CN106324291A - Graphene film ball probe for atomic force microscopes and method of acquiring friction coefficient - Google Patents
Graphene film ball probe for atomic force microscopes and method of acquiring friction coefficient Download PDFInfo
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- CN106324291A CN106324291A CN201610669303.1A CN201610669303A CN106324291A CN 106324291 A CN106324291 A CN 106324291A CN 201610669303 A CN201610669303 A CN 201610669303A CN 106324291 A CN106324291 A CN 106324291A
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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
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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
- G01Q60/26—Friction force microscopy
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- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
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Abstract
The invention provides a graphene film ball probe for atomic force microscopes, comprising a cantilever and a tip, wherein the tip comprises a spherical base and a graphene layer, and the graphene layer coats the surface of the spherical base and directly contacts the spherical base. The invention further provides a method of acquiring an interlayer friction coefficient by use of the graphene film ball probe. The graphene film ball probe and the method of acquiring an interlayer friction coefficient by use of the graphene film ball probe have excellent wear resistance.
Description
Technical field
The present invention relates to a kind of probe for atomic force microscope and the method utilizing this probe to obtain coefficient of friction, especially
It relates to a kind of graphene film talent scout's pin and the method utilizing this graphene film talent scout's pin to obtain interfacial friction coefficient.
Background technology
Friction between the surface and interface of moving component generally can cause the inefficacy of the even parts of wearing and tearing.Component of machine
Abrasion and the energy of friction loss more highlight the realistic meaning of friction, lubrication.Hydrodynamic lubrication material is due to the limitation of itself
Property, easily lost efficacy under the severe rugged environment such as low speed, extreme pressure.The introducing of solid lubrication, breaches the film lubrication limit, in poles such as spaces
Under end occasion, demonstrate huge superiority.For micro electronmechanical (MEMS) system of super hot investment casting, due to the reduction of size,
The gap of friction pair is generally at nanoscale, and the now appearance of nanostructured solid lubricating film, mill drops in the anti-attrition at MEMS system
Field is widely used.
Exploration to Nanotribology is mainly based upon atomic force microscope (AFM), is possible not only to realize nano-grade size
With receive the measurement of the micro-power of cattle level, and the information such as three-dimensional appearance can be obtained, it is achieved for the measurement of process simultaneously.But, by
Abrasion it is easy to so that the life-span of probe is shorter and resolution is the highest, causes micro-power under common afm tip is at contact mode
Measurement error so that measurement result precision is the highest.
Summary of the invention
In sum, a kind of atomic force microscope probe with high measurement accuracy of necessary offer and coefficient of friction
Acquisition methods.
A kind of graphene film talent scout's pin for atomic force microscope, including a cantilever and a needle point, wherein, described needle point
Including a spherical substrate and a graphene layer, described graphene layer is coated on the surface of described spherical substrate, described graphene layer
In be pure Graphene.
Wherein in an embodiment, described graphene layer includes that multi-layer graphene film, the number of plies of described graphene film are
3-10 layer, the thickness of every layer graphene film is that 1 nanometer is to 3 nanometers.
Wherein in an embodiment, described graphene layer is coated with described spherical substrate completely, and described graphene layer by
Pure Graphene forms, and does not contains functional group.
Wherein in an embodiment, the material of described spherical substrate is silicon oxide, and described graphene layer is directly coated on
The outer surface of the spherical substrate of described silicon oxide.
Wherein in an embodiment, a diameter of 5 microns to 10 microns of described spherical substrate.
A kind of method utilizing graphene film talent scout's pin as above to obtain coefficient of friction, including:
A substrate, the surface of described substrate is provided to have a carbon material layer；
The graphene layer of graphene film ball probe tip is contacted carbon material layer, applies initial load to needle point, and just
Under beginning load effect, rub back and forth needle point on carbon material layer surface, it is thus achieved that first group of voltage signal of needle point lateral twisting, and leads to
Cross first group of voltage signal and obtain the first interfacial friction between graphene layer and carbon material layer；
Changing the size of load, rub back and forth needle point again on the surface of carbon material layer, it is thus achieved that second group of voltage signal, and
The second interfacial friction is obtained by second group of voltage signal；
By that analogy, by again changing the size of load, obtain N group interfacial friction, wherein N >=2 altogether, and then obtain
N group interfacial friction, with the curve of load change, obtains rubbing between graphene layer and carbon material layer by the described slope of curve
Wipe coefficient.
Wherein in an embodiment, the material of described carbon material layer is graphite or Graphene.
Wherein in an embodiment, described needle point is perpendicular to prolonging of described cantilever relative to the frictional direction of carbon material layer
Stretch direction.
Wherein in an embodiment, N is less than or equal to 100 more than or equal to 10.
Wherein in an embodiment, described graphene film talent scout's pin and described carbon material layer are arranged in liquid medium,
Described graphene film talent scout's pin is carried out all the time in the process of the mantle friction of described carbon material layer in liquid medium.
Compared with prior art, by Graphene being directly coated on the surface of needle point so that graphene film talent scout's pin
There is the wear resistance of excellence, it is possible to reduce the adhesion between probe and other surfaces, and there is extraordinary moisture-proof
Degree performance, during so that utilize this graphene film ball probe measurement interfacial friction, has the highest certainty of measurement and use
In the life-span, adaptability is good.
Accompanying drawing explanation
The structural representation of the graphene film talent scout's pin for atomic force microscope that Fig. 1 provides for the embodiment of the present invention.
Fig. 2 is the electromicroscopic photograph of the graphene film talent scout's pin described in Fig. 1.
Fig. 3 is the electromicroscopic photograph of graphene layer in the graphene film talent scout's pin described in Fig. 1.
Fig. 4 for the embodiment of the present invention provide utilize graphene film talent scout's pin obtain coefficient of friction schematic diagram.
The graphene film talent scout's pin recorded under the different loads that Fig. 5 provides for the embodiment of the present invention and conventional probe respectively with
The comparison diagram of the coefficient of friction between graphite.
Graphene film talent scout's pin that Fig. 6 provides for the embodiment of the present invention and the wear resistance schematic diagram of conventional probe.
Fig. 7 is the frictional force between graphene film talent scout's pin and the graphite that the embodiment of the present invention records under different humidity
Schematic diagram.
Main element symbol description
Graphene film talent scout's pin 100
Cantilever 10
Needle point 20
Spherical substrate 21
Graphene layer 22
Substrate 200
Carbon material layer 30
Specific examples below will further illustrate the present invention in conjunction with above-mentioned accompanying drawing.
Detailed description of the invention
The graphene film talent scout's pin for atomic force microscope that the present invention provides is described in detail below with reference to accompanying drawing, and
Utilize the method that this graphene film talent scout's pin obtains coefficient of friction.For convenience of describing, first the present invention introduces and shows for atomic force
Graphene film talent scout's pin of micro mirror.
Seeing also Fig. 1 to Fig. 3, the embodiment of the present invention provides a kind of graphene film talent scout's pin 100, described graphene film
Talent scout's pin 100 includes that a cantilever 10 and needle point 20, described needle point 20 include spherical substrate 21 and a graphene layer 22, a described ball
Shape substrate 21 is a chondritic.
Concrete, that described spherical substrate 21 is formed for homogenous material spherical entity structure.The material of described spherical substrate 21
Material can be metal, nonmetal, high molecular polymer etc., as long as Graphene can be carried and for hard material, and such as gold, oxygen
The hard materials such as SiClx, carborundum, silicon nitride, polystyrene, can select as required.In the present embodiment, described ball
The material of shape substrate 21 is silicon oxide, and the most described graphene layer 22 can directly be coated on described silicon oxide spherical substrate 21 table
Face, and directly contact with described spherical substrate 21.Preferably, described graphene layer 22 is coated on the whole of described spherical substrate 21
Surface.Concrete, described graphene layer 22 can be directly grown in the surface of described spherical substrate 21, thus with described spherical substrate
The surface of 21 directly contacts, it is to avoid functional group and the impact of other impurity.Being shaped as of described spherical substrate 21 is spherical, described ball
The diameter of shape substrate 21 can be that 10 nanometers are to 100 microns.Preferably, a diameter of 5 microns to 10 microns of described spherical substrate 21,
Make described needle point 20 be easier to preparation, and be more beneficial for the measurement of follow-up interfacial friction.It is appreciated that described spherical base
The shape at the end 21 is alternatively elliposoidal, and described ellipsoid one pair of which claims axle to be parallel to the bearing of trend of described cantilever 10.
Described graphene layer 22 includes that at least one single layer graphene film, the number of plies of described graphene layer 22 can be 3-10 layer,
The thickness of described graphene layer 22 can be 1 nanometer to 3 nanometers so that described graphene layer 22 is easier to preparation, and reduce
The influence of crust deformation of probe.Described graphene film is a continuous print monolayer carbon atomic layer, i.e. single-layer graphene, and thickness is 0.34 to receive
Rice.Preferably, described Graphene once 22 the number of plies less than or equal to 4 layers, on the one hand can reduce cost, reduce preparation difficulty, separately
On the one hand, stablizing of graphene layer 22 in follow-up friction process can be kept, effectively prevent the number of plies from too much causing in friction process
Come off.Further, described graphene layer 22 is made up of pure Graphene, contains only pure Graphene in described graphene layer 22, and
And described pure Graphene contains only carbon atom, without other impurity and functional group such that it is able to reduce the impact of other impurity,
Avoid the adsorption of other impurity such as functional group, improve follow-up certainty of measurement.Further, due to described graphene layer 22 by
Pure Graphene is constituted, and the most described graphene layer 22 can firmly be coated on the surface of described spherical substrate 21, it is possible to effectively keeps away
Exempt from coming off during follow-up measurement.
Described graphene layer 22 continuous print is coated on the surface of described spherical substrate 21, and straight with described spherical substrate 21
Contact, thus the spherical gapless cladding of substrate 21 is got up.Described needle point 20 is positioned at one end of described cantilever 10.Specifically
, described needle point 20 can be attached at the surface of described cantilever 10 by a tack coat (not shown).Due in needle point 20, described stone
The surface being coated on spherical substrate 21 of ink alkene layer 22 entirety, the most described graphene layer 22 is by tack coat and described cantilever 10
Intimate surface contact, thus needle point 20 entirety is firmly fixed to one end of described cantilever 10.
Referring to Fig. 4, the embodiment of the present invention also provides for one and utilizes described graphene film talent scout's pin 100 to obtain coefficient of friction
Method, comprise the steps:
Step S10 a, it is provided that substrate 200, the surface of described substrate 200 has a carbon material layer 30；
Step S20, contacts carbon material layer 30 by graphene film talent scout's pin 100, applies initial load to needle point 20, and just
Under beginning load effect, rub back and forth needle point 20 on carbon material layer 30 surface, it is thus achieved that first group of electricity that needle point 20 lateral twisting produces
Pressure signal, and obtain the first interfacial friction by first group of voltage signal；
Step S30, changes the size of load, and rub back and forth needle point 20 again on the surface of carbon material layer 30, it is thus achieved that second
Group voltage signal, and obtain the second interfacial friction by second group of voltage signal；
Step S40, by that analogy, by again changing the size of load, it is thus achieved that N group interfacial friction, N >=2, and obtains
N group frictional force, with the curve of load change, obtains between graphene layer and carbon material layer 30 by analyzing the described slope of curve
Coefficient of friction.
In step slo, the surface of described substrate 200 is a plane, and described carbon material layer 30 entirety is attached at described base
On the surface of plate 200.Described carbon material layer 30 material can be the one in graphite, Graphene, and the list of described carbon material layer is former
Sublayer is two dimension six-membered ring structure.Described carbon material layer 30 entirety is attached at the surface of described substrate 200, described material with carbon element
The thickness of layer 30 does not limits, as long as ensureing that the surface entirety of described substrate 200 can be covered by described carbon material layer 30.
In step S20, described graphene film talent scout's pin 100 can be according to need relative to the frictional direction of carbon material layer 30
Select, if guarantee to get needle point 20 with the frictional force that is subject in the friction of carbon material layer 30.Tool
Body, if the bearing of trend of cantilever 10 is X-direction, it is perpendicular to X-direction and to be parallel to the direction on substrate 200 surface be Y-direction, then
The frictional direction of described needle point 20 and X-direction form an angle theta, and described θ is less than or equal to 90 degree more than 0 degree.Preferably, described pin
The frictional direction of point 20 is perpendicular to the bearing of trend of described cantilever 10, and the angle theta i.e. formed with X-direction is 90 degree such that it is able to
Be more prone to the get signal of telecommunication that the lateral twisting that needle point 20 is subject to produces, and then the convenient frictional force that obtains, and
And ensure subsequent calculations and the accuracy of result of calculation.It can be voltage signal or electric current that described needle point 20 reverses the signal of telecommunication produced
Signal, can obtain, by a magnetic levitation equipment (not shown), the voltage signal that needle point 20 lateral twisting produces, and be calculated
The first interlayer between the size of the frictional force between needle point 20 and carbon material layer 30, namely graphene layer 22 and carbon material layer 30
The size of frictional force.
The computational methods of described frictional force may utilize frictional force ring.It is past that frictional force ring refers to that afm scan obtains
Two sections of multiple force signals, the computational methods of frictional force are to subtract each other the force signal of drag ring divided by 2.
In step S30 to step S40, by changing load, and then change rubbing between needle point 20 and carbon material layer 30
The size of wiping power.The voltage signal produced by exploratory probe lateral twisting again, can be by being calculated needle point 20 and carbon material
The size of the second interfacial friction between the size of frictional force, namely graphene layer 22 and carbon material layer 30 between the bed of material 30.Logical
Cross the first interfacial friction and the second interfacial friction can tentatively obtain the friction between graphene layer 22 and carbon material layer 30
The size of coefficient.Further, for obtaining more accurate result, the size of load can be varied multiple times, and then detection obtains N group voltage
Signal, thus obtain the N group interfacial friction curve with load change.By analyzing frictional force-curve of load slope,
To coefficient of friction.Further, described N can be more than or equal to 10 less than or equal to 100, on the one hand it can be avoided that obtain when data are very few
Frictional force-curve of load slope inaccurate, the difficulty calculated when on the other hand also reducing too much number of times and to Graphene
The abrasion of layer 22.During changing load, the difference that can fix changes magnitude of load, it is also possible to enter according to actual needs
Row selects.It addition, during friction, the angle repeatedly rubbed can keep consistent.
Refer to Fig. 5, the present embodiment uses graphite as carbon material layer 30, measure the graphite under 16 groups of different loads
Frictional force between alkene film talent scout's pin and graphite, and contrast the coefficient of friction between silicon oxide and graphite and graphene film talent scout
Coefficient of friction between pin and graphite.From in figure, when employing silicon oxide bead probe, directly and graphite is to when rubbing, and friction is
Number is 0.046.And when using graphene film talent scout's pin and graphite to when rubbing, it is thus achieved that coefficient of friction be reduced to 0.003, i.e. reach
Superslide state (coefficient of friction is less than 0.01).
Further, seeing also Fig. 6, the stability of described graphene film talent scout's pin is carried out by the present embodiment further
Test.Described graphene film talent scout's pin rubs at the same position of graphite, up to two hours repeatedly with the contact stress of 1Gpa
Superslide just lost efficacy afterwards, it was demonstrated that described graphene film talent scout is capable of stable superslide state for graphite.It addition, when this position
After the superslide state put lost efficacy, when described graphene film talent scout's pin is moved to new position, still it is obtained in that superslide, thus
Prove that described graphene film talent scout's pin especially needle point has the most excellent wear resistance.
It addition, refer to Fig. 7, the moisture resistance performance of described graphene film talent scout's pin is surveyed by the present embodiment further
Examination.By steam and nitrogen are passed through environmental chamber with predetermined ratio, obtain different humidity, resistance to graphene film talent scout's pin
Psychometric performance is tested.By in Fig. 7 it can be seen that described graphene film talent scout's pin is in the environment that humidity is 31.8%, phase
When being 1 micron to 10 microns for the displacement of graphite, all it is able to maintain that superslide state；It addition, described graphene film talent scout
Between pin and graphite when humidity is up to 51%, remain able to maintain superslide state, thus prove described graphene film talent scout's pin
There is extraordinary moisture resistance, and still there is in the case of high humility the wear resistance of excellence.
Graphene film talent scout's pin that the present invention provides and utilize the method that this graphene film talent scout's pin obtains coefficient of friction is logical
Cross the surface that Graphene is directly coated on tradition needle point so that graphene film talent scout's needle set has the wear resistance of excellence, energy
Enough reduce the adhesion between probe and other surfaces, and there is extraordinary moisture resistance performance, so that utilize this stone
During ink alkene film ball probe measurement interfacial friction, having the highest certainty of measurement and service life, adaptability is good, especially at tide
Wet or liquid medium still has the highest certainty of measurement so that described graphene film talent scout's needle set has wide application empty
Between, and can and carbon material layer between reach the state of superslide.
Each technical characteristic of embodiment described above can combine arbitrarily, for making description succinct, not to above-mentioned reality
The all possible combination of each technical characteristic executed in example is all described, but, as long as the combination of these technical characteristics is not deposited
In contradiction, all it is considered to be the scope that this specification is recorded.
Embodiment described above only have expressed the several embodiments of the present invention, and it describes more concrete and detailed, but also
Therefore the restriction to the scope of the claims of the present invention can not be interpreted as.It should be pointed out that, for those of ordinary skill in the art
For, without departing from the inventive concept of the premise, it is also possible to make some deformation and improvement, these broadly fall into the guarantor of the present invention
Protect scope.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (10)
1. for graphene film talent scout's pin of atomic force microscope, including a cantilever and a needle point, it is characterised in that described
Needle point includes a spherical substrate and a graphene layer, and described graphene layer is coated on the surface of described spherical substrate, described graphite
It alkene layer is pure Graphene.
2. the graphene film talent scout's pin for atomic force microscope as claimed in claim 1, it is characterised in that described Graphene
Layer includes that multi-layer graphene film, the number of plies of described graphene film are 3-10 layer, and the thickness of every layer graphene film is that 1 nanometer is received to 3
Rice.
3. the graphene film talent scout's pin for atomic force microscope as claimed in claim 1, it is characterised in that described Graphene
Layer is coated with described spherical substrate completely, and described graphene layer is made up of pure Graphene, does not contains functional group.
4. the graphene film talent scout's pin for atomic force microscope as claimed in claim 1, it is characterised in that described spherical base
The material at the end is silicon oxide, and described graphene layer is directly coated on the outer surface of the spherical substrate of described silicon oxide.
5. the graphene film talent scout's pin for atomic force microscope as claimed in claim 1, it is characterised in that described spherical base
A diameter of 5 microns to 10 microns of the end.
6. utilize in claim 1-5 the method that the graphene film talent scout's pin described in any one obtains coefficient of friction, bag
Include:
A substrate, the surface of described substrate is provided to have a carbon material layer；
The graphene layer of graphene film ball probe tip is contacted carbon material layer, applies initial load to needle point, and carry initial
Under lotus effect, rub back and forth needle point on carbon material layer surface, it is thus achieved that first group of voltage signal of needle point lateral twisting, and by the
One group of voltage signal obtains the first interfacial friction between graphene layer and carbon material layer；
Changing the size of load, rub back and forth needle point again on the surface of carbon material layer, it is thus achieved that second group of voltage signal, and passes through
Second group of voltage signal obtains the second interfacial friction；
By that analogy, by again changing the size of load, obtain N group interfacial friction, wherein N >=2 altogether, and then obtain N group
Interfacial friction, with the curve of load change, obtains the friction system between graphene layer and carbon material layer by the described slope of curve
Number.
7. the method obtaining coefficient of friction as claimed in claim 6, it is characterised in that the material of described carbon material layer is graphite
Or Graphene.
8. the method obtaining coefficient of friction as claimed in claim 6, it is characterised in that described needle point is relative to carbon material layer
Frictional direction is perpendicular to the bearing of trend of described cantilever.
9. the method obtaining coefficient of friction as claimed in claim 6, it is characterised in that N is less than or equal to 100 more than or equal to 10.
10. the method obtaining coefficient of friction as claimed in claim 6, it is characterised in that described graphene film talent scout's pin and institute
Stating carbon material layer to be arranged in liquid medium, described graphene film talent scout's pin begins in the process of the mantle friction of described carbon material layer
Carry out in liquid medium eventually.
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| CN108375687A (en) * | 2018-03-09 | 2018-08-07 | 北京协同创新研究院 | A method of the coated graphite alkene on atomic force microscope probe needle point |
| CN108845161A (en) * | 2018-03-21 | 2018-11-20 | 清华大学 | The preparation method of atomic force microscope probe, atomic force microscope and probe |
| CN109030870A (en) * | 2018-07-19 | 2018-12-18 | 清华大学 | Two-dimensional layer material wraps up atomic force microscope probe and preparation method thereof and application |
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| CN110749752A (en) * | 2019-10-12 | 2020-02-04 | 清华大学 | Two-dimensional material probe for atomic force microscope and preparation method and application thereof |
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| CN108375687A (en) * | 2018-03-09 | 2018-08-07 | 北京协同创新研究院 | A method of the coated graphite alkene on atomic force microscope probe needle point |
| CN108845161A (en) * | 2018-03-21 | 2018-11-20 | 清华大学 | The preparation method of atomic force microscope probe, atomic force microscope and probe |
| CN109030870A (en) * | 2018-07-19 | 2018-12-18 | 清华大学 | Two-dimensional layer material wraps up atomic force microscope probe and preparation method thereof and application |
| CN110735286A (en) * | 2018-07-20 | 2020-01-31 | 青岛海尔洗衣机有限公司 | friction force detection device, washing machine and control method thereof |
| CN110735286B (en) * | 2018-07-20 | 2023-04-11 | 青岛海尔洗衣机有限公司 | Friction force detection device, washing machine and control method of washing machine |
| CN110749752A (en) * | 2019-10-12 | 2020-02-04 | 清华大学 | Two-dimensional material probe for atomic force microscope and preparation method and application thereof |
| CN111439746A (en) * | 2020-05-20 | 2020-07-24 | 东华大学 | Preparation method of single-layer graphene folding structure with controllable torsion angle |
| CN111439746B (en) * | 2020-05-20 | 2021-07-23 | 东华大学 | Preparation method of single-layer graphene folding structure with controllable torsion angle |
| CN113686732A (en) * | 2021-07-27 | 2021-11-23 | 清华大学 | Platform liquid drop probe, preparation method thereof and liquid drop friction force and normal force detection method |
| CN113686732B (en) * | 2021-07-27 | 2022-04-22 | 清华大学 | Platform liquid drop probe, preparation method thereof and liquid drop friction force and normal force detection method |
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