CN107328956A - A kind of atomic force microscope probe preparation method for wrapping up two-dimensional material - Google Patents
A kind of atomic force microscope probe preparation method for wrapping up two-dimensional material Download PDFInfo
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- CN107328956A CN107328956A CN201710413065.2A CN201710413065A CN107328956A CN 107328956 A CN107328956 A CN 107328956A CN 201710413065 A CN201710413065 A CN 201710413065A CN 107328956 A CN107328956 A CN 107328956A
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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
Embodiments of the invention provide a kind of atomic force microscope probe preparation method for wrapping up two-dimensional material, are related to modification and the processing technique field of atomic force microscope probe.Method provided in an embodiment of the present invention, can stablize in 500 DEG C of environment and stick on needle point in air or vacuum, the acquisition that AFM realizes various atomic force microscope images can be applied in air and vacuum；It can apply to study the surface property of two dimensional surface material, the especially adhesion between two-dimensional material, the mechanical mechanics property such as friction easily studies the special nature of large quantities of low-dimensional materials；And manufacturing process is ripe easy, it is adapted to laboratory and commercial application makes two-dimensional material modified tips probe.
Description
Technical field
The present invention relates to the modification of atomic force microscope probe and processing technique field, more particularly to a kind of two-dimentional material of parcel
The atomic force microscope probe preparation method of material.
Background technology
AFM is that the Gerd Binnig by IBM Corporation Zurich research center in 1985 are invented, and it can
The surface roughness of base material is detected with high-resolution, surface is electric, magnetic and mechanical performance, the surface property such as surface adhesion,
Have become multidisciplinary, including physics, chemistry, biology, material science, electricity, the microstructure observation of mechanics etc., micro-nano chi
Degree processing, micro-nano displacement and the application of micro- power etc..Atomic force microscope probe generally comprises main body, and micro-cantilever and micro needlepoint etc. are several
Part, micro-cantilever shape is divided into rectangle, and triangle etc. is several.The needle point of probe dominates the performance and kind of AFM
Class, common atomic force microscope probe is made by the manufacturing procedure of semi-conducting material, routinely with silicon, based on silicon nitride
Material is made, using metal deposit, and the metal cladding such as sputtering improves the conductive or new performance of increase；Recent decades, to atomic force
The modification and processing of microscope needle-tip have received increasing concern, and it is with the various various low-dimensionals including CNT
The property of material obtains various with new function, fabulous resolution ratio and excellent picture quality, or meets a certain
The particular/special requirement in field etc..
Two-dimensional material since graphenes in 2004 and receive and receive significant attention, mainly including graphene, boron nitride, two
Molybdenum sulfide etc., it has an excellent electricity to graphene, light, the property such as magnetic, and rather extensive to its research, graphene also has
There is high mechanical property, its elastic constant reaches 1TPa；Due to the great surface texture of two-dimensional material, graphene can be born
20% face internal strain is without causing structural damage；Boron nitride is the two-dimentional material with the crystal structure similar with graphene
Material, it has preferable insulating properties, and its surface atom level flatness and insulating properties are as a kind of ideal material of substrate, to nitrogen
The surface property research for changing boron is also focus；Molybdenum disulfide has special electricity, optics and catalytic performance and closed extensively
Note, its surface property all plays leading role in optics and catalysis；Research to the surface property of two-dimensional material accounts for two-dimentional material
Expect the significant portion of research, often deploy the work of this respect by means of AFM, but visit with common atomic force
The research of pin can only study the interaction between material and two-dimensional material such as silicon, it is impossible to the phase interaction between study two-dimensional material
With having no report and the research of related method.
The content of the invention
Embodiments of the invention provide a kind of atomic force microscope probe preparation method for wrapping up two-dimensional material, can be in sky
The acquisition that AFM realizes various atomic force microscope images is applied in gas and vacuum, manufacturing process is ripe easy,
It is adapted to laboratory and commercial application makes two-dimensional material modified tips probe.
To reach above-mentioned purpose, embodiments of the invention are adopted the following technical scheme that：
In a first aspect, embodiments of the invention provide a kind of atomic force microscope probe preparation side for wrapping up two-dimensional material
Method, including：
S01, is placed in the high adhesive tape of think of by two-dimensional material and sticks together face, 10 to 20 high adhesive tapes of think of of doubling form adhesive tape and sticked
Face two-dimensional material distribution；
S02, the adhesive tape face of sticking together is bonded in the oxide layer of silicon chip surface, and increase contact so that in silicon chip
Oxide layer surface residual two-dimensional material, selects the silicon chip of below thickness 30nm two-dimensional material；
S03, the silicon chip of below the thickness 30nm of selection two-dimensional material is placed on spin coating platform, spin coating polypropylene carbonate
Dried after base ester glue；
S04, intercepts one section and thinks high adhesive tape, mark the one 3 square hole to 6mm, stick at the silicon chip table dried again
Two-dimensional material piece on face, the high adhesive tape of think of of tearing, the propylene carbonate ester gum and silicon chip of spin coating departs from adhesive tape, in the pros
Shape hole tunnel opening area, forms two-dimensional material and the complex of propylene carbonate ester gum；
S05, the adhesive tape for being stained with two-dimensional material and propylene carbonate ester gum complex is placed on probe station support, hole
Part is suspended from centre, and two-dimensional material is located at propylene carbonate ester gum upper end；
S06, will have the support for thinking high adhesive tape to be rigidly secured on Probe clip, will choose average probe, will be anti-using elargol
Face is sticked on silicon chip, quartz plate or slide substrate, and it is micro- that probe tip part is placed in the temp.-regulating type four-dimension upward, by whole probe
Fixed on operating platform and with elargol；
S07, two-dimensional material is alignd with average probe needle point, adjusts 55 DEG C of initial temperature, is gradually adjusted vertical direction and is put down
The movement of platform is contacted and wrapped up with probe tip until two-dimensional material piece, increases the temperature to 120 DEG C, waits 20-30min, carbonic acid
Propylidene ester gum melts and departs from the high adhesive tape of think of, is cooled to normal temperature；
S8, the probe vacuum annealing removing glue of two-dimensional material piece will be covered with using vacuum annealing device, vacuum is 10-5Pa,
Temperature is 380 DEG C, continues 30min.
As a preferred embodiment, the oxidated layer thickness of the silicon chip surface is 300nm.
As a preferred embodiment, the silicon chip of the two-dimensional material of below the selection thickness 30nm, in addition to：
The silicon chip that two-dimensional material is distributed with is placed under light microscope, according to different two-dimensional materials on silicon chip layer
Different optical contrasts selects the two-dimensional material piece close to 30nm；
The two-dimensional material for selecting below thickness 30nm is placed under AFM and characterizes its precise thickness, 30nm is selected
Following two-dimensional material.
As a preferred embodiment, dried after spin coating propylene carbonate ester gum described in step S03, including：
Spin quality fraction is 14% propylene carbonate ester gum, and the propylene carbonate peptizing agent is methyl phenyl ethers anisole, rotation
It is that 500r/min continues 20s to apply parameter, and 1750r/s continues 40s；
The silicon chip that spin coating terminates is placed on 95 DEG C of warm table and dries 5min.
As a preferred embodiment, probe station described in step S05 includes：Computer, temp.-regulating type four-dimension microoperation platform,
Light microscope, charge coupled cell, Probe clip, optics vibration-damped table；It is characterized in that：One is secured in optics vibration-damped table
Temp.-regulating type four-dimension microoperation platform, is the movable part of the probe station, including three translations in direction and turning for horizontal direction
It is dynamic；It is vertically arranged in equipped with the light microscope of charge coupled cell directly over four-dimensional microoperation platform, charge coupled cell connects
It is connected to computer, the rigid structure region that Probe clip is fixed in optics vibration-damped table.
As a preferred embodiment, average probe described in step S06 is the finished product probe with needle point；It is either general
Logical probe or the finished product probe for being covered with metal coating.
As a preferred embodiment, two-dimensional material is alignd with average probe needle point described in step S07 is：Using micro-
Mirror image and the photo of computer collection will be general on the four-dimensional microoperation platform of the target two-dimensional material piece on Probe clip and temp.-regulating type
Logical probe tip alignment.
As a preferred embodiment, vacuum used in the method for two-dimensional material modified tips probe is prepared described in step S08
Annealing device is finished product high temperature process furnances, sets target temperature and reaches time required for target temperature, temperature up to 1200 DEG C,
The mechanical pump and molecular pump of outfit, make air pressure be down to 10-5Pa。
A kind of atomic force microscope probe preparation method for wrapping up two-dimensional material provided in an embodiment of the present invention, in air or
In vacuum, it can stablize in 500 DEG C and the environment of the above and stick on needle point, atomic force can be applied in air and vacuum
Microscope realizes the acquisition of various atomic force microscope images；The surface property research to two dimensional surface material is can apply to,
Adhesion especially between two-dimensional material, friction etc. mechanical mechanics property, easily study the special nature of large quantities of low-dimensional materials；
And manufacturing process is ripe easy, it is adapted to laboratory and commercial application makes two-dimensional material modified tips probe.
Brief description of the drawings
Technical scheme in order to illustrate the embodiments of the present invention more clearly, below by using required in embodiment
Accompanying drawing is briefly described, it should be apparent that, drawings in the following description are only some embodiments of the present invention, for ability
For the those of ordinary skill of domain, on the premise of not paying creative work, it can also be obtained according to these accompanying drawings other attached
Figure.
Fig. 1 is the schematic flow sheet of the embodiment of the present invention；
Fig. 2 has covered the table of the atomic force microscope probe of multi-layer graphene for a pair provided in an embodiment of the present invention
Levy：Wherein, (a), (b) are characterized to the light microscope of multi-layer graphene probe respectively and SEM is characterized；(c) it is right
The schematic diagram for the multi-layer graphene probe answered；(d) to the Raman Characterization for the multi-layer graphene for being attached to probe tip surface.
Embodiment
To make those skilled in the art more fully understand technical scheme, below in conjunction with the accompanying drawings and specific embodiment party
Formula is described in further detail to the present invention.It is described in more detail below embodiments of the present invention, the embodiment is shown
Example is shown in the drawings, wherein same or similar label represents same or similar element or with identical or class from beginning to end
Like the element of function.The embodiment described below with reference to accompanying drawing is exemplary, is only used for explaining the present invention, and can not
It is construed to limitation of the present invention.
Those skilled in the art of the present technique are appreciated that unless otherwise defined, all terms used herein (including technology art
Language and scientific terminology) with the general understanding identical meaning with the those of ordinary skill in art of the present invention.Should also
Understand, those terms defined in such as general dictionary, which should be understood that, to be had and the meaning in the context of prior art
The consistent meaning of justice, and unless defined as here, will not be explained with idealization or excessively formal implication.
Embodiments of the invention provide a kind of atomic force microscope probe preparation method for wrapping up two-dimensional material, can be in sky
The acquisition that AFM realizes various atomic force microscope images is applied in gas and vacuum, manufacturing process is ripe easy,
It is adapted to laboratory and commercial application makes two-dimensional material modified tips probe.
To reach above-mentioned purpose, embodiments of the invention are adopted the following technical scheme that：
In a first aspect, embodiments of the invention provide a kind of atomic force microscope probe preparation side for wrapping up two-dimensional material
Method, as shown in figure 1, including：
S01, mechanical stripping two-dimensional material；The mechanical stripping two-dimensional material is that two-dimensional material is placed in into the high adhesive tape of think of to stick together
Face, 10 to 20 high adhesive tapes of think of of doubling, forms adhesive tape and sticks together face two-dimensional material distribution；
S02, the adhesive tape face of sticking together is bonded in the oxide layer of silicon chip surface, and increase contact so that in silicon chip
Oxide layer surface residual two-dimensional material, selects the silicon chip of below thickness 30nm two-dimensional material；
S03, the silicon chip of below the thickness 30nm of selection two-dimensional material is placed on spin coating platform, spin coating polypropylene carbonate
Dried after base ester glue；
S04, intercepts one section and thinks high adhesive tape, mark the one 3 square hole to 6mm, stick at the silicon chip table dried again
Two-dimensional material piece on face, the high adhesive tape of think of of tearing, the propylene carbonate ester gum and silicon chip of spin coating departs from adhesive tape, in the pros
Shape hole tunnel opening area, forms two-dimensional material and the complex of propylene carbonate ester gum；
S05, the adhesive tape for being stained with two-dimensional material and propylene carbonate ester gum complex is placed on probe station support, hole
Part is suspended from centre, and two-dimensional material is located at propylene carbonate ester gum upper end；
S06, will have the support for thinking high adhesive tape to be rigidly secured on Probe clip, will choose average probe, will be anti-using elargol
Face is sticked on silicon chip, quartz plate or slide substrate, and it is micro- that probe tip part is placed in the temp.-regulating type four-dimension upward, by whole probe
Fixed on operating platform and with elargol；
S07, two-dimensional material is alignd with average probe needle point, adjusts 55 DEG C of initial temperature, is gradually adjusted vertical direction and is put down
The movement of platform is contacted and wrapped up with probe tip until two-dimensional material piece, increases the temperature to 120 DEG C, waits 20-30min, carbonic acid
Propylidene ester gum melts and departs from the high adhesive tape of think of, is cooled to normal temperature；
S8, the probe vacuum annealing removing glue of two-dimensional material piece will be covered with using vacuum annealing device, vacuum is 10-5Pa,
Temperature is 380 DEG C, continues 30min.
As a preferred embodiment, the oxidated layer thickness of the silicon chip surface is 300nm.
As a preferred embodiment, the silicon chip of the two-dimensional material of below the selection thickness 30nm, in addition to：
The silicon chip that two-dimensional material is distributed with is placed under light microscope, according to different two-dimensional materials on silicon chip layer
Different optical contrasts selects the two-dimensional material piece close to 30nm；
The two-dimensional material for selecting below thickness 30nm is placed under AFM and characterizes its precise thickness, 30nm is selected
Following two-dimensional material.
As a preferred embodiment, dried after spin coating propylene carbonate ester gum described in step S03, including：
Spin quality fraction is 14% propylene carbonate ester gum, and the propylene carbonate peptizing agent is methyl phenyl ethers anisole, rotation
It is that 500r/min continues 20s to apply parameter, and 1750r/s continues 40s；
The silicon chip that spin coating terminates is placed on 95 DEG C of warm table and dries 5min.
As a preferred embodiment, probe station described in step S05 includes：Computer, temp.-regulating type four-dimension microoperation platform,
Light microscope, charge coupled cell, Probe clip, optics vibration-damped table；It is characterized in that：One is secured in optics vibration-damped table
Temp.-regulating type four-dimension microoperation platform, is the movable part of the probe station, including three translations in direction and turning for horizontal direction
It is dynamic；It is vertically arranged in equipped with the light microscope of charge coupled cell directly over four-dimensional microoperation platform, charge coupled cell connects
It is connected to computer, the rigid structure region that Probe clip is fixed in optics vibration-damped table.
As a preferred embodiment, average probe described in step S06 is the finished product probe with needle point；It is either general
Logical probe or the finished product probe for being covered with metal coating.
As a preferred embodiment, two-dimensional material is alignd with average probe needle point described in step S07 is：Using micro-
Mirror image and the photo of computer collection will be general on the four-dimensional microoperation platform of the target two-dimensional material piece on Probe clip and temp.-regulating type
Logical probe tip alignment.
As a preferred embodiment, vacuum used in the method for two-dimensional material modified tips probe is prepared described in step S08
Annealing device is finished product high temperature process furnances, sets target temperature and reaches time required for target temperature, temperature up to 1200 DEG C,
The mechanical pump and molecular pump of outfit, make air pressure be down to 10-5Pa。
Specifically, the present invention is illustrated using high starch breeding, boron nitride, molybdenum disulfide as embodiment：
Embodiment 1：
The high starch breeding of selection 2mm × 2mm sizes is placed in the high adhesive tape of think of that length is about 10cm and sticks together face, mechanical stripping
High starch breeding；The mechanical stripping high starch breeding is that high starch breeding is placed in into the high adhesive tape of think of to stick together face, doubling 10 to 20
The secondary high adhesive tape of think of, forms adhesive tape and sticks together face high starch breeding distributed areas, the oxidated layer thickness of the silicon chip surface is
300nm。
The adhesive tape is sticked together into face high starch breeding distributed areas to be bonded in the oxide layer of silicon chip surface, and increases contact pressure
Power so that in the remaining high starch breeding of silicon chip layer surface, select the silicon chip of below thickness 30nm high starch breeding.It is described
The silicon chip of below thickness 30nm high starch breeding is selected, in addition to：
The silicon chip that high starch breeding is distributed with is placed under light microscope, according to different high starch breedings in silicon chip
Different optical contrasts selects the high starch breeding piece close to 30nm on layer；
The high starch breeding for selecting below thickness 30nm is placed under AFM and characterizes its precise thickness, is selected
Below 30nm high starch breeding.
The silicon chip of below the thickness 30nm of selection high starch breeding is placed on spin coating platform, spin coating propylene carbonate
Dried after ester gum.Specifically, the silicon chip of the multi-layer graphene piece is placed on spin coating platform, at normal temperatures, spin quality fraction
For 14% propylene carbonate ester gum, the propylene carbonate peptizing agent is methyl phenyl ethers anisole, and spin coating parameters continue for 500r/min
20s, 1750r/s continue 40s；
The silicon chip that spin coating terminates is placed on 95 DEG C of warm table and dries 5min.
Again intercept one section and think high adhesive tape, mark the one 3 square hole to 6mm, stick at the silicon chip surface dried.Tear
The lower high starch breeding piece thought on high adhesive tape, the propylene carbonate ester gum and silicon chip of spin coating departs from adhesive tape, in the square
Hole tunnel opening area, forms the complex of high starch breeding and propylene carbonate ester gum.
The adhesive tape for being stained with high starch breeding and propylene carbonate ester gum complex is placed on probe station support, hole portion
Divide and be suspended from centre, high starch breeding is located at propylene carbonate ester gum upper end.
Specifically, the probe station includes：Computer, temp.-regulating type four-dimension microoperation platform, light microscope, Charged Couple
Element, Probe clip, optics vibration-damped table；It is characterized in that：The four-dimensional microoperation of a temp.-regulating type is secured in optics vibration-damped table to put down
Platform, is the movable part of the probe station, includes the translation and the rotation of horizontal direction in three directions；Equipped with Charged Couple member
The light microscope of part is vertically arranged in directly over four-dimensional microoperation platform, and charge coupled cell is connected to computer, and probe is clamping
Due to the rigid structure region in optics vibration-damped table.
There to be the support for thinking high adhesive tape to be rigidly secured on Probe clip, average probe will be chosen, glued reverse side using elargol
On silicon chip, quartz plate or slide substrate, whole probe upward, is placed in the four-dimensional microoperation of temp.-regulating type by probe tip part
Fixed on platform and with elargol.
Wherein, the average probe, is the finished product probe with needle point；Either average probe or it is covered with metal coating
Finished product probe.
High starch breeding is alignd with average probe needle point, 55 DEG C of initial temperature is adjusted, vertical direction platform is gradually adjusted
Movement contact and wrap up with probe tip until high starch breeding piece, increase the temperature to 120 DEG C, wait 20-30min, carbonic acid
Propylidene ester gum melts and departs from the high adhesive tape of think of, is cooled to normal temperature.
Described high starch breeding aligns with average probe needle point be：The photo gathered using MIcrosope image and computer will
High starch breeding on Probe clip aligns with the average probe needle point on the four-dimensional microoperation platform of temp.-regulating type.
The probe vacuum annealing removing glue of high starch breeding piece will be covered with using vacuum annealing device, vacuum is 10-5Pa,
Temperature is 380 DEG C, continues 30min, you can obtain final product and be covered with high starch breeding (being also referred to as when wherein, the number of plies is very more
For multi-layer graphene) atomic force microscope probe.
Vacuum annealing device used in the method for preparing two-dimensional material modified tips probe is finished product high temperature process furnances, if
Put target temperature and reach the time required for target temperature, temperature is up to 1200 DEG C, and the mechanical pump and molecular pump of outfit make air pressure
It is down to 10-5Pa。
The series of the present embodiment is characterized as shown in Fig. 2 Fig. 2 is visited to having covered the AFM of multi-layer graphene
The sign of pin：Wherein, what (a), (b) were represented is that the light microscope sign and scanning electron of multi-layer graphene probe are shown respectively
Micro mirror is characterized；(c) what is represented is the schematic diagram of corresponding multi-layer graphene probe；(d) what is represented is to being attached to probe tip
The Raman Characterization of the multi-layer graphene on surface.
Embodiment 2：
The boron nitride of selection 2mm × 2mm sizes is placed in the high adhesive tape of think of that length is about 10cm and sticks together face, mechanical stripping nitridation
Boron；The mechanical stripping boron nitride is that boron nitride is placed in into the high adhesive tape of think of to stick together face, 10 to 20 high adhesive tapes of think of of doubling, shape
Plastic band sticks together face boron nitride distributed areas, and the oxidated layer thickness of the silicon chip surface is 300nm.
The adhesive tape is sticked together into face boron nitride distributed areas to be bonded in the oxide layer of silicon chip surface, and increases contact,
So that in the remaining boron nitride of silicon chip layer surface, selecting the silicon chip of below thickness 30nm boron nitride.The selection thickness
The silicon chip of below 30nm boron nitride, in addition to：
The silicon chip that boron nitride is distributed with is placed under light microscope, according to different boron nitride on silicon chip layer it is different
Optical contrast select the boron nitride piece close to 30nm；
The boron nitride for selecting below thickness 30nm is placed under AFM and characterizes its precise thickness, selection 30nm with
Under boron nitride.
The silicon chip of below the thickness 30nm of selection boron nitride is placed on spin coating platform, spin coating propylene carbonate ester gum
After dry.Specifically, the silicon chip of the multi-layer graphene piece is placed on spin coating platform, at normal temperatures, spin quality fraction is
14% propylene carbonate ester gum, the propylene carbonate peptizing agent is methyl phenyl ethers anisole, and spin coating parameters continue for 500r/min
20s, 1750r/s continue 40s；
The silicon chip that spin coating terminates is placed on 95 DEG C of warm table and dries 5min.
Again intercept one section and think high adhesive tape, mark the one 3 square hole to 6mm, stick at the silicon chip surface dried.Tear
The lower boron nitride piece thought on high adhesive tape, the propylene carbonate ester gum and silicon chip of spin coating departs from adhesive tape, in the square hole hole
Mouth region domain, forms the complex of boron nitride and propylene carbonate ester gum.
The adhesive tape for being stained with boron nitride and propylene carbonate ester gum complex is placed on probe station support, hole part hangs
In centre, boron nitride is located at propylene carbonate ester gum upper end.
Specifically, the probe station includes：Computer, temp.-regulating type four-dimension microoperation platform, light microscope, Charged Couple
Element, Probe clip, optics vibration-damped table；It is characterized in that：The four-dimensional microoperation of a temp.-regulating type is secured in optics vibration-damped table to put down
Platform, is the movable part of the probe station, includes the translation and the rotation of horizontal direction in three directions；Equipped with Charged Couple member
The light microscope of part is vertically arranged in directly over four-dimensional microoperation platform, and charge coupled cell is connected to computer, and probe is clamping
Due to the rigid structure region in optics vibration-damped table.
There to be the support for thinking high adhesive tape to be rigidly secured on Probe clip, average probe will be chosen, glued reverse side using elargol
On silicon chip, quartz plate or slide substrate, whole probe upward, is placed in the four-dimensional microoperation of temp.-regulating type by probe tip part
Fixed on platform and with elargol.
Wherein, the average probe, is the finished product probe with needle point；Either average probe or it is covered with metal coating
Finished product probe.
Boron nitride is alignd with average probe needle point, 55 DEG C of initial temperature is adjusted, the shifting of vertical direction platform is gradually adjusted
It is dynamic to increase the temperature to 120 DEG C until boron nitride piece is contacted and wrapped up with probe tip, wait 20-30min, propylene carbonate
Glue melts and departs from the high adhesive tape of think of, is cooled to normal temperature.
Described boron nitride aligns with average probe needle point be：The photo gathered using MIcrosope image and computer is by probe
Boron nitride on folder aligns with the average probe needle point on the four-dimensional microoperation platform of temp.-regulating type.
The probe vacuum annealing removing glue of boron nitride piece will be covered with using vacuum annealing device, vacuum is 10-5Pa, temperature
For 380 DEG C, continue 30min, you can obtain the atomic force microscope probe that final product is covered with boron nitride.
Vacuum annealing device used in the method for preparing two-dimensional material modified tips probe is finished product high temperature process furnances, if
Put target temperature and reach the time required for target temperature, temperature is up to 1200 DEG C, and the mechanical pump and molecular pump of outfit make air pressure
It is down to 10-5Pa。
Embodiment 3：
The molybdenum disulfide of selection 2mm × 2mm sizes is placed in the high adhesive tape of think of that length is about 10cm and sticks together face, mechanical stripping two
Molybdenum sulfide；The mechanical stripping molybdenum disulfide is that molybdenum disulfide is placed in into the high adhesive tape of think of to stick together face, 10 to 20 think ofs of doubling
High adhesive tape, forms adhesive tape and sticks together face molybdenum disulfide distributed areas, the oxidated layer thickness of the silicon chip surface is 300nm.
The adhesive tape is sticked together into face molybdenum disulfide distributed areas to be bonded in the oxide layer of silicon chip surface, and increases contact pressure
Power so that in the remaining molybdenum disulfide of silicon chip layer surface, select the silicon chip of below thickness 30nm molybdenum disulfide.The selection
The silicon chip of below thickness 30nm molybdenum disulfide, in addition to：
The silicon chip that molybdenum disulfide is distributed with is placed under light microscope, according to different molybdenum disulfide on silicon chip layer
Different optical contrasts selects the curing molybdenum sheet close to 30nm；
The molybdenum disulfide for selecting below thickness 30nm is placed under AFM and characterizes its precise thickness, 30nm is selected
Following molybdenum disulfide.
The silicon chip of below the thickness 30nm of selection molybdenum disulfide is placed on spin coating platform, spin coating propylene carbonate
Dried after glue.Specifically, the silicon chip of the multi-layer graphene piece is placed on spin coating platform, at normal temperatures, spin quality fraction is
14% propylene carbonate ester gum, the propylene carbonate peptizing agent is methyl phenyl ethers anisole, and spin coating parameters continue for 500r/min
20s, 1750r/s continue 40s；
The silicon chip that spin coating terminates is placed on 95 DEG C of warm table and dries 5min.
Again intercept one section and think high adhesive tape, mark the one 3 square hole to 6mm, stick at the silicon chip surface dried.Tear
The lower curing molybdenum sheet thought on high adhesive tape, the propylene carbonate ester gum and silicon chip of spin coating departs from adhesive tape, in the square hole
Tunnel opening area, forms the complex of molybdenum disulfide and propylene carbonate ester gum.
The adhesive tape for being stained with molybdenum disulfide and propylene carbonate ester gum complex is placed on probe station support, hole part
Centre is suspended from, molybdenum disulfide is located at propylene carbonate ester gum upper end.
Specifically, the probe station includes：Computer, temp.-regulating type four-dimension microoperation platform, light microscope, Charged Couple
Element, Probe clip, optics vibration-damped table；It is characterized in that：The four-dimensional microoperation of a temp.-regulating type is secured in optics vibration-damped table to put down
Platform, is the movable part of the probe station, includes the translation and the rotation of horizontal direction in three directions；Equipped with Charged Couple member
The light microscope of part is vertically arranged in directly over four-dimensional microoperation platform, and charge coupled cell is connected to computer, and probe is clamping
Due to the rigid structure region in optics vibration-damped table.
There to be the support for thinking high adhesive tape to be rigidly secured on Probe clip, average probe will be chosen, glued reverse side using elargol
On silicon chip, quartz plate or slide substrate, whole probe upward, is placed in the four-dimensional microoperation of temp.-regulating type by probe tip part
Fixed on platform and with elargol.
Wherein, the average probe, is the finished product probe with needle point；Either average probe or it is covered with metal coating
Finished product probe.
Molybdenum disulfide is alignd with average probe needle point, 55 DEG C of initial temperature is adjusted, vertical direction platform is gradually adjusted
It is mobile to increase the temperature to 120 DEG C until curing molybdenum sheet is contacted and wrapped up with probe tip, wait 20-30min, polypropylene carbonate
Base ester glue melts and departs from the high adhesive tape of think of, is cooled to normal temperature.
Described molybdenum disulfide aligns with average probe needle point be：The photo gathered using MIcrosope image and computer will be visited
Molybdenum disulfide on pin folder aligns with the average probe needle point on the four-dimensional microoperation platform of temp.-regulating type.
The probe vacuum annealing removing glue of curing molybdenum sheet will be covered with using vacuum annealing device, vacuum is 10-5Pa, temperature
For 380 DEG C, continue 30min, you can obtain the atomic force microscope probe that final product is covered with molybdenum disulfide.
Vacuum annealing device used in the method for preparing two-dimensional material modified tips probe is finished product high temperature process furnances, if
Put target temperature and reach the time required for target temperature, temperature is up to 1200 DEG C, and the mechanical pump and molecular pump of outfit make air pressure
It is down to 10-5Pa。
A kind of atomic force microscope probe preparation method for wrapping up two-dimensional material provided in an embodiment of the present invention, in air or
In vacuum, it can stablize in 500 DEG C of environment and stick on needle point, AFM can be applied in air and vacuum
Realize the acquisition of various atomic force microscope images；The surface property research to two dimensional surface material is can apply to, especially
Adhesion between two-dimensional material, friction etc. mechanical mechanics property, easily study the special nature of large quantities of low-dimensional materials；And make
Process matures are easy, be adapted to laboratory and commercial application makes two-dimensional material modified tips probe.
Each embodiment in this specification is described by the way of progressive, identical similar portion between each embodiment
Divide mutually referring to what each embodiment was stressed is the difference with other embodiment.It is real especially for equipment
Apply for example, because it is substantially similar to embodiment of the method, so describing fairly simple, related part is referring to embodiment of the method
Part explanation.
The foregoing is only a specific embodiment of the invention, but protection scope of the present invention is not limited thereto, any
Those familiar with the art the invention discloses technical scope in, the change or replacement that can be readily occurred in, all should
It is included within the scope of the present invention.Therefore, protection scope of the present invention should be defined by scope of the claims.
Claims (8)
1. a kind of atomic force microscope probe preparation method for wrapping up two-dimensional material, it is characterised in that including：
S01, is placed in the high adhesive tape of think of by two-dimensional material and sticks together face, 10 to 20 high adhesive tapes of think of of doubling form adhesive tape and stick together face
Two-dimensional material is distributed；
S02, the adhesive tape face of sticking together is bonded in the oxide layer of silicon chip surface, and increase contact so that in silicon chip
Layer surface residue two-dimensional material, selects the silicon chip of below thickness 30nm two-dimensional material；
S03, the silicon chip of below the thickness 30nm of selection two-dimensional material is placed on spin coating platform, spin coating propylene carbonate
Dried after glue；
S04, intercepts one section and thinks high adhesive tape, mark the one 3 square hole to 6mm, stick at the silicon chip surface dried, tear again
The lower two-dimensional material piece thought on high adhesive tape, the propylene carbonate ester gum and silicon chip of spin coating departs from adhesive tape, in the square hole
Tunnel opening area, forms two-dimensional material and the complex of propylene carbonate ester gum；
S05, the adhesive tape for being stained with two-dimensional material and propylene carbonate ester gum complex is placed on probe station support, hole part
Centre is suspended from, two-dimensional material is located at propylene carbonate ester gum upper end；
S06, will have the support for thinking high adhesive tape to be rigidly secured on Probe clip, will choose average probe, glued reverse side using elargol
On silicon chip, quartz plate or slide substrate, whole probe upward, is placed in the four-dimensional microoperation of temp.-regulating type by probe tip part
Fixed on platform and with elargol；
S07, two-dimensional material is alignd with average probe needle point, adjusts 55 DEG C of initial temperature, gradually adjusts vertical direction platform
It is mobile to increase the temperature to 120 DEG C until two-dimensional material piece is contacted and wrapped up with probe tip, wait 20-30min, polypropylene carbonate
Base ester glue melts and departs from the high adhesive tape of think of, is cooled to normal temperature；
S08, the probe vacuum annealing removing glue of two-dimensional material piece will be covered with using vacuum annealing device, vacuum is 10-5Pa, temperature
For 380 DEG C, continue 30min.
2. a kind of atomic force microscope probe preparation method for wrapping up two-dimensional material according to claim 1, its feature exists
In：
The oxidated layer thickness of the silicon chip surface is 300nm.
3. a kind of atomic force microscope probe preparation method for wrapping up two-dimensional material according to claim 1, its feature exists
In, the silicon chip of the two-dimensional material of selection below the thickness 30nm, in addition to：
The silicon chip that two-dimensional material is distributed with is placed under light microscope, according to different two-dimensional materials on silicon chip layer it is different
Optical contrast select the two-dimensional material piece close to 30nm；
The two-dimensional material for selecting below thickness 30nm is placed under AFM and characterizes its precise thickness, below 30nm is selected
Two-dimensional material.
4. a kind of atomic force microscope probe preparation method for wrapping up two-dimensional material according to claim 1, its feature exists
In, dried after spin coating propylene carbonate ester gum described in step S03, including：
Spin quality fraction is 14% propylene carbonate ester gum, and the propylene carbonate peptizing agent is methyl phenyl ethers anisole, spin coating ginseng
Number continues 20s for 500r/min, and 1750r/s continues 40s；
The silicon chip that spin coating terminates is placed on 95 DEG C of warm table and dries 5min.
5. a kind of atomic force microscope probe preparation method for wrapping up two-dimensional material according to claim 1, its feature exists
In probe station described in step S05 includes：Computer, temp.-regulating type four-dimension microoperation platform, light microscope, charge coupled cell,
Probe clip, optics vibration-damped table；It is characterized in that：The four-dimensional microoperation platform of a temp.-regulating type is secured in optics vibration-damped table, is
The movable part of the probe station, includes the translation and the rotation of horizontal direction in three directions；Equipped with charge coupled cell
Light microscope is vertically arranged in directly over four-dimensional microoperation platform, and charge coupled cell is connected to computer, and Probe clip is fixed on
Rigid structure region in optics vibration-damped table.
6. a kind of atomic force microscope probe preparation method for wrapping up two-dimensional material according to claim 1, its feature exists
In average probe described in step S06 is the finished product probe with needle point；Either average probe or be covered with metal coating into
Product probe.
7. a kind of atomic force microscope probe preparation method for wrapping up two-dimensional material according to claim 1, its feature exists
In two-dimensional material is alignd with average probe needle point described in step S07 is：The photo gathered using MIcrosope image and computer will
Target two-dimensional material piece on Probe clip aligns with the average probe needle point on the four-dimensional microoperation platform of temp.-regulating type.
8. a kind of atomic force microscope probe preparation method for wrapping up two-dimensional material according to claim 1, its feature exists
In, vacuum annealing device used in the method for preparation two-dimensional material modified tips probe described in step S08 is finished product high temperature process furnances,
Target temperature is set and time required for target temperature is reached, temperature is up to 1200 DEG C, and the mechanical pump and molecular pump of outfit make gas
Pressure drop is to 10-5Pa。
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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 |
| CN108398578A (en) * | 2018-01-15 | 2018-08-14 | 大连理工大学 | A method of using modified by magnetic nanoparticles atomic force microscope probe |
| CN108502620A (en) * | 2018-03-15 | 2018-09-07 | 东南大学 | A kind of folding system and its application method of two-dimensional material |
| 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 |
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| CN114236183A (en) * | 2021-12-17 | 2022-03-25 | 湘潭大学 | Preparation method of atomic force microscope probe wrapping two-dimensional material |
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| CN108398578A (en) * | 2018-01-15 | 2018-08-14 | 大连理工大学 | A method of using modified by magnetic nanoparticles atomic force microscope probe |
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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 |
| CN108375687B (en) * | 2018-03-09 | 2020-12-04 | 北京协同创新研究院 | Method for coating graphene on probe tip of atomic force microscope |
| CN108502620A (en) * | 2018-03-15 | 2018-09-07 | 东南大学 | A kind of folding system and its application method of two-dimensional material |
| CN108502620B (en) * | 2018-03-15 | 2019-08-27 | 东南大学 | A kind of folding system and its application method of two-dimensional material |
| 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 |
| 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 |
| 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 |
| CN110117780A (en) * | 2019-03-19 | 2019-08-13 | 中国科学院上海微***与信息技术研究所 | A kind of two-dimensional material layer and preparation method |
| WO2021120233A1 (en) * | 2019-12-20 | 2021-06-24 | 江苏集萃微纳自动化***与装备技术研究所有限公司 | Real-time stiffness adjustment method for probe of atomic force microscope |
| CN114236183A (en) * | 2021-12-17 | 2022-03-25 | 湘潭大学 | Preparation method of atomic force microscope probe wrapping two-dimensional material |
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