-D-lysine aqueous solution when
Between be 10s~60s, preferably 25s~35s.
5. according to the method described in Claims 1 to 4 any one, which is characterized in that the number of plies of the graphene is 1~5 layer,
Preferably 1 layer.
6. according to the method described in claim 5, it is characterized in that, the solvent of the graphene solution be water, ethyl alcohol, propyl alcohol,
N-Methyl pyrrolidone or dimethylformamide, preferably water.
7. according to the method described in claim 6, it is characterized in that, a concentration of 0.1mg/ml~2mg/ of the graphene solution
Ml, preferably 0.8mg/ml~1.2mg/ml.
8. according to the method described in claim 5~7 any one, which is characterized in that submerged in the graphene solution
Time is 10s~60s, preferably 25~35s.
9. using the atomic force microscope probe for the coated graphite alkene that claim 1~8 any one the method is prepared.
10. application of the atomic force microscope probe of coated graphite alkene described in claim 9 in preparing atomic force microscope.
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Cited By (3)
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CN113219211A (en) * | 2021-04-28 | 2021-08-06 | 西安交通大学 | Preparation method of nano probe |
CN114217097A (en) * | 2021-11-19 | 2022-03-22 | 国家纳米科学中心 | Preparation method of graphene functionalized silicon-based probe |
CN114354978A (en) * | 2021-11-17 | 2022-04-15 | 中南林业科技大学 | Device for preventing surface of atomic force microscope probe from generating bubbles and using method |
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Cited By (6)
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CN113219211A (en) * | 2021-04-28 | 2021-08-06 | 西安交通大学 | Preparation method of nano probe |
CN113219211B (en) * | 2021-04-28 | 2022-02-22 | 西安交通大学 | Preparation method of nano probe |
CN114354978A (en) * | 2021-11-17 | 2022-04-15 | 中南林业科技大学 | Device for preventing surface of atomic force microscope probe from generating bubbles and using method |
CN114354978B (en) * | 2021-11-17 | 2024-04-19 | 中南林业科技大学 | Device for avoiding bubble generation on surface of atomic force microscope probe and use method |
CN114217097A (en) * | 2021-11-19 | 2022-03-22 | 国家纳米科学中心 | Preparation method of graphene functionalized silicon-based probe |
CN114217097B (en) * | 2021-11-19 | 2024-03-05 | 国家纳米科学中心 | Preparation method of graphene functionalized silicon-based probe |
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