CN109030870A - Two-dimensional layer material wraps up atomic force microscope probe and preparation method thereof and application - Google Patents
Two-dimensional layer material wraps up atomic force microscope probe and preparation method thereof and application Download PDFInfo
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- CN109030870A CN109030870A CN201810797392.7A CN201810797392A CN109030870A CN 109030870 A CN109030870 A CN 109030870A CN 201810797392 A CN201810797392 A CN 201810797392A CN 109030870 A CN109030870 A CN 109030870A
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- dimensional layer
- needle point
- atomic force
- force microscope
- microscope probe
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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
Abstract
The present invention provides a kind of two-dimensional layer material package atomic force microscope probe, including cantilever；From the cantilever surfaces pyramidal needle point outstanding；And it is wrapped in the top surface of the pyramidal needle point and the two-dimensional layer sheet of material of at least partly side.The present invention also provides a kind of preparation method and application of two-dimensional layer material package atomic force microscope probe.
Description
Technical field
The present invention relates to probes of a kind of atomic force microscope and preparation method thereof and application more particularly to one kind to be used for
Homogeneity or the probe of atomic force microscope of heterogeneous interlayer frictional behavior research and preparation method thereof and application.
Background technique
The interfacial friction measurement system of building micro-nano-scale is of great significance.On the one hand, friction is in our daily
It is seen everywhere in life, the friction between the component of machine of relative motion occurs and consumes a large amount of energy.Therefore, in currently
State's energy notch is increasing, in the case that effect of the equipment manufacture in national economy is increasingly stronger, improves machine components
Between Frotteurism and coefficient of friction be effectively reduced just seem and be even more important.On the other hand, in the past few decades, perhaps
More scholars are dedicated to reducing the adverse effect (including reducing energy dissipation) of friction until realizing the superslide state that frictional force is zero.
Academia achieves breakthrough in terms of superslide, it was found that fluid lubricant and solid lubricant with superslide characteristic.
Fluid lubricant is vulnerable under the harsh environments such as low temperature, extreme pressure.And solid lubrication can then break through the film lubrication limit, display
Great advantage out.For micro electronmechanical (MEMS) system of super hot investment casting, due to the reduction of size, the secondary gap that rubs is usual
In nanoscale, nanostructure solid lubricating film is widely used in the anti-attrition drop mill of MEMS system.
And in solid superslide field, the interfacial friction measurement system of micro-nano-scale is constructed, especially the contact of realization monocrystalline
Homogeneity or heterogeneous interlayer rub measurement under state are current more scabrous problems.To the main base of the exploration of Nanotribology
In atomic force microscope (AFM), the measurement of nano-grade size and Na Niu grades of micro- power not only may be implemented, but also can obtain simultaneously
To information such as three-dimensional appearances, the measurement for the process of being directed to is realized.For the interfacial friction measurement system for constructing micro-nano-scale, there is research
Graphene growth will be grown in metallic substrates on afm tip, or using wet process transfer using chemical vapour deposition technique by person
On graphene be transferred on needle point, and or prepare the needle point for being enclosed with graphene of special substance using the method for photoengraving.
However these methods are complicated, the usual defect of obtained graphene is more, and is difficult to obtain the package of the material in addition to graphene
Needle point.In addition also there is researcher using the direct adsorbent material small pieces of afm tip, this method has certain contingency, and material
Material is insecure in conjunction with needle point, is easy to happen and falls off.
Summary of the invention
Based on this, it is necessory to provide a kind of two-dimensional layer material package atomic force microscope probe and preparation method thereof with
And application
A kind of two-dimensional layer material package atomic force microscope probe, comprising:
Cantilever；
From the cantilever surfaces pyramidal needle point outstanding；And
It is wrapped in the top surface of the pyramidal needle point and the two-dimensional layer sheet of material of at least partly side.
In one embodiment, the two-dimensional layer sheet of material is mono-crystalline structures.
In one embodiment, the two-dimensional layer sheet of material is selected from graphite flake layer, boron nitride lamella, molybdenum disulfide
At least one of lamella, tantalum disulfide lamella and rhenium disulfide lamella.
In one embodiment, the two-dimensional layer sheet of material with a thickness of 10 nanometers to 70 nanometers, the two dimension
The size of stratified material lamella is 1 μm to 10 μm of 10 μ m of 1 μ m.
In one embodiment, the length of the top surface of the pyramidal needle point or diameter are received for 100 nanometers to 300
Rice.
In one embodiment, the top surface of the pyramidal needle point is the plane of disruption, etched surface or rubbing surface.
In one embodiment, the top surface of the pyramidal needle point is the surface of fresh exposure.
In one embodiment, the plane of disruption, etched surface or the rubbing surface of the pyramidal needle point are fresh formation
Surface.
In one embodiment, the material of the pyramidal needle point is monocrystalline silicon.
In one embodiment, the two-dimensional layer sheet of material and the pyramidal needle point pass through Van der Waals force knot
It closes.
A kind of application of the two-dimensional layer material package atomic force microscope probe, for obtaining and the two-dimensional layer
The interfacial friction specificity analysis of shape sheet of material homogeneous material or dissimilar materials.
In one embodiment, for obtaining and the two-dimensional layer sheet of material homogeneous material or dissimilar materials monocrystalline
Interfacial friction specificity analysis under contact condition.
In one embodiment, including by the two-dimensional layer material atomic force microscope probe and the homogeneity are wrapped up
It is aobvious to obtain the two-dimensional layer material package atomic force to friction system for material or dissimilar materials relative friction, building monocrystalline
Micro mirror probe is in the frictional force under different loads between the homogeneous material or dissimilar materials, by the frictional force with load
The slope of change curve obtains the coefficient of friction.
In one embodiment, including the two-dimensional layer material package atomic force microscope probe is used to obtain monocrystalline
The relationship of the relative rotation of frictional force and friction pair between graphite flake layer and mono-crystal nitride boron, the single crystal graphite lamella and institute
The frictional force between mono-crystal nitride boron heterojunction structure is stated not change with the secondary relative rotation of friction and change.
In one embodiment, including the two-dimensional layer material package atomic force microscope probe is used to obtain two sulphur
Change atomic resolution interlayer lateral force image between rhenium lamella and homogeneous material.
A kind of preparation method of two-dimensional layer material package atomic force microscope probe, comprising:
The stratified material that surface is cleavage surface is provided, the part of the cleavage surface has two-dimensional layer sheet of material, makes institute
Cleavage surface is stated in step-like；
It provides from cantilever surfaces pyramidal needle point outstanding, the area of the two-dimensional layer sheet of material is greater than the frustum
The top surface of shape needle point；
It contacts the top surface of the pyramidal needle point with the two-dimensional layer sheet of material being heated, and passes through institute
It states pyramidal needle point and load is applied to the two-dimensional layer sheet of material；And
Make under conditions of applying the load the pyramidal needle point two-dimensional layer sheet of material surface back and forth
Reciprocating friction, to make the two-dimensional layer sheet of material remove from layered material under heat auxiliary, and described in package
Pyramidal needle point.
In one embodiment, the step of offer pyramidal needle point outstanding from cantilever surfaces includes:
It provides from cantilever surfaces cone cell needle point outstanding；And
The tip of the cone cell needle point is removed to obtain the pyramidal needle point that the top surface is fresh surface.It is described
Fresh surface has dangling bonds.
In one embodiment, the step of tip of the removal cone cell needle point includes:
Hard substrate is provided, the hard substrate has first surface, in the hard substrate far from the first surface
Side be provided with expandable material；
By first surface described in the cone cell needle point face and it is spaced a predetermined distance setting；
Make the expandable material expanded by heating under hot subsidiary conditions, to make the hard substrate and the cone cell needle
Point bumps against, and is broken the tip of the cone cell needle point, to obtain the pyramidal needle point that the top surface is the fresh plane of disruption.
In one embodiment, the hard substrate is layered material, and the first surface is the cleavage surface.
In one embodiment, the preset distance is several microns to more than ten microns.
In one embodiment, the heating temperature is 150 DEG C to 200 DEG C.
In one embodiment, the step of tip of the removal cone cell needle point includes:
Etching removes the tip of the cone cell needle point, obtains the pyramidal needle point that the top surface is fresh etched surface；
Or
Mechanical friction removes the tip of the cone cell needle point, obtains the pyramidal needle that the top surface is fresh rubbing surface
Point.
In one embodiment, the size for applying load is 500nN to 800nN.
In one embodiment, the amplitude of described time reciprocating friction corresponds to the ruler of the two-dimensional layer sheet of material
It is very little.
In one embodiment, the top surface of the pyramidal needle point has dangling bonds.
In one embodiment, the material of the pyramidal needle point is monocrystalline silicon, and the top surface is monocrystalline silicon surface.
Two-dimensional layer material package atomic force microscope probe provided by the invention and preparation method thereof utilizes pyramidal needle
The top surface of point provides and the biggish contact area of two-dimensional layer sheet of material, the surface of fresh formation is preferably provided, with two dimension
The contact of stratified material lamella, and the reciprocating friction back and forth while applying load makes the two dimension under conditions of heating auxiliary
Stratified material lamella is removed from layered material, and is stablized and firmly wrapped up the pyramidal needle point.The probe
Preparation method is simple and convenient, and assists mechanical stripping transfer process for a kind of heat, and two-dimensional layer sheet of material can preselect,
Defect will not be introduced during the preparation process, and the probe made is highly suitable for tribological field, is especially used for homogeneity or different
The research of matter interfacial friction characteristic.
Detailed description of the invention
Fig. 1 is that the two-dimensional layer material of the embodiment of the present invention wraps up the structural schematic diagram of atomic force microscope probe；
Fig. 2 is the process that the two-dimensional layer material of the embodiment of the present invention wraps up the preparation method of atomic force microscope probe
Figure；
Fig. 3 is the structural schematic diagram of the stratified material of the embodiment of the present invention；
Fig. 4 A to Fig. 4 C is that the two-dimensional layer material of one embodiment of the invention wraps up the preparation side of atomic force microscope probe
The process schematic of method；
Fig. 5 is the stereochemical structure signal of the pyramidal needle point for being enclosed with two-dimensional layer sheet of material of the embodiment of the present invention
Figure；
Fig. 6 is the plan structure signal of the pyramidal needle point for being enclosed with two-dimensional layer sheet of material of the embodiment of the present invention
Figure；
Fig. 7 and Fig. 8 is the stereoscan photograph that the cone cell needle point of one embodiment of the invention severs front and back；
Fig. 9 is the stereoscan photograph of the pyramidal needle point for being enclosed with graphite flake layer of one embodiment of the invention；
Figure 10 is the transmission electron microscope photo of the pyramidal needle point for being enclosed with graphite flake layer of one embodiment of the invention；
Figure 11 is that the high resolution TEM of the pyramidal needle point for being enclosed with graphite flake layer of one embodiment of the invention shines
Piece；
Figure 12 is the Raman spectrum test chart of the pyramidal needle point for being enclosed with graphite flake layer of one embodiment of the invention；
Figure 13 is the transmission electron microscope photo of the pyramidal needle point for being enclosed with boron nitride lamella of one embodiment of the invention；
Figure 14 is the transmission electron microscope photo of the pyramidal needle point for being enclosed with rhenium disulfide lamella of one embodiment of the invention；
Figure 15 is the transmission electron microscope photo of the pyramidal needle point for being enclosed with molybdenum disulfide lamella of one embodiment of the invention；
Figure 16 is the pyramidal needle point for being enclosed with graphite flake layer and the friction of hexagonal boron nitride interlayer of one embodiment of the invention
Coefficient test data figure.
Figure 17 is the frustum for being enclosed with hexagonal boron obtained by atomic force microscope of one embodiment of the invention
Shape needle point and hexagonal boron nitride atomic resolution interlayer lateral force image.
Figure 18 is the pyramidal needle point for being enclosed with graphite flake layer and the friction of hexagonal boron nitride interlayer of one embodiment of the invention
Power with the secondary relative rotation that rubs test data figure.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, right with reference to the accompanying drawings and embodiments
The present invention is further elaborated.It should be appreciated that described herein, specific examples are only used to explain the present invention, not
For limiting the present invention.
" stratified material " mentioned in the present invention refers to the material with layered crystal structure, and macroscopical shape of non-limiting material
Shape.Preferably, the atom interlayer of layered material is connected by Van der Waals force, is easy to dissociate or remove.Stratified material can be with
Enumerate but be not limited to graphite, boron nitride, molybdenum disulfide, tantalum disulfide and rhenium disulfide.
Referring to Fig. 1, the embodiment of the present invention provides a kind of two-dimensional layer material package atomic force microscope probe, including outstanding
Arm 10 from 10 surface of cantilever pyramidal needle point 20 outstanding, and is wrapped in 22 He of top surface of the pyramidal needle point 20
At least partly two-dimensional layer sheet of material 30 of side 24.
The shape of the pyramidal needle point 20 can be the frustum of a cone or the frustum of a pyramid, the preferably frustum of a cone.The pyramidal needle
The bottom surface of point 20 is oppositely arranged with the top surface 22, and the bottom surface is arranged on 10 surface of cantilever, is preferably arranged on described
One end of the side of cantilever 10.The top surface 22 with surface to be scanned for being oppositely arranged.The shape of the top surface 22 can be with
For round, ellipse or polygon.
The two-dimensional layer sheet of material 30 is directly wrapped in the top surface 22 and side 24.Preferably, described pyramidal
There is stronger molecular separating force, such as Van der Waals force between the top surface 22 of needle point 20 and the two-dimensional layer sheet of material 30, make
Obtaining the two can stablize and firmly combine.The top surface 22 of the pyramidal needle point 20 preferably has dangling bonds, to make described
Van der Waals force between top surface 22 and the two-dimensional layer sheet of material 30 is stronger.It is total in an embodiment, the pyramidal needle point
20 material is monocrystalline silicon, and the top surface 22 is fresh monocrystalline silicon surface, and the dangling bonds are the dangling bonds of silicon.The frustum
The top surface 22 of shape needle point 20 preferably has large surface area, to make to have between the top surface 22 and the two-dimensional material lamella 30
There is biggish bonded area, so that the two is in conjunction with more stable.In one embodiment, the length of the top surface 22 or diameter are preferred
It is 100 nanometers to 300 nanometers.The length of the top surface 22 refers to pass through when the top surface 22 is non-circular
Longest distance.Preferably, the top surface 22 has biggish adhesion strength for being combined with the two-dimensional layer sheet of material 30.For
Make the top surface 22 with fresh surface and there are dangling bonds, the top surface 22 can be for by by traditional cone cell needle point top
Fracture the fresh plane of disruption to be formed, or by etching the fresh etched surface formed behind removal top, Huo Zhetong to cone cell needle point
Cross the fresh rubbing surface that will be formed behind cone cell needle point friction removal top.These methods can remove the oxide of material surface
Film makes material surface form a large amount of dangling bonds, these dangling bonds can react in air with oxygen, it is therefore preferred that in shape
The two-dimensional layer sheet of material 30 should be wrapped up on pyramidal 20 top of needle point as early as possible at after dangling bonds.
The two-dimensional layer sheet of material 30 comes from stratified material, is one layer removed from the cleavage surface of layered material
Or the atomic layer being repeatedly overlapped.Preferably, the two-dimensional layer sheet of material 30 has mono-crystalline structures, makes the two-dimensional layer material
Material package atomic force microscope probe can be used in constructing homogeneity/heterojunction structure interlayer rub measurement body under monocrystalline contact condition
System.The two-dimensional layer sheet of material 30 is selected from but not limited to graphite flake layer, boron nitride lamella, molybdenum disulfide lamella, curing
At least one of tantalum piece layer and rhenium disulfide lamella.The area of the two-dimensional layer sheet of material 30 and the pyramidal needle point
20 tip size matching, can wrap up the top surface 22 and at least partly side 24 of the pyramidal needle point 20.The two-dimensional layer
The thickness of shape sheet of material 30 is preferably 10 nanometers to 70 nanometers；It is preferably sized to 1 μm of 1 μ m to 10 μm of 10 μ m, more preferably
It is 5 μm to 10 μm of 10 μ m of 5 μ m.
Please refer to figs. 2 and 3, and the embodiment of the present invention also provides a kind of two-dimensional layer material package atomic force microscope probe
Preparation method, comprising:
S1, provides the stratified material 32 that surface is cleavage surface 34, and the part of the cleavage surface 34 has two-dimensional layer material
Lamella 30 makes the cleavage surface 34 in step-like；
S2 is provided from 10 surface of cantilever pyramidal needle point 20 outstanding, and the area of the two-dimensional layer sheet of material 30 is big
In the top surface 22 of the pyramidal needle point 20；
S3 connects the top surface 22 of the pyramidal needle point 20 with the two-dimensional layer sheet of material 30 being heated
Touching, and load is applied to the two-dimensional layer sheet of material 30 by the pyramidal needle point 20；And
S4 makes the pyramidal needle point 20 in 30 table of two-dimensional layer sheet of material under conditions of applying the load
Face reciprocating friction back and forth, so that the two-dimensional layer sheet of material 30 be made to shell from layered material 32 under hot subsidiary conditions
From, and wrap up the pyramidal needle point 20.
Layered material 32 can be set on 40 surface of support substrate.In one embodiment, the support substrate 40 is
Silica substrate.The atom interlayer of layered material 32 is connected by Van der Waals force, is easy to dissociate or remove.It is layered
At least one of graphite, boron nitride, molybdenum disulfide, tantalum disulfide and rhenium disulfide can be enumerated but be not limited to material 32.Institute
The method that stating cleavage surface 34 can for example be by mechanically pulling off is formed.In one embodiment, it can be adhered to adhesive tape layered
The surface of material 32 while throwing off adhesive tape stratified material lamella can be removed from layered material 32, to be formed
The cleavage surface 34.Preferably, the cleavage surface 34 is the cleavage surface of fresh formation, to avoid the cleavage surface 34 by other objects
Matter pollution.Due to the lattice defect of stratified material itself, atomic layer will not be complete during formation for the cleavage surface 34
It is stripped, but the cleavage surface 34 can be made to form platform in some two-dimensional layer sheet of material 30 of Local residues of cleavage surface 34
Stepped structure.These two-dimensional layer sheet of material 30 are distributed in the regional area of the cleavage surface 34 in island, with stratified material
The connection stable still through Van der Waals force of 32 ontology.
In order to realize complete and stable package, it is suitable to need to find area in the cleavage surface 34 before carrying out step S3
Two-dimensional layer sheet of material 30.The area of the two-dimensional layer sheet of material 30 is greater than the top surface of the pyramidal needle point 20
22, but cannot be too big.The excessive two-dimensional layer sheet of material 30 of area be difficult to by with pyramidal 20 reciprocating friction of needle point
Mode be stripped and wrap up the pyramidal needle point 20.The two-dimensional layer sheet of material 30 is preferably sized to 1 μm of 1 μ m
To 10 μm of 10 μ m, more preferably size is 5 μm to 10 μm of 10 μ m of 5 μ m.The thickness of the two-dimensional layer sheet of material 30
For nanoscale, preferably 10 nanometers to 70 nanometers, that is to say, that the step height of the step-like cleavage surface 34 is nanoscale,
Preferably 10 nanometers to 70 nanometers.It, can be by existing to find suitable two-dimensional layer sheet of material 30 in the cleavage surface 34
Atomic force microscope probe, or preferably the pyramidal needle point 20 is regard as atomic force microscope probe, described in scanning
The surface of cleavage surface 34.The image of 34 surface topography of cleavage surface is generated, in real time by atomic force microscope to confirm suitable two
Tie up the position of stratified material lamella 30.In addition, 34 surface of cleavage surface is scanned and can be selected by atomic force microscope probe
Regular appearance and flawless two-dimensional layer sheet of material 30 are selected, experiment shows subsequent mechanical stripping and package step to two dimension
The quality of stratified material lamella 30 can readily avoid the two-dimensional layer in finally obtained detecting probe surface almost without influence
There are more defects in shape sheet of material 30.
In one embodiment, the step S3 and S4 can be by regarding the pyramidal needle point 20 as atomic force microscope
Probe, and the probe is controlled in oriented 30 surface scan of the two-dimensional layer sheet of material reality by atomic force microscope
It is existing.Preferably, during step S3 and S4, layered material is in and is heated state, is conducive to promote the two dimension
Stratified material lamella 30 is easier to be removed by the pyramidal needle point 20 and wraps up the pyramidal needle point 20.The heating temperature
Preferably 150 DEG C to 200 DEG C of degree.
In step S3 and S4, the cantilever 10 is substantially parallel with 34 surface of cleavage surface, and perpendicular to it is described back and forth
The moving direction of reciprocating friction passes through the friction between the top surface 22 and the two-dimensional layer sheet of material 30 of pyramidal needle point 20
Power makes the two-dimensional layer sheet of material 30 remove and crimp from the ontology of layered material 32, to be wrapped in described
The almost synchronous generation of the top surface 22 of pyramidal needle point 20 and at least partly side 24, the removing and the process of package.The cone
The top surface 22 of mesa-shaped needle point 20 is pressed in the two-dimensional layer sheet of material 30, and by applying the load, progress is past back and forth simultaneously
Multiple friction, can increase the frictional force, the load is preferably 500nN to 800nN, more preferably 500nN.It is described pyramidal
The reciprocating friction back and forth between the opposite both ends of the two-dimensional layer sheet of material 30 of needle point 20.The pyramidal needle point 20 is opposite
In the frequency of the two-dimensional layer sheet of material 30 reciprocating friction back and forth be preferably 5Hz to 10Hz, the reciprocating friction back and forth
The equal length of amplitude and the two-dimensional layer sheet of material 30.In one embodiment, the two-dimensional layer sheet of material 30
Length is 8 microns, and the amplitude of the reciprocating friction back and forth is 8 microns.
Preferably, the step S2 further comprises the step of preparing pyramidal needle point 20.It is appreciated that in order to make
The two-dimensional layer sheet of material 30 can be removed smoothly from layered material 32, and the top with pyramidal needle point 20
Face 22 forms stable and firm combination, and the top surface 22 of the pyramidal needle point 20 is preferably fresh surface, has more suspension
Key.In one embodiment, the preparation step of the pyramidal needle point 20 includes:
S21 is provided from 10 surface of the cantilever cone cell needle point outstanding；And
S22 removes the tip of the cone cell needle point to obtain the pyramidal needle point 20.
The diameter at the tip of the cone cell needle point is, for example, 10 nanometers to 20 nanometers.The removal is preferably through Mechanical Method
Or chemical method removal, the tip by removing cone cell needle point form the top surface 22, the material inside cone cell needle point can be made sudden and violent
Expose, makes the fresh surface in the top surface 22, to form a large amount of dangling bonds.These dangling bonds in air can be anti-with oxygen
Answer, therefore the step of preparing pyramidal needle point 20 preferably carries out before step S3 immediately, more preferably in the step S3 and
It is carried out in the same chamber of S4, top surface 22 is avoided to react to form oxidation film with oxygen.
In a preferred embodiment, the material of the cone cell needle point 26 is silicon, the surface of silicon needle point silica easy to form
Film forms the pyramidal needle point 20 by way of removing tip 28, and silicon can be made to be exposed to the top surface 22, is formed big
Measure the dangling bonds of silicon.
Fig. 4 A to Fig. 4 C and Fig. 5 and Fig. 6 are please referred to, in one embodiment, the step S22 includes:
S221 provides hard substrate, and the hard substrate has first surface, in the hard substrate far from described first
The side on surface is provided with expandable material 50, it is preferred that the hard substrate is same substrate, institute with layered material 32
Stating first surface is the cleavage surface 34；
S222 by first surface 34 described in 26 face of cone cell needle point and is spaced a predetermined distance setting；And
S223 makes 50 expanded by heating of expandable material by heating, to make the hard substrate and the cone cell
Needle point 26 bumps against, and is broken the tip 28 of the cone cell needle point 26, is the fresh plane of disruption and has to obtain the top surface 22
The pyramidal needle point 20 of the dangling bonds.
It is appreciated that the hard substrate and layered material 32 or different base, as long as can have one
Determine intensity, is broken the tip 28 of the cone cell needle point 26 by hitting.It is preferred that directly being made using layered material 32
Hit the cone cell needle point 26 for the hard substrate, more preferably using the two-dimensional layer sheet of material 30 as with the cone
The region that the tip 28 of shape needle point 26 directly contacts, so that the cone formed can be utilized at once after severing the cone cell needle point 26
The top surface 22 of mesa-shaped needle point 20 rubs to the two-dimensional layer sheet of material 30, i.e., carry out subsequent step S3 in situ and
S4 to avoid dangling bonds from reacting with oxygen to greatest extent, or introduces other pollutants, in addition it can simplify operation step
Suddenly, easy to accomplish.
In the step S222, the preset distance is preferably several microns to more than ten microns.The distance at the interval with
Volume change after 50 expanded by heating of expandable material is related, as long as by institute after capable of making 50 expanded by heating of expandable material
Hard substrate is stated, such as layered material 32 pushes up the tip 28 to the cone cell needle point 26 and severs the tip 28.
The expandable material 50 can be set on another surface of hard substrate, be preferably provided at the support substrate 40
Another surface.The expandable material 50 can generate volume expansion by heating, and expansion is more rapid, to generate
Certain impact force, makes the hard substrate, such as layered material 32 is sufficiently large to the impact force of the cone cell needle point 26.
In one embodiment, the elargol that it is 150 DEG C to 200 DEG C for expansion point temperature that the expandable material 50, which for example can choose,.
When the hard substrate is layered material 32, heat expandable material 50 whiles, can make layered
Material 32 is heated together, and heating process had not only made stratified material 32 and the collision of cone cell needle point 26 form pyramidal needle point 20, but also
So that the pollutant or hydrone etc. in stratified material 32 are removed, clean stratified material 32 more, become prone to remove, benefit
In the progress of subsequent step S3 and S4, operating procedure is further simplified.The heating temperature of the step S223 is preferably 150 DEG C
To 200 DEG C.
Fig. 7 and Fig. 8 are please referred to, in one embodiment, the cone cell needle point 26 is silicon needle point, and tip diameter is 16 nanometers,
The diameter that the top surface 22 of pyramidal needle point 20 is formed after severing is about 150 nanometers.In one embodiment, layered material 32 is
Graphite, the two-dimensional layer sheet of material 30 are the graphite flake layer of nanometer grade thickness.By the step S3 and S4 by graphite flake
Layer is wrapped on the pyramidal silicon needle point severed, please refers to Fig. 9 and Figure 10, it can be seen that graphite flake layer is substantially smooth and complete
Wrap up the top surface 22 and at least partly side of the pyramidal silicon needle point.Figure 11 and Figure 12 are please referred to, to the partial zones of top surface 22
Domain carries out high resolution TEM and Raman spectrum test, and Figure 12 is the graphite flake layer Raman spectrum test being wrapped on needle point
Graphite flake layer Raman spectrum test data in data and hard substrate.Raman spectrum can reveal that graphite sp2In the face of atom
Vibration, the information such as the stack manner of carbon atom and fault of construction.The typical Raman peaks of graphite are located at 1580cm-1Neighbouring
The peak G and 2700cm-1The neighbouring peak 2D.The peak G results from sp2The in plane vibration of atom, and the peak 2D is then derived from second order double resonance drawing
Graceful scattering process.Usually using the ratio at the peak G and the peak 2D as the foundation for judging the graphite number of plies in Raman spectrum,
Wherein ratio 2D peak intensity in the peak G is big, then is graphite, otherwise is graphene.In addition the defects of graphite can be reflected in 1350cm-1Near
The peak D on, and the test result of the embodiment of the present invention does not find the presence at the peak D, and the graphite flake layer for showing to wrap up on needle point is several
There is no defect.
In another embodiment, layered material 32 is hexagonal boron nitride, and the two-dimensional layer sheet of material 30 is to receive
The boron nitride lamella of meter level thickness.Please refer to Figure 13, it can be seen that the method for the embodiment of the present invention is same to hexagonal boron nitride
Sample is applicable in, and forms the pyramidal silicon needle point of complete package hexagonal boron nitride lamella.
In another embodiment, layered material 32 is rhenium disulfide, and the two-dimensional layer sheet of material 30 is nanometer
The rhenium disulfide lamella of grade thickness.Please refer to Figure 14, it can be seen that the method for the embodiment of the present invention is same to rhenium disulfide
It is applicable in, forms the pyramidal silicon needle point of complete package rhenium disulfide lamella.
In another embodiment, layered material 32 is molybdenum disulfide, and the two-dimensional layer sheet of material 30 is nanometer
The molybdenum disulfide lamella of grade thickness.Please refer to Figure 15, it can be seen that the method for the embodiment of the present invention is same to molybdenum disulfide
It is applicable in, forms the pyramidal silicon needle point of complete package molybdenum disulfide lamella.
It is formed it is appreciated that the pyramidal needle point 20 is not limited by the above-mentioned mode severed.In another embodiment,
Can be by the tip 28 of cone cell needle point 26 described in mechanical friction, to remove the tip 28, it is new for obtaining the top surface 22
Fresh rubbing surface and the pyramidal needle point 20 with the dangling bonds.In another embodiment, it can be removed by chemical method
The tip 28, such as the tip 28 of the cone cell needle point 26 is removed by chemical etching, obtaining the top surface 22 is fresh quarter
Erosion face and the pyramidal needle point 20 with the dangling bonds.
Two-dimensional layer material package atomic force microscope probe provided by the invention and preparation method thereof utilizes pyramidal needle
The top surface of point is provided to be made with the biggish contact area of two-dimensional layer sheet of material, the reciprocating friction back and forth while applying load
The two-dimensional layer sheet of material is removed from layered material, and is stablized and firmly wrapped up the pyramidal needle point.Institute
The preparation method for stating probe is simple and convenient, and assists mechanical stripping transfer process for a kind of heat, and two-dimensional layer sheet of material can be with
It is Yu Xianxuanding, and it is not limited to graphite material, and the material of the layered crystal structure connected to interlayer by Van der Waals force can be expanded
Expect, will not introduce defect in preparation process, the probe made is highly suitable for tribological field, is especially used for homogeneity or different
The research of matter interfacial friction characteristic can carry out atom level interlayer Analysis of Side Force.
The embodiment of the present invention also provides the application side of the package atomic force microscope probe of two-dimensional layer material described in one kind
Method is obtained using the atomic force microscope probe and is rubbed with 30 homogeneous material of two-dimensional layer sheet of material or dissimilar materials
Wipe the interfacial friction characteristic under characteristic, especially monocrystalline contact condition.The frictional behavior includes but unlimited and coefficient of friction, former
Relationship between sub- grade interlayer lateral force and atom level interlayer lateral force and crystal lattice orientation.
In one embodiment, coefficient of friction can be obtained by following steps, comprising:
By two-dimensional layer material package, atomic force microscope probe is opposite with the homogeneous material or dissimilar materials rubs
It wipes；
Obtain two-dimensional layer material package atomic force microscope probe under different loads with the homogeneous material or
Frictional force between dissimilar materials；And
The coefficient of friction is obtained with load change slope of a curve by the frictional force.
Specifically, in the probe for being applied with the first load and the homogeneity or the process of dissimilar materials relative friction
In, first group of voltage signal of probe lateral twisting can be obtained by atomic force microscope, and pass through first group of voltage signal
Obtain the first interfacial friction.Then change magnitude of load, obtain the corresponding second group of voltage signal of the second load, and pass through the
Two groups of voltage signals obtain the second interfacial friction.And so on, it is corresponding with differentiated friction power to obtain a series of different loads
Relationship, to establish the frictional force with load change curve, the slope of a curve be the two-dimensional layer sheet of material with
Coefficient of friction between the homogeneous material or dissimilar materials.
The homogeneous material refers to material identical with the two-dimensional layer sheet of material, such as when the two-dimensional layer material
When lamella 30 is graphite flake layer, homogeneous material is graphite or graphene.The dissimilar materials refers to and the two-dimensional layer material piece
The different material of layer, such as when the two-dimensional layer sheet of material 30 is graphite flake layer, dissimilar materials can be boron nitride piece
At least one of layer, molybdenum disulfide lamella, tantalum disulfide lamella and rhenium disulfide lamella.Preferably, the two-dimensional layer material
Tablet layer 30 and the homogeneous material or dissimilar materials are monocrystal material, to construct monocrystalline to friction system.
Figure 16 is please referred to, in one embodiment, the two-dimensional layer sheet of material 30 is single crystal graphite lamella, uses atom
Force microscope carries out the needle point for being enclosed with single crystal graphite lamella and hexagonal boron nitride to the test that rubs, and load is gradually increased from 0nN
To 400nN, frictional force between the two is in superslide state, warp close to 0nN under different loads as can see from Figure 16
The needle point and hexagonal boron nitride interlayer coefficient of friction for calculating parcel form crystalline substance graphite flake layer also turn out described two down to 0.0001
Dimension stratified material lamella 30 firm stable is wrapped in the needle surface, is mono-crystalline structures and almost zero defect.And through reality
It issues after examination and approval now, superslide still may be implemented when ambient humidity is 60% in the probe of the embodiment of the present invention, has extremely strong resistance to
Polishing machine.
In another embodiment, it is secondary to friction former that the two-dimensional layer material package atomic force microscope probe can be used
Sub- grade lateral force is tested, including by the two-dimensional layer material package atomic force microscope probe and the homogeneous material or
Dissimilar materials relative friction；And atomic resolution interlayer lateral force image is obtained by atomic force microscope.
Figure 17 is please referred to, in one embodiment, the two-dimensional layer sheet of material 30 is rhenium disulfide lamella, will be enclosed with
The needle point of rhenium disulfide lamella and homogeneous material rhenium disulfide relative friction, obtain that rhenium disulfide lamella is opposite with homogeneous material to rub
The atomic resolution interlayer lateral force image of wiping, first observed to rhenium disulfide interfacial friction extreme value is in hexagon distribution
Image.
In another embodiment, it is secondary to friction former that the two-dimensional layer material package atomic force microscope probe can be used
Relationship between sub- grade lateral force and crystal lattice orientation is tested, including the two-dimensional layer material is wrapped up atomic force microscope
Probe and the homogeneous material or dissimilar materials are along different directions relative friction；And obtain the two-dimensional layer material package original
The frictional force on different directions between sub- force microscope probe and the homogeneous material or dissimilar materials.
Figure 18 is please referred to, in one embodiment, the two-dimensional layer sheet of material 30 is graphite flake layer, will be enclosed with graphite
The needle point of lamella and the hexagonal boron nitride relative friction, by the substrate where rotation hexagonal boron nitride, along multiple directions phase
To friction, experimentally find the frictional force between the graphite flake layer and the dissimilar materials boron nitride not as friction is secondary for the first time
Relative rotation variation and change.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
Limitations on the scope of the patent of the present invention therefore cannot 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, various modifications and improvements can be made, these belong to guarantor of the invention
Protect range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (21)
1. a kind of two-dimensional layer material wraps up atomic force microscope probe characterized by comprising
Cantilever；
From the cantilever surfaces pyramidal needle point outstanding；And
It is wrapped in the top surface of the pyramidal needle point and the two-dimensional layer sheet of material of at least partly side.
2. two-dimensional layer material according to claim 1 wraps up atomic force microscope probe, which is characterized in that the two dimension
Stratified material lamella is mono-crystalline structures.
3. two-dimensional layer material according to claim 1 wraps up atomic force microscope probe, which is characterized in that the two dimension
Stratified material lamella is in graphite flake layer, boron nitride lamella, molybdenum disulfide lamella, tantalum disulfide lamella and rhenium disulfide lamella
At least one.
4. two-dimensional layer material according to claim 1 wraps up atomic force microscope probe, which is characterized in that the frustum
The top surface of shape needle point is the plane of disruption, etched surface or rubbing surface.
5. two-dimensional layer material according to claim 1 wraps up atomic force microscope probe, which is characterized in that the frustum
The material of shape needle point is monocrystalline silicon.
6. two-dimensional layer material according to claim 1 wraps up atomic force microscope probe, which is characterized in that the two dimension
Stratified material lamella and the pyramidal needle point by Van der Waals force in conjunction with.
7. a kind of two-dimensional layer material package atomic force microscope probe according to any one of claim 1 to 6 is answered
With, which is characterized in that for obtaining the interfacial friction characteristic with the two-dimensional layer sheet of material homogeneous material or dissimilar materials.
8. the application of two-dimensional layer material package atomic force microscope probe according to claim 7, which is characterized in that packet
It includes two-dimensional layer material package atomic force microscope probe and the homogeneous material or dissimilar materials relative friction, building
Monocrystalline to friction system, obtain the two-dimensional layer material package atomic force microscope probe under different loads with it is described same
Frictional force between material or dissimilar materials, obtaining the friction with load change slope of a curve by the frictional force is
Number.
9. the application of two-dimensional layer material package atomic force microscope probe according to claim 7, which is characterized in that packet
It includes and is obtained between single crystal graphite lamella and mono-crystal nitride boron using two-dimensional layer material package atomic force microscope probe
The relationship of the relative rotation of frictional force and friction pair, between the single crystal graphite lamella and the mono-crystal nitride boron heterojunction structure
Frictional force does not change with the secondary relative rotation of friction and is changed.
10. the application of two-dimensional layer material package atomic force microscope probe according to claim 7, which is characterized in that
It is former between rhenium disulfide lamella and homogeneous material including using the two-dimensional layer material package atomic force microscope probe to obtain
Sub- class resolution ratio interlayer lateral force image.
11. a kind of preparation method of two-dimensional layer material package atomic force microscope probe, comprising:
The stratified material that surface is cleavage surface is provided, the part of the cleavage surface has two-dimensional layer sheet of material, makes the solution
Reason face is in step-like；
It provides from cantilever surfaces pyramidal needle point outstanding, the area of the two-dimensional layer sheet of material is greater than the pyramidal needle
The top surface of point；
It contacts the top surface of the pyramidal needle point with the two-dimensional layer sheet of material being heated, and passes through the cone
Mesa-shaped needle point applies load to the two-dimensional layer sheet of material；And
Make the pyramidal needle point reciprocal back and forth on the two-dimensional layer sheet of material surface under conditions of applying the load
Friction so that the two-dimensional layer sheet of material be made to remove from layered material under heat auxiliary, and wraps up the frustum
Shape needle point.
12. the preparation method of two-dimensional layer material package atomic force microscope probe according to claim 11, feature
It is, the step of offer pyramidal needle point outstanding from cantilever surfaces includes:
It provides from cantilever surfaces cone cell needle point outstanding；And
The tip of the cone cell needle point is removed to obtain the pyramidal needle point that the top surface is fresh surface.
13. the preparation method of two-dimensional layer material package atomic force microscope probe according to claim 12, feature
It is, the step of tip of the removal cone cell needle point includes:
There is provided hard substrate, the hard substrate have first surface, the hard substrate far from the first surface one
Side is provided with expandable material；
By first surface described in the cone cell needle point face and it is spaced a predetermined distance setting；
Make the expandable material expanded by heating under hot subsidiary conditions, to make the hard substrate and the cone cell needle point phase
It hits, is broken the tip of the cone cell needle point, to obtain the pyramidal needle point that the top surface is the fresh plane of disruption.
14. the preparation method of two-dimensional layer material package atomic force microscope probe according to claim 13, feature
It is, the hard substrate is layered material, and the first surface is the cleavage surface.
15. the preparation method of two-dimensional layer material package atomic force microscope probe according to claim 13, feature
It is, the preset distance is several microns to more than ten microns.
16. the preparation method of two-dimensional layer material package atomic force microscope probe according to claim 13, feature
It is, the heating temperature is 150 DEG C to 200 DEG C.
17. the preparation method of two-dimensional layer material package atomic force microscope probe according to claim 12, feature
It is, the step of tip of the removal cone cell needle point includes:
Etching removes the tip of the cone cell needle point, obtains the pyramidal needle point that the top surface is fresh etched surface；Or
Mechanical friction removes the tip of the cone cell needle point, obtains the pyramidal needle point that the top surface is fresh rubbing surface.
18. the preparation method of two-dimensional layer material package atomic force microscope probe according to claim 11, feature
It is, the size for applying load is 500nN to 800nN.
19. the preparation method of two-dimensional layer material package atomic force microscope probe according to claim 11, feature
It is, the amplitude of described time reciprocating friction corresponds to the size of the two-dimensional layer sheet of material.
20. the preparation method of two-dimensional layer material package atomic force microscope probe according to claim 11, feature
It is, the top surface of the pyramidal needle point has dangling bonds.
21. the preparation method of two-dimensional layer material package atomic force microscope probe according to claim 11, feature
It is, the material of the pyramidal needle point is monocrystalline silicon, and the top surface is monocrystalline silicon surface.
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| PCT/CN2018/113075 WO2020015243A1 (en) | 2018-07-19 | 2018-10-31 | Atomic force microscope probe wrapped with two-dimensional layered structure, preparation method therefor, and application thereof |
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| CN110697779A (en) * | 2019-09-23 | 2020-01-17 | 清华大学 | Friction regulation and control method, device and system for molybdenum disulfide |
| WO2020015243A1 (en) * | 2018-07-19 | 2020-01-23 | 清华大学 | Atomic force microscope probe wrapped with two-dimensional layered structure, preparation method therefor, and application thereof |
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| CN113702279A (en) * | 2021-07-12 | 2021-11-26 | 清华大学 | Device and method for preparing graphite nanosheet probe and method for detecting graphite friction |
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| WO2020015243A1 (en) | 2020-01-23 |
| CN109030870B (en) | 2019-10-25 |
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