CN107328956B - Preparation method of atomic force microscope probe wrapping two-dimensional material - Google Patents
Preparation method of atomic force microscope probe wrapping two-dimensional material Download PDFInfo
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- CN107328956B CN107328956B CN201710413065.2A CN201710413065A CN107328956B CN 107328956 B CN107328956 B CN 107328956B CN 201710413065 A CN201710413065 A CN 201710413065A CN 107328956 B CN107328956 B CN 107328956B
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- 239000000463 material Substances 0.000 title claims abstract description 115
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- 238000000034 method Methods 0.000 claims abstract description 32
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- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 claims description 53
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- RDOXTESZEPMUJZ-UHFFFAOYSA-N anisole Chemical group COC1=CC=CC=C1 RDOXTESZEPMUJZ-UHFFFAOYSA-N 0.000 claims description 12
- 229910052709 silver Inorganic materials 0.000 claims description 12
- 239000004332 silver Substances 0.000 claims description 12
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- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 30
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
- G01Q60/00—Particular types of SPM [Scanning Probe Microscopy] or microscopes; Essential components thereof
- G01Q60/24—AFM [Atomic Force Microscopy] or apparatus therefor, e.g. AFM probes
- G01Q60/38—Probes, their manufacture, or their related instrumentation, e.g. holders
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- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Radiology & Medical Imaging (AREA)
- Length Measuring Devices With Unspecified Measuring Means (AREA)
- Testing Or Measuring Of Semiconductors Or The Like (AREA)
Abstract
The embodiment of the invention provides a preparation method of an atomic force microscope probe wrapping a two-dimensional material, and relates to the technical field of modification and processing of atomic force microscope probes. The method provided by the embodiment of the invention can be stably adhered to the needle point in the air or vacuum environment at 500 ℃, and can be applied to an atomic force microscope in the air and vacuum environment to realize the acquisition of various atomic force microscope images; the method can be applied to the surface property research of two-dimensional plane materials, especially the mechanical properties such as adhesion and friction between two-dimensional materials, and can conveniently research the special properties of a large quantity of low-dimensional materials; and the manufacturing process is mature and simple, and the method is suitable for manufacturing the two-dimensional material modified probe tip in laboratories and industrialized application.
Description
Technical Field
The invention relates to the technical field of modification and processing of atomic force microscope probes, in particular to a preparation method of an atomic force microscope probe wrapping a two-dimensional material.
Background
The atomic force microscope is invented by Gerd Binnig of research center of Zurich of IBM company in 1985, can detect surface properties such as surface roughness, surface electric, magnetic and mechanical properties, surface adhesion and the like of a substrate material with high resolution, and has become a multidisciplinary, including microstructure observation of physics, chemistry, biology, material science, electricity, mechanics and the like, micro-nano scale processing, micro-nano displacement, micro-force application and the like. The atomic force microscope probe generally comprises a main body, a micro-cantilever, a micro-tip and the like, wherein the shape of the micro-cantilever is divided into a rectangle, a triangle and the like. The probe tip of the probe dominates the performance and the variety of the atomic force microscope, a common atomic force microscope probe is manufactured through the processing procedure of semiconductor materials, conventionally made of silicon and silicon nitride as basic materials, and metal plating layers such as metal deposition, sputtering and the like are utilized to improve the conductivity or increase the new performance; in recent decades, much attention has been paid to the modification and processing of atomic force microscope tips, which use the special properties of various low dimensional materials including carbon nanotubes to obtain various materials having new functions, excellent resolution and excellent image quality, or to meet the special requirements of a certain field, etc.
Two-dimensional materials have attracted wide attention since 2004, mainly including graphene, boron nitride, molybdenum disulfide and the like, the graphene has excellent electrical, optical, magnetic and other properties, and is widely and deeply researched, the graphene also has extremely high mechanical properties, and the elastic constant of the graphene reaches 1 TPa; due to the extremely large surface structure of the two-dimensional material, the graphene can bear 20% of in-plane strain without causing structural damage; boron nitride is a two-dimensional material with a crystal structure similar to graphene, has good insulating property, has surface atomic-level flatness and insulating property as an ideal material of a substrate, and is a hot spot for the surface performance research of boron nitride; molybdenum disulfide has special electrical, optical and catalytic properties and is widely concerned, and the surface properties of molybdenum disulfide play a leading role in both optics and catalysis; the research on the surface performance of the two-dimensional material accounts for a large part of the research on the two-dimensional material, and the work in this respect is usually carried out by taking an atomic force microscope as a means, but the research on the common atomic force probe can only research the interaction between the material such as silicon and the two-dimensional material, but cannot research the interaction between the two-dimensional material, and no report and research on related methods are found.
Disclosure of Invention
The embodiment of the invention provides a preparation method of an atomic force microscope probe wrapped by a two-dimensional material, which can be applied to an atomic force microscope in air and vacuum to realize the acquisition of various atomic force microscope images, has mature and simple manufacturing process, and is suitable for manufacturing a two-dimensional material modified needle point probe in a laboratory and industrialized application.
In order to achieve the above purpose, the embodiment of the invention adopts the following technical scheme:
in a first aspect, an embodiment of the present invention provides a method for preparing an atomic force microscope probe wrapped in a two-dimensional material, including:
s01, placing the two-dimensional material on the adhesive surface of the Siji adhesive tape, folding the Siji adhesive tape for 10 to 20 times to form two-dimensional material distribution of the adhesive surface of the adhesive tape;
s02, adhering the adhesive surface of the adhesive tape to the oxide layer on the surface of the silicon wafer, and increasing the contact pressure to ensure that two-dimensional materials remain on the surface of the oxide layer of the silicon wafer, wherein the silicon wafer is made of two-dimensional materials with the thickness of less than 30 nm;
s03, placing the selected silicon wafer of the two-dimensional material with the thickness of less than 30nm on a spin-coating table, spin-coating the propylene carbonate glue, and drying;
s04, cutting a section of Siji tape again, marking a square hole of 3-6 mm, adhering the square hole on the surface of the dried silicon wafer, tearing off the Siji tape, separating the spin-coated propylene carbonate adhesive and the two-dimensional material sheet on the silicon wafer along with the tape, and forming a complex of the two-dimensional material and the propylene carbonate adhesive in the area of the square hole;
s05, placing the adhesive tape adhered with the two-dimensional material and the propylene carbonate glue complex on a probe station support, suspending the hole part in the middle, and positioning the two-dimensional material at the upper end of the propylene carbonate glue;
s06, rigidly fixing the support of the Sigao tape on a probe clamp, selecting a common probe, adhering the back surface on a silicon wafer, a quartz plate or a glass slide substrate by utilizing silver colloid, enabling the probe tip to face upwards, placing the whole probe on a temperature-regulating four-dimensional micro-operation platform and fixing the whole probe by utilizing the silver colloid;
s07, aligning the two-dimensional material with the tip of a common probe, adjusting the initial temperature to 55 ℃, gradually adjusting the movement of the platform in the vertical direction until the two-dimensional material sheet is contacted with and wrapped by the tip of the probe, raising the temperature to 120 ℃, waiting for 20-30min, melting the propylene carbonate adhesive, separating from the Sigao tape, and cooling to normal temperature;
s8, performing vacuum annealing and glue removal on the probe coated with the two-dimensional material sheet by using a vacuum annealing device, wherein the vacuum degree is 10-5Pa, at 380 ℃ for 30 min.
As a preferred embodiment, the thickness of the oxide layer on the surface of the silicon wafer is 300 nm.
As a preferred embodiment, the selecting a silicon wafer of two-dimensional material with a thickness of 30nm or less further comprises:
placing the silicon wafer distributed with the two-dimensional material under an optical microscope, and selecting a two-dimensional material sheet with the thickness close to 30nm according to different optical contrasts of different two-dimensional materials on an oxide layer of the silicon wafer;
and (3) placing the two-dimensional material with the thickness of below 30nm under an atomic force microscope to characterize the accurate thickness of the two-dimensional material, and selecting the two-dimensional material with the thickness of below 30 nm.
As a preferred embodiment, the spin-coating of the propylene carbonate paste in step S03 is followed by drying, which includes:
carrying out spin coating on 14% propylene carbonate glue by mass, wherein a propylene carbonate glue solvent is anisole, and spin coating parameters are 500r/min for 20s and 1750r/s for 40 s;
and (3) drying the silicon wafer subjected to spin coating for 5min on a heating table at 95 ℃.
As a preferred embodiment, the probe station of step S05 includes: the system comprises a computer, a temperature-adjusting four-dimensional micro-operation platform, an optical microscope, a charge coupling element, a probe clamp and an optical shock absorption table; the method is characterized in that: a temperature-adjusting four-dimensional micro-operation platform is fixed on the optical shock absorption platform, is a moving part of the probe platform and comprises translation in three directions and rotation in the horizontal direction; an optical microscope equipped with a charge-coupled device is vertically arranged right above the four-dimensional micro-operation platform, the charge-coupled device is connected with a computer, and a probe clamp is fixed on a rigid structure area on an optical shock absorption platform.
As a preferred embodiment, the general probe of step S06 is a finished probe with a tip; or a common probe or a finished probe coated with a metal coating.
As a preferred embodiment, the step S07 of aligning the two-dimensional material with a common probe tip is: and aligning a target two-dimensional material sheet on the probe clamp with a common probe tip on the temperature-regulating four-dimensional micro-operation platform by using a microscope image and a photo acquired by a computer.
As a preferred embodiment, the vacuum annealing apparatus used in the method for preparing a two-dimensional material modified tip probe described in step S08 is a high-temperature tube furnace for the final product, and the target temperature and the time required to reach the target temperature are set to 1200 ℃ and a mechanical pump and a molecular pump are provided to reduce the gas pressure to 10%-5Pa。
The atomic force microscope probe coated with the two-dimensional material can be stably adhered to a needle tip in air or vacuum at the temperature of 500 ℃ or above, and can be applied to an atomic force microscope in air and vacuum to obtain various atomic force microscope images; the method can be applied to the surface property research of two-dimensional plane materials, especially the mechanical properties such as adhesion and friction between two-dimensional materials, and can conveniently research the special properties of a large quantity of low-dimensional materials; and the manufacturing process is mature and simple, and the method is suitable for manufacturing the two-dimensional material modified probe tip in laboratories and industrialized application.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic flow chart of an embodiment of the present invention;
fig. 2 is a representation of a pair of afm probes that have been covered with multi-layer graphene according to an embodiment of the present invention: respectively representing the optical microscope and the scanning electron microscope of the multilayer graphene probe by (a) and (b); (c) a schematic representation of a corresponding multi-layer graphene probe; (d) and (3) characterizing the Raman spectrum of the multilayer graphene attached to the surface of the probe tip.
Detailed Description
In order to make the technical solutions of the present invention better understood, the present invention will be described in further detail with reference to the accompanying drawings and specific embodiments. Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the accompanying drawings are illustrative only for the purpose of explaining the present invention, and are not to be construed as limiting the present invention.
It will be understood by those skilled in the art that, unless otherwise defined, all terms (including technical and scientific terms) used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. It will be further understood that terms, such as those defined in commonly used dictionaries, should be interpreted as having a meaning that is consistent with their meaning in the context of the prior art and will not be interpreted in an idealized or overly formal sense unless expressly so defined herein.
The embodiment of the invention provides a preparation method of an atomic force microscope probe wrapped by a two-dimensional material, which can be applied to an atomic force microscope in air and vacuum to realize the acquisition of various atomic force microscope images, has mature and simple manufacturing process, and is suitable for manufacturing a two-dimensional material modified needle point probe in a laboratory and industrialized application.
In order to achieve the above purpose, the embodiment of the invention adopts the following technical scheme:
in a first aspect, an embodiment of the present invention provides a method for preparing an atomic force microscope probe wrapped in a two-dimensional material, as shown in fig. 1, including:
s01, mechanically stripping the two-dimensional material; the mechanical peeling of the two-dimensional material is to place the two-dimensional material on the adhesive surface of the SiGao adhesive tape, and fold the SiGao adhesive tape for 10 to 20 times to form the two-dimensional material distribution of the adhesive surface of the adhesive tape;
s02, adhering the adhesive surface of the adhesive tape to the oxide layer on the surface of the silicon wafer, and increasing the contact pressure to ensure that two-dimensional materials remain on the surface of the oxide layer of the silicon wafer, wherein the silicon wafer is made of two-dimensional materials with the thickness of less than 30 nm;
s03, placing the selected silicon wafer of the two-dimensional material with the thickness of less than 30nm on a spin-coating table, spin-coating the propylene carbonate glue, and drying;
s04, cutting a section of Siji tape again, marking a square hole of 3-6 mm, adhering the square hole on the surface of the dried silicon wafer, tearing off the Siji tape, separating the spin-coated propylene carbonate adhesive and the two-dimensional material sheet on the silicon wafer along with the tape, and forming a complex of the two-dimensional material and the propylene carbonate adhesive in the area of the square hole;
s05, placing the adhesive tape adhered with the two-dimensional material and the propylene carbonate glue complex on a probe station support, suspending the hole part in the middle, and positioning the two-dimensional material at the upper end of the propylene carbonate glue;
s06, rigidly fixing the support of the Sigao tape on a probe clamp, selecting a common probe, adhering the back surface on a silicon wafer, a quartz plate or a glass slide substrate by utilizing silver colloid, enabling the probe tip to face upwards, placing the whole probe on a temperature-regulating four-dimensional micro-operation platform and fixing the whole probe by utilizing the silver colloid;
s07, aligning the two-dimensional material with the tip of a common probe, adjusting the initial temperature to 55 ℃, gradually adjusting the movement of the platform in the vertical direction until the two-dimensional material sheet is contacted with and wrapped by the tip of the probe, raising the temperature to 120 ℃, waiting for 20-30min, melting the propylene carbonate adhesive, separating from the Sigao tape, and cooling to normal temperature;
s8, performing vacuum annealing and glue removal on the probe coated with the two-dimensional material sheet by using a vacuum annealing device, wherein the vacuum degree is 10-5Pa, at 380 ℃ for 30 min.
As a preferred embodiment, the thickness of the oxide layer on the surface of the silicon wafer is 300 nm.
As a preferred embodiment, the selecting a silicon wafer of two-dimensional material with a thickness of 30nm or less further comprises:
placing the silicon wafer distributed with the two-dimensional material under an optical microscope, and selecting a two-dimensional material sheet with the thickness close to 30nm according to different optical contrasts of different two-dimensional materials on an oxide layer of the silicon wafer;
and (3) placing the two-dimensional material with the thickness of below 30nm under an atomic force microscope to characterize the accurate thickness of the two-dimensional material, and selecting the two-dimensional material with the thickness of below 30 nm.
As a preferred embodiment, the spin-coating of the propylene carbonate paste in step S03 is followed by drying, which includes:
carrying out spin coating on 14% propylene carbonate glue by mass, wherein a propylene carbonate glue solvent is anisole, and spin coating parameters are 500r/min for 20s and 1750r/s for 40 s;
and (3) drying the silicon wafer subjected to spin coating for 5min on a heating table at 95 ℃.
As a preferred embodiment, the probe station of step S05 includes: the system comprises a computer, a temperature-adjusting four-dimensional micro-operation platform, an optical microscope, a charge coupling element, a probe clamp and an optical shock absorption table; the method is characterized in that: a temperature-adjusting four-dimensional micro-operation platform is fixed on the optical shock absorption platform, is a moving part of the probe platform and comprises translation in three directions and rotation in the horizontal direction; an optical microscope equipped with a charge-coupled device is vertically arranged right above the four-dimensional micro-operation platform, the charge-coupled device is connected with a computer, and a probe clamp is fixed on a rigid structure area on an optical shock absorption platform.
As a preferred embodiment, the general probe of step S06 is a finished probe with a tip; or a common probe or a finished probe coated with a metal coating.
As a preferred embodiment, the step S07 of aligning the two-dimensional material with a common probe tip is: and aligning a target two-dimensional material sheet on the probe clamp with a common probe tip on the temperature-regulating four-dimensional micro-operation platform by using a microscope image and a photo acquired by a computer.
As a preferred embodiment, the vacuum annealing apparatus used in the method for preparing a two-dimensional material modified tip probe described in step S08 is a high-temperature tube furnace for the final product, and the target temperature and the time required to reach the target temperature are set to 1200 ℃ and a mechanical pump and a molecular pump are provided to reduce the gas pressure to 10%-5Pa。
Specifically, the invention is illustrated by taking highly oriented graphite, boron nitride and molybdenum disulfide as examples:
example 1:
selecting high-orientation graphite with the size of 2mm multiplied by 2mm, placing the high-orientation graphite on an adhesive surface of a Sichuan tape with the length of about 10cm, and mechanically stripping the high-orientation graphite; the mechanical stripping of the highly oriented graphite is to place the highly oriented graphite on the adhesive surface of the SiGao tape, fold the SiGao tape for 10 to 20 times to form the distribution area of the highly oriented graphite on the adhesive surface of the tape, and the thickness of the oxide layer on the surface of the silicon wafer is 300 nm.
And adhering the highly-oriented graphite distribution region of the adhesive tape adhesion surface to an oxide layer on the surface of the silicon wafer, and increasing contact pressure to ensure that highly-oriented graphite remains on the surface of the oxide layer of the silicon wafer, and selecting the silicon wafer with the thickness of less than 30nm and highly-oriented graphite. The silicon wafer of highly oriented graphite with the thickness of less than 30nm is selected, and further comprises:
placing the silicon wafer distributed with the highly oriented graphite under an optical microscope, and selecting the highly oriented graphite sheet close to 30nm according to different optical contrasts of different highly oriented graphite on an oxide layer of the silicon wafer;
and (3) placing the highly-oriented graphite with the thickness of less than 30nm under an atomic force microscope to characterize the accurate thickness of the highly-oriented graphite, and selecting the highly-oriented graphite with the thickness of less than 30 nm.
And placing the selected highly-oriented graphite silicon wafer with the thickness of less than 30nm on a spin-coating table, spin-coating the propylene carbonate adhesive, and drying. Specifically, a silicon wafer of the multilayer graphene sheet is placed on a spin-coating platform, propylene carbonate glue with the mass fraction of 14% is spin-coated at normal temperature, the propylene carbonate glue solvent is anisole, the spin-coating parameter is 500r/min and lasts for 20s, and the spin-coating parameter is 1750r/s and lasts for 40 s;
and (3) drying the silicon wafer subjected to spin coating for 5min on a heating table at 95 ℃.
And cutting a section of Sigao adhesive tape again, marking a square hole with the diameter of 3-6 mm, and adhering the square hole on the surface of the dried silicon wafer. Tearing off the Sigao adhesive tape, separating the spin-coated propylene carbonate adhesive and the highly oriented graphite flakes on the silicon wafer along with the adhesive tape, and forming a complex of highly oriented graphite and the propylene carbonate adhesive in the square hole area.
And (3) placing the adhesive tape adhered with the highly oriented graphite and the propylene carbonate adhesive compound on a probe station support, wherein the hole part is suspended in the middle, and the highly oriented graphite is positioned at the upper end of the propylene carbonate adhesive.
Specifically, the probe station includes: the system comprises a computer, a temperature-adjusting four-dimensional micro-operation platform, an optical microscope, a charge coupling element, a probe clamp and an optical shock absorption table; the method is characterized in that: a temperature-adjusting four-dimensional micro-operation platform is fixed on the optical shock absorption platform, is a moving part of the probe platform and comprises translation in three directions and rotation in the horizontal direction; an optical microscope equipped with a charge-coupled device is vertically arranged right above the four-dimensional micro-operation platform, the charge-coupled device is connected with a computer, and a probe clamp is fixed on a rigid structure area on an optical shock absorption platform.
Rigidly fixing a support of the Sichuang adhesive tape on a probe clamp, selecting a common probe, adhering the reverse side on a silicon wafer, a quartz plate or a glass slide substrate by using silver adhesive, enabling the probe tip to face upwards, and placing the whole probe on a temperature-regulating four-dimensional micro-operation platform and fixing the whole probe by using the silver adhesive.
Wherein, the common probe is a finished probe with a needle tip; or a common probe or a finished probe coated with a metal coating.
Aligning the highly oriented graphite with the tip of a common probe, adjusting the initial temperature to 55 ℃, gradually adjusting the movement of the platform in the vertical direction until the highly oriented graphite sheet is contacted with and wrapped by the tip of the probe, raising the temperature to 120 ℃, waiting for 20-30min, melting the propylene carbonate adhesive, separating the propylene carbonate adhesive from the Sigao adhesive tape, and cooling to normal temperature.
The alignment of the highly oriented graphite with the tip of a common probe is as follows: aligning the highly oriented graphite on the probe clamp with the common probe tip on the temperature-regulating four-dimensional micro-operation platform by using a microscope image and a photo collected by a computer.
And (3) carrying out vacuum annealing and glue removal on the probe coated with the highly oriented graphite sheet by using a vacuum annealing device, wherein the vacuum degree is 10-5Pa, the temperature is 380 ℃, and the operation lasts for 30min, so that the final product of the atomic force microscope probe coated with the highly oriented graphite (wherein, the probe is also called multi-layer graphene when the number of layers is very large) can be obtained.
The vacuum annealing device used in the method for preparing the two-dimensional material modified probe tip is a finished product high-temperature tube furnace, the target temperature and the time required for reaching the target temperature are set, the temperature reaches 1200 ℃, and a mechanical pump and a molecular pump are arranged to reduce the air pressure to 10 DEG-5Pa。
The series of characterizations of this example is shown in fig. 2, which is a characterization of an atomic force microscope probe that has been covered with multi-layer graphene: wherein (a) and (b) represent optical microscope characterization and scanning electron microscope characterization of the multilayer graphene probe respectively; (c) represented is a schematic representation of a corresponding multi-layer graphene probe; (d) raman spectral characterization of multilayer graphene attached to the surface of the probe tip is shown.
Example 2:
selecting boron nitride with the size of 2mm multiplied by 2mm, placing the boron nitride on the adhesive surface of the Sichuan adhesive tape with the length of about 10cm, and mechanically stripping the boron nitride; and the mechanical stripping of the boron nitride is to place the boron nitride on the adhesion surface of the SiGeh adhesive tape, fold the SiGeh adhesive tape for 10 to 20 times to form a boron nitride distribution area of the adhesion surface of the adhesive tape, wherein the thickness of the oxide layer on the surface of the silicon wafer is 300 nm.
And adhering the boron nitride distribution area of the adhesive tape adhesion surface to an oxide layer on the surface of the silicon wafer, and increasing the contact pressure to ensure that boron nitride remains on the surface of the oxide layer of the silicon wafer, wherein the thickness of the silicon wafer of the boron nitride is below 30 nm. The silicon wafer for selecting the boron nitride with the thickness of less than 30nm further comprises:
placing the silicon wafer distributed with boron nitride under an optical microscope, and selecting the boron nitride wafer with the thickness close to 30nm according to different optical contrasts of different boron nitrides on an oxide layer of the silicon wafer;
and (3) placing the boron nitride with the thickness below 30nm under an atomic force microscope to characterize the accurate thickness of the boron nitride, and selecting the boron nitride with the thickness below 30 nm.
And placing the selected boron nitride silicon wafer with the thickness of less than 30nm on a spin-coating table, spin-coating the propylene carbonate adhesive, and drying. Specifically, a silicon wafer of the multilayer graphene sheet is placed on a spin-coating platform, propylene carbonate glue with the mass fraction of 14% is spin-coated at normal temperature, the propylene carbonate glue solvent is anisole, the spin-coating parameter is 500r/min and lasts for 20s, and the spin-coating parameter is 1750r/s and lasts for 40 s;
and (3) drying the silicon wafer subjected to spin coating for 5min on a heating table at 95 ℃.
And cutting a section of Sigao adhesive tape again, marking a square hole with the diameter of 3-6 mm, and adhering the square hole on the surface of the dried silicon wafer. Tearing off the Sigao adhesive tape, separating the spin-coated propylene carbonate adhesive and the boron nitride sheet on the silicon wafer along with the adhesive tape, and forming a complex of boron nitride and the propylene carbonate adhesive in the square hole area.
And placing the adhesive tape adhered with the boron nitride and propylene carbonate adhesive compound on a probe station support, wherein the hole part is suspended in the middle, and the boron nitride is positioned at the upper end of the propylene carbonate adhesive.
Specifically, the probe station includes: the system comprises a computer, a temperature-adjusting four-dimensional micro-operation platform, an optical microscope, a charge coupling element, a probe clamp and an optical shock absorption table; the method is characterized in that: a temperature-adjusting four-dimensional micro-operation platform is fixed on the optical shock absorption platform, is a moving part of the probe platform and comprises translation in three directions and rotation in the horizontal direction; an optical microscope equipped with a charge-coupled device is vertically arranged right above the four-dimensional micro-operation platform, the charge-coupled device is connected with a computer, and a probe clamp is fixed on a rigid structure area on an optical shock absorption platform.
Rigidly fixing a support of the Sichuang adhesive tape on a probe clamp, selecting a common probe, adhering the reverse side on a silicon wafer, a quartz plate or a glass slide substrate by using silver adhesive, enabling the probe tip to face upwards, and placing the whole probe on a temperature-regulating four-dimensional micro-operation platform and fixing the whole probe by using the silver adhesive.
Wherein, the common probe is a finished probe with a needle tip; or a common probe or a finished probe coated with a metal coating.
Aligning boron nitride with the tip of a common probe, adjusting the initial temperature to 55 ℃, gradually adjusting the movement of the platform in the vertical direction until the boron nitride sheet is contacted with and wrapped by the probe tip, raising the temperature to 120 ℃, waiting for 20-30min, melting the propylene carbonate adhesive, separating the propylene carbonate adhesive from the Sigao adhesive tape, and cooling to the normal temperature.
The alignment of boron nitride with a common probe tip is: aligning the boron nitride on the probe clamp with the common probe tip on the temperature-regulating four-dimensional micro-operation platform by using a microscope image and a photo collected by a computer.
The probe coated with the boron nitride sheet is subjected to vacuum annealing and glue removal by using a vacuum annealing device, wherein the vacuum degree is 10-5Pa, at 380 deg.C for 30min to obtain the final product coated with boron nitride atomic force microscope probe.
The vacuum annealing device used in the method for preparing the two-dimensional material modified probe tip is a finished product high-temperature tube furnace, the target temperature and the time required for reaching the target temperature are set, the temperature reaches 1200 ℃, and a mechanical pump and a molecular pump are arranged to reduce the air pressure to 10 DEG-5Pa。
Example 3:
selecting molybdenum disulfide with the size of 2mm multiplied by 2mm, placing the molybdenum disulfide on the adhesive surface of the Sichuan adhesive tape with the length of about 10cm, and mechanically stripping the molybdenum disulfide; the mechanical stripping of the molybdenum disulfide is to place the molybdenum disulfide on the adhesion surface of the SiGao adhesive tape, fold the SiGao adhesive tape for 10 to 20 times to form a molybdenum disulfide distribution area on the adhesion surface of the adhesive tape, and the thickness of the oxidation layer on the surface of the silicon wafer is 300 nm.
And adhering the molybdenum disulfide distribution area on the adhesive surface of the adhesive tape to an oxide layer on the surface of the silicon wafer, and increasing the contact pressure to ensure that molybdenum disulfide remains on the surface of the oxide layer of the silicon wafer, wherein the thickness of the molybdenum disulfide silicon wafer is less than 30 nm. The silicon wafer for selecting the molybdenum disulfide with the thickness of less than 30nm further comprises:
placing the silicon wafer distributed with molybdenum disulfide under an optical microscope, and selecting molybdenum disulfide pieces close to 30nm according to different optical contrasts of different molybdenum disulfide on an oxide layer of the silicon wafer;
and (3) placing the molybdenum disulfide with the thickness below 30nm under an atomic force microscope to characterize the accurate thickness of the molybdenum disulfide, and selecting the molybdenum disulfide with the thickness below 30 nm.
And placing the selected silicon wafer of the molybdenum disulfide with the thickness of less than 30nm on a spin-coating table, spin-coating the propylene carbonate adhesive, and drying. Specifically, a silicon wafer of the multilayer graphene sheet is placed on a spin-coating platform, propylene carbonate glue with the mass fraction of 14% is spin-coated at normal temperature, the propylene carbonate glue solvent is anisole, the spin-coating parameter is 500r/min and lasts for 20s, and the spin-coating parameter is 1750r/s and lasts for 40 s;
and (3) drying the silicon wafer subjected to spin coating for 5min on a heating table at 95 ℃.
And cutting a section of Sigao adhesive tape again, marking a square hole with the diameter of 3-6 mm, and adhering the square hole on the surface of the dried silicon wafer. Tearing off the Sigao adhesive tape, separating the spin-coated propylene carbonate adhesive and the molybdenum disulfide sheet on the silicon wafer along with the adhesive tape, and forming a complex of molybdenum disulfide and the propylene carbonate adhesive in the square hole area.
And placing the adhesive tape adhered with the molybdenum disulfide and the propylene carbonate adhesive compound on a probe stand support, wherein the hole part is suspended in the middle, and the molybdenum disulfide is positioned at the upper end of the propylene carbonate adhesive.
Specifically, the probe station includes: the system comprises a computer, a temperature-adjusting four-dimensional micro-operation platform, an optical microscope, a charge coupling element, a probe clamp and an optical shock absorption table; the method is characterized in that: a temperature-adjusting four-dimensional micro-operation platform is fixed on the optical shock absorption platform, is a moving part of the probe platform and comprises translation in three directions and rotation in the horizontal direction; an optical microscope equipped with a charge-coupled device is vertically arranged right above the four-dimensional micro-operation platform, the charge-coupled device is connected with a computer, and a probe clamp is fixed on a rigid structure area on an optical shock absorption platform.
Rigidly fixing a support of the Sichuang adhesive tape on a probe clamp, selecting a common probe, adhering the reverse side on a silicon wafer, a quartz plate or a glass slide substrate by using silver adhesive, enabling the probe tip to face upwards, and placing the whole probe on a temperature-regulating four-dimensional micro-operation platform and fixing the whole probe by using the silver adhesive.
Wherein, the common probe is a finished probe with a needle tip; or a common probe or a finished probe coated with a metal coating.
Aligning molybdenum disulfide with the tip of a common probe, adjusting the initial temperature to 55 ℃, gradually adjusting the movement of the platform in the vertical direction until a molybdenum disulfide sheet is contacted with and wrapped on the tip of the probe, raising the temperature to 120 ℃, waiting for 20-30min, melting and separating the propylene carbonate adhesive from the Sigao adhesive tape, and cooling to the normal temperature.
The alignment of the molybdenum disulfide with the tip of a common probe is as follows: aligning the molybdenum disulfide on the probe clamp with the common probe tip on the temperature-regulating four-dimensional micro-operation platform by using a microscope image and a photo collected by a computer.
The probe coated with the molybdenum disulfide sheet is subjected to vacuum annealing and glue removal by using a vacuum annealing device, wherein the vacuum degree is 10-5Pa, the temperature is 380 ℃, and the reaction lasts for 30min, thus obtaining the final product of the atomic force microscope probe coated with molybdenum disulfide.
The vacuum annealing device used in the method for preparing the two-dimensional material modified probe tip is a finished product high-temperature tube furnace, the target temperature and the time required for reaching the target temperature are set, the temperature reaches 1200 ℃, and a mechanical pump and a molecular pump are arranged to reduce the air pressure to 10 DEG-5Pa。
The atomic force microscope probe coated with the two-dimensional material can be stably adhered to a needle tip in air or vacuum at 500 ℃, and can be applied to an atomic force microscope in air and vacuum to obtain various atomic force microscope images; the method can be applied to the surface property research of two-dimensional plane materials, especially the mechanical properties such as adhesion and friction between two-dimensional materials, and can conveniently research the special properties of a large quantity of low-dimensional materials; and the manufacturing process is mature and simple, and the method is suitable for manufacturing the two-dimensional material modified probe tip in laboratories and industrialized application.
The embodiments in the present specification are described in a progressive manner, and the same and similar parts among the embodiments are referred to each other, and each embodiment focuses on the differences from the other embodiments. In particular, for the apparatus embodiment, since it is substantially similar to the method embodiment, it is relatively simple to describe, and reference may be made to some descriptions of the method embodiment for relevant points.
The above description is only for the specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (7)
1. A preparation method of an atomic force microscope probe wrapping a two-dimensional material is characterized by comprising the following steps:
s01, placing the two-dimensional material on the adhesive surface of the Siji adhesive tape, folding the Siji adhesive tape for 10 to 20 times to form two-dimensional material distribution of the adhesive surface of the adhesive tape;
s02, adhering the adhesive surface of the adhesive tape to the oxide layer on the surface of the silicon wafer, and increasing the contact pressure to ensure that two-dimensional materials remain on the surface of the oxide layer of the silicon wafer, wherein the silicon wafer is made of two-dimensional materials with the thickness of less than 30 nm;
s03, placing the selected silicon wafer of the two-dimensional material with the thickness of less than 30nm on a spin-coating table, spin-coating the propylene carbonate glue, and drying;
s04, cutting a section of Siji tape again, marking a square hole of 3-6 mm, adhering the square hole on the surface of the dried silicon wafer, tearing off the Siji tape, separating the spin-coated propylene carbonate adhesive and the two-dimensional material sheet on the silicon wafer along with the tape, and forming a complex of the two-dimensional material and the propylene carbonate adhesive in the area of the square hole;
s05, placing the adhesive tape adhered with the two-dimensional material and the propylene carbonate glue complex on a probe station support, suspending the hole part in the middle, and positioning the two-dimensional material at the upper end of the propylene carbonate glue;
s06, rigidly fixing the support of the Sigao tape on a probe clamp, selecting a common probe, adhering the back surface on a silicon wafer, a quartz plate or a glass slide substrate by using silver adhesive, enabling the probe tip to face upwards, placing the whole probe on a temperature-regulating four-dimensional micro-operation platform and fixing the whole probe by using the silver adhesive;
s07, aligning the two-dimensional material with the tip of a common probe, adjusting the initial temperature to 55 ℃, gradually adjusting the movement of the platform in the vertical direction until the two-dimensional material sheet is contacted with and wrapped by the tip of the probe, raising the temperature to 120 ℃, waiting for 20-30min, melting the propylene carbonate adhesive, separating from the Sigao tape, and cooling to normal temperature;
s08, performing vacuum annealing and glue removal on the probe coated with the two-dimensional material sheet by using a vacuum annealing device, wherein the vacuum degree is 10-5Pa, at 380 ℃ for 30 min.
2. The method for preparing the atomic force microscope probe wrapped by the two-dimensional material according to claim 1, wherein the method comprises the following steps:
the thickness of the oxide layer on the surface of the silicon wafer is 300 nm.
3. The method for preparing the atomic force microscope probe wrapped by the two-dimensional material according to claim 1, wherein the selecting the silicon wafer of the two-dimensional material with the thickness of 30nm or less further comprises:
placing the silicon wafer distributed with the two-dimensional material under an optical microscope, and selecting a two-dimensional material sheet with the thickness close to 30nm according to different optical contrasts of different two-dimensional materials on an oxide layer of the silicon wafer;
and (3) placing the two-dimensional material with the thickness of below 30nm under an atomic force microscope to characterize the accurate thickness of the two-dimensional material, and selecting the two-dimensional material with the thickness of below 30 nm.
4. The method for preparing the atomic force microscope probe wrapping a two-dimensional material according to claim 1, wherein the spin coating of the propylene carbonate adhesive in the step S03 is followed by drying, and the method comprises:
carrying out spin coating on 14% propylene carbonate glue by mass, wherein a propylene carbonate glue solvent is anisole, and spin coating parameters are 500r/min for 20s and 1750r/s for 40 s;
and (3) drying the silicon wafer subjected to spin coating for 5min on a heating table at 95 ℃.
5. The method for preparing the AFM probe as claimed in claim 1, wherein the probe stage of step S05 comprises: the system comprises a computer, a temperature-adjusting four-dimensional micro-operation platform, an optical microscope, a charge coupling element, a probe clamp and an optical shock absorption table; the method is characterized in that: a temperature-adjusting four-dimensional micro-operation platform is fixed on the optical shock absorption platform, is a moving part of the probe platform and comprises translation in three directions and rotation in the horizontal direction; an optical microscope equipped with a charge-coupled device is vertically arranged right above the four-dimensional micro-operation platform, the charge-coupled device is connected with a computer, and a probe clamp is fixed on a rigid structure area on an optical shock absorption platform.
6. The method for preparing the AFM probe wrapping the two-dimensional material as claimed in claim 1, wherein the step S07 for aligning the two-dimensional material with the tip of the ordinary probe is: and aligning a target two-dimensional material sheet on the probe clamp with a common probe tip on the temperature-regulating four-dimensional micro-operation platform by using a microscope image and a photo acquired by a computer.
7. The method for preparing the AFM probe coated with two-dimensional material as claimed in claim 1, wherein the vacuum annealing device of step S08 is a high temperature tube furnace, the target temperature and the time required to reach the target temperature are set at 1200 ℃, and a mechanical pump and a molecular pump are provided to reduce the pressure to 10 ℃-5Pa。
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| CN108845161B (en) * | 2018-03-21 | 2020-05-12 | 深圳清力技术有限公司 | Atomic force microscope probe, atomic force microscope and probe preparation method |
| CN109030870B (en) * | 2018-07-19 | 2019-10-25 | 清华大学 | Two-dimensional layer material wraps up atomic force microscope probe and preparation method thereof and application |
| CN110117780B (en) * | 2019-03-19 | 2021-03-12 | 中国科学院上海微系统与信息技术研究所 | Two-dimensional material layer and preparation method thereof |
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