CN108414435A - A method of graphene surface friction coefficient is regulated and controled by surface limited effect - Google Patents
A method of graphene surface friction coefficient is regulated and controled by surface limited effect Download PDFInfo
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- CN108414435A CN108414435A CN201810058232.0A CN201810058232A CN108414435A CN 108414435 A CN108414435 A CN 108414435A CN 201810058232 A CN201810058232 A CN 201810058232A CN 108414435 A CN108414435 A CN 108414435A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N19/00—Investigating materials by mechanical methods
- G01N19/02—Measuring coefficient of friction between materials
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/194—After-treatment
Abstract
The present invention provides a kind of methods regulating and controlling graphene surface friction coefficient by surface limited effect, include the following steps：Copper platinum of the surface with PMMA/ graphene films is etched with iron nitrate solution；Obtained PMMA/ graphene films are put into distilled water and are cleaned；Anodic alumina film is picked up upwards below PMMA/ graphene films, being heated after its drying makes graphene film flatten；Carried out acetone bath；Friction measurement is carried out under contact mode with atomic force needle point；The average transverse power that output voltage provides is converted to the frictional force generated due to the torsion of cantilever；Measure instantaneous desorption force curve；Molecular dynamics simulation is carried out, the change curve of frictional force and normal load is obtained；Calculate interaction energy when tip is above scanned on the surface of graphene.The present invention, which uses, has clear boundary, specifies the AAO templates of the nano-pore structure of structure to support graphene, receives the control of micro-friction with the basic process and realization by AFM nano-scale grade frictions.
Description
Technical field
The invention belongs to graphene film tribology technology fields, more particularly to a kind of to regulate and control stone by surface limited effect
The method of black alkene skin-friction coefficient.
Background technology
It is well known that nano level rub is unfavorable for working efficiency, the output power of micro-/ nano Mechatronic Systems (M/NEMS)
And application reliability.Hydrodynamic lubrication be minimize the usual method of sliding interface friction, but under nano-micro scale two it is relatively sliding
Shear pressure between dynamic contact surface can make liquid be squeezed out contact area easily, so as to cause direct solid-solid interface
Contact the increase so that adhesion strength and frictional force.As substitute strategy, two-dimentional graphene material can be made very thin
Solid lubricant.Friction between the single layer and bilayer graphene film of SiC substrate support shows significant difference, this difference
The significant reduction that Electron-phonon couples in the different bilayer for being interpreted to disclose by angle resolved photoelectron spectroscope.It moreover has been found that rubbing
It wipes as graphene film is from single layer to the increase of multilayer and monotone decreasing, is combined with support substrate weaker.Film corrugation effect
It is considered as the reason of causing graphene layer frictional behavior, it is considerable in order to avoid that may cause by using atomic force microscope
The abrasion of the surface damage observed so that the significant difference of subsequent rub measurement, 11 relatively thin graphene planes are to find ratio
Thicker is easier to be layered.This layering causes the graphene layer around AFM tip to be put down due to tip-graphene adherency
Out-of-plane deformation, to generate the contact area and therefore higher frictional force of bigger.It is worth noting that, corrugation caused by bonding
Mechanism may the performance difference of the contact with larger.However, being found in molecular dynamics simulation, larger tip (2.5 or 30nm
Radius) influence to frictional force is much greater, to provide the contact area of bigger.By being fluorinated on graphene,
It can mainly be influenced by the most soft bending phonon of bending stiffness out of plane or graphene with regulating friction force to 6 times.It is specific and
Speech, elastic graphite alkene piece snap into tip due to adherency, and if sheet material is sufficiently thin and part wrinkles, from connecing for deformity out of plane
Touching region needs more power by tip forward slip.For thicker graphene film, i.e. graphite, due to the bending stiffness of piece
It is larger, fold unobvious, therefore it is relatively low to rub.However, because ink sheet material is micron or millimetre-sized, and point between M/NEMS
It can be from 1 μm/100nm to contact, so graphite is not suitable as the lubricant of M/NEMS from range.I.e. nano level lubricating film
Be it is very promising, and graphene film by be nanoscale lubricating film ideal chose.Nevertheless, graphene interface atomic structure
(including out-of-plane deformation) and adherency, the correlation between friction is still challenging, although numerous studies nanoscale scape
It sees and the influence graphene of machinery and interface behavior is had been completed.Therefore, this needs to further investigate graphene, this will
Promote the understanding to originate from all to adhering to and rubbing, and leads to its implementation in following M/NEMS devices.
Invention content
Technical problem：In order to solve the defects of prior art, the present invention provides one kind is regulated and controled by surface limited effect
The method of graphene surface friction coefficient.
Technical solution：A kind of side regulating and controlling graphene surface friction coefficient by surface limited effect provided by the invention
Method, it is characterised in that：Include the following steps：
Step 1：Graphene shifts
Step 1.1：Copper platinum of the surface with PMMA/ graphene films is etched with iron nitrate solution, until PMMA/ graphene films
Float to solution surface；
Step 1.2：PMMA/ graphene films are picked up to be put into distilled water and clean 10min, to wash nitre remaining on film
Sour ferrous solution；
Step 1.3：One piece of anodic alumina film is picked up with tweezers, is picked up upwards below PMMA/ graphene films, obtains sun
Pole alumina-supported PMMA/ graphene films；
Step 1.4：Step 3 is obtained into anodic alumina support PMMA/ graphene films and is statically placed in air drying；
Step 1.5：Heating is so that graphene film flattens；
Step 1.6：Acetone bath obtains anodic alumina support graphene film to remove the PMMA on surface；
Step 2：Tribology tester
Step 2.1：Using Dimension Icon AFM instruments, SNL-10 (tip radius 2nm) atomic force needle point is selected
Friction measurement is carried out under contact mode；
Step 2.2：The normal spring constant that needle point tip is calibrated using the deflection sensitivity of supporting cantilever, will be normal
Load signal is converted to real normal load ox from volt, and calibration process is had to carry out when using different cantilevers；
Step 2.3：The average transverse power that output voltage provides is converted to the frictional force generated due to the torsion of cantilever, and
Acquisition average value is taken multiple measurements in multiple sample positions；
Step 2.4：Instantaneous desorption force curve is measured, to obtain adherency force parameter；
Step 3：Molecular simulation
Step 3.1：Molecular dynamics is carried out using the nano-diamond tip slided on the graphene film that AAO is supported
Simulation, obtains the change curve of frictional force and normal load, and demonstrating has specific nanometer on the single-layer graphene of AAO supports
The friction in hole is less than the conclusion of the friction on multi-layer graphene, double-deck according to single layer, the deformation of three layers and multi-layer graphene system
Curve, frictional force is increased the reason is that part " corrugation " effect when demonstrating graphene thickness increase on AAO；
Step 3.2：Calculating tip on the graphene surface that AAO is supported when scanning between graphene layer and AAO substrates
Interaction energy, has probed into the reason of local " corrugation " acts on, stronger mutual between single-layer graphene and AAO to demonstrate
The theory of effect.
As a kind of prioritization scheme：Iron nitrate concentration is 0.27g/mL in iron nitrate solution described in step 1.1.
As advanced optimizing scheme：PMMA/ graphene films are put into distilled water described in step 1.2 and clean 3 times, every time
Scavenging period is 10min.
As advanced optimizing scheme：Step 1.4 drying time is 30min.
As advanced optimizing scheme：Step 1.5 heating temperature is 80 DEG C, heating time 30min.
As advanced optimizing scheme：It is repeatedly 5 times that step 2.4, which measures,.
Advantageous effect：Single layer is suspended in the friction on anodised aluminium (AAO) to multi-layer graphene and is increased monotonically, and this
Trend is in the graphene layer that flat copper foil supports on the contrary, friction coefficient smaller under achieving the effect that smaller szie；
No matter how scanning distance shows uniform friction profile to the single-layer graphene of AAO supports, and double-deck and three
Gradually increased trend is presented with the increase of sliding distance in layer graphene；This " inclined drag ring " obviously appears on AAO
Multi-layer graphene friction profile on；
The frictional strength for obtaining the single-layer graphene on the frictional strength ratio AAO of the multi-layer graphene on AAO is high by about two
Result again.
Description of the drawings
Fig. 1 is Raman spectrogram of the graphene film 514nm at of AAO loads and graphene layer that AAO is supported and pure
The surface topography map of AAO base materials；
Fig. 2 be copper-base graphite alkene film sample under the different numbers of plies, the column analysis chart of skin-friction force and adhesion strength.
Specific implementation mode
In the following with reference to the drawings and specific embodiments, the present invention is furture elucidated, it should be understood that these embodiments are merely to illustrate
It the present invention rather than limits the scope of the invention, after having read the present invention, those skilled in the art are to of the invention each
The modification of kind equivalent form falls within the application range as defined in the appended claims.
Embodiment 1
Step 1：Graphene shifts
Step 1.1：Copper platinum of the surface with PMMA/ graphene films is etched with iron nitrate solution, until PMMA/ graphene films
Float to solution surface.Iron nitrate solution a concentration of 0.27g/mL in distilled water；
Step 1.2：PMMA/ graphene films are picked up and are put into 10min in distilled water, and in triplicate, to wash on film
Remaining iron nitrate solution；
Step 1.3：One piece of anodic alumina film is picked up with tweezers, is picked up upwards below PMMA/ graphene films, obtains sun
Pole alumina-supported PMMA/ graphene films；
Step 1.4：Step 3 is obtained into anodic alumina support PMMA/ graphene films and is statically placed in air drying 30min；
Step 1.5：80 DEG C of heating 30min are so that graphene film flattens；
Step 1.6：Acetone bath obtains anodic alumina support graphene film to remove the PMMA on surface.
Step 2：Tribology tester
Step 2.1：Using Dimension Icon AFM instruments, SNL-10 (tip radius 2nm) atomic force needle point is selected
Friction measurement is carried out under contact mode；
Step 2.2：The normal spring constant that needle point tip is calibrated using the deflection sensitivity of supporting cantilever, will be normal
Load signal is converted to real normal load ox from volt, and calibration process is had to carry out when using different cantilevers；
Step 2.3：The average transverse power that output voltage provides is converted to the frictional force generated due to the torsion of cantilever；
Step 2.4：Five times, which are carried out, in multiple sample positions measures acquisition average value；
Step 2.5：Instantaneous desorption force curve is measured, to obtain adherency force parameter.
Step 3：Molecular simulation
Step 3.1：Molecule power has been carried out using the nano-diamond tip slided on the graphene film that AAO is supported
Learn simulation；
Step 3.2：The change curve of frictional force and normal load is obtained, demonstrates and has on the single-layer graphene of AAO supports
There is conclusion of the friction less than the friction on multi-layer graphene of specific nano-pore；
Step 3.3：Double-deck according to single layer, the deformation curve of three layers and multi-layer graphene system demonstrates graphite on AAO
Frictional force is increased the reason is that part " corrugation " effect when alkene thickness increases；
Step 3.4：Calculating tip on the graphene surface that AAO is supported when scanning between graphene layer and AAO substrates
Interaction energy, has probed into the reason of local " corrugation " acts on, stronger mutual between single-layer graphene and AAO to demonstrate
The theory of effect.
Embodiment 2
By the anodic oxidation aluminium substrate in the step 1.1 of embodiment 1, it is changed to even mesoporous polymer R/HMTA-0.3,
He is consistent condition.
Embodiment 3
By the anodic oxidation aluminium substrate in the step 1.1 of embodiment 1, titanium oxide nanotubes are changed to, other conditions keep one
It causes.
Embodiment 4
By the anodic oxidation aluminium substrate in the step 1.1 of embodiment 1, it is changed to titanium sheet, other conditions are consistent.
Embodiment 5
By the anodic oxidation aluminium substrate in the step 1.1 of embodiment 1, it is changed to silicon chip, other conditions are consistent.
Embodiment 6
By the graphene film in the step 1.1 of embodiment 1, it is changed to the PMMA polymer film that spin coating obtains, other conditions are protected
It holds consistent.
Embodiment 7
By the graphene film in the step 1.1 of embodiment 1, it is changed to graphene that spin coating obtains and ionic liquid is proportional
The liquid film of even mixing, other conditions are consistent.
Embodiment 8
Diamond tip in the step 3 of embodiment 1 is changed to the tips Si, substrate is changed to the graphene of AAO and Cu loads,
Other conditions are consistent.
The present invention relates to a kind of technologies for realizing the special tribological properties of graphene film based on AAO templates, in this work
In work, we specify the AAO templates of the nano-pore structure of structure to support graphene, to pass through AFM using having clear boundary
The control of micro-friction is received in the basic process of nano-scale grade friction and realization.
Claims (6)
1. a kind of method regulating and controlling graphene surface friction coefficient by surface limited effect, it is characterised in that：Including following step
Suddenly：
Step 1：Graphene shifts
Step 1.1：Copper platinum of the surface with PMMA/ graphene films is etched with iron nitrate solution, until PMMA/ graphene films float
To solution surface；
Step 1.2：PMMA/ graphene films are picked up to be put into distilled water and are cleaned；
Step 1.3：One piece of anodic alumina film is pressed from both sides with tweezers, is picked up upwards below PMMA/ graphene films；
Step 1.4：Anodic alumina support PMMA/ graphene films obtained above are statically placed in air drying；
Step 1.5：By the above-mentioned dry anodic alumina support PMMA/ graphene films heating terminated, make graphene film thereon
It flattens；
Step 1.6：Acetone bath is carried out to above-mentioned anodic alumina support PMMA/ graphene films, obtains anodic alumina support stone
Black alkene film；
Step 2：Tribology tester
Step 2.1：Using Dimension Icon AFM instruments, SNL-10 (tip radius 2nm) atomic force needle point is selected to connect
Friction measurement is carried out under touch formula；
Step 2.2：The normal spring constant at needle point tip is calibrated using the deflection sensitivity of supporting cantilever；
Step 2.3：The average transverse power that output voltage provides is converted to the frictional force generated due to the torsion of cantilever, and more
A sample position takes multiple measurements acquisition average value；
Step 2.4：Measure instantaneous desorption force curve；
Step 3：Molecular simulation
Step 3.1：Molecular dynamics mould is carried out using the nano-diamond tip slided on the graphene film that AAO is supported
It is quasi-, obtain the change curve of frictional force and normal load；
Step 3.2：It is mutual between graphene layer and AAO substrates when being scanned on the graphene surface that AAO is supported to calculate tip
Act on energy.
2. the method according to claim 1 for regulating and controlling graphene surface friction coefficient by surface limited effect, feature
It is：Iron nitrate concentration is 0.27g/mL in iron nitrate solution described in step 1.1.
3. the method according to claim 1 for regulating and controlling graphene surface friction coefficient by surface limited effect, feature
It is：PMMA/ graphene films are put into distilled water described in step 1.2 and are cleaned 3 times, each scavenging period is 10min.
4. the method according to claim 1 for regulating and controlling graphene surface friction coefficient by surface limited effect, feature
It is：Step 1.4 drying time is 30min.
5. the method according to claim 1 for regulating and controlling graphene surface friction coefficient by surface limited effect, feature
It is：Step 1.5 heating temperature is 80 DEG C, heating time 30min.
6. the method according to claim 1 for regulating and controlling graphene surface friction coefficient by surface limited effect, feature
It is：It is repeatedly 5 times that step 2.4, which measures,.
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| CN112128275A (en) * | 2020-09-12 | 2020-12-25 | 东北石油大学 | Frictional resistance increasing method based on interface mechanical effect |
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