CN110542768A - method for processing micro-cantilever probe for measuring ultralow friction coefficient - Google Patents
method for processing micro-cantilever probe for measuring ultralow friction coefficient Download PDFInfo
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- CN110542768A CN110542768A CN201910724255.5A CN201910724255A CN110542768A CN 110542768 A CN110542768 A CN 110542768A CN 201910724255 A CN201910724255 A CN 201910724255A CN 110542768 A CN110542768 A CN 110542768A
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- cantilever
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
- G01Q60/00—Particular types of SPM [Scanning Probe Microscopy] or microscopes; Essential components thereof
- G01Q60/24—AFM [Atomic Force Microscopy] or apparatus therefor, e.g. AFM probes
- G01Q60/26—Friction force microscopy
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
- G01Q60/00—Particular types of SPM [Scanning Probe Microscopy] or microscopes; Essential components thereof
- G01Q60/24—AFM [Atomic Force Microscopy] or apparatus therefor, e.g. AFM probes
- G01Q60/38—Probes, their manufacture, or their related instrumentation, e.g. holders
Abstract
The invention relates to the technical field of atomic force microscope probes, and provides a method for processing a micro-cantilever probe for measuring an ultralow friction coefficient, which comprises the following steps of 1: establishing a model for measuring the friction coefficient by using a micro-cantilever probe; according to the measuring principle of an atomic force microscope, expressions for measuring friction force and positive pressure are respectively established through the torsion and the bending of a probe; establishing a model for measuring the friction coefficient of the probe by the expression in a simultaneous manner; step 2: determining the size parameters, length l, width w, thickness t and the like of the micro-cantilever probe according to the model; and step 3: and (4) processing the probe. Therefore, the invention establishes a model of the micro-cantilever probe for measuring the friction coefficient, determines the size parameter of the micro-cantilever probe according to the model, and then processes and manufactures the probe. The invention establishes a model for measuring the friction coefficient by the micro-cantilever probe and realizes the processing and the manufacturing of the probe by utilizing the high-precision optical imaging system and the high-precision motion control system of the existing atomic force microscope.
Description
Technical Field
the invention belongs to the technical field of atomic force microscope probes, and particularly relates to a method for processing a micro-cantilever probe for measuring an ultralow friction coefficient.
background
atomic Force Microscopy (AFM), has been widely used in a variety of scientific fields as well as in the industrial fields of semiconductors, integrated circuits, and the like.
In particular, with the development of micron-nanometer scientific technology, especially atomic force microscopy, atomic force microscopy plays an increasingly important role in the observation and imaging of microstructures, the characterization of microstructures, and the detection of physical and chemical properties of a sample to be tested, such as optothermal electroacoustics.
One of the key components of AFM to achieve high resolution detection is the probe. In the testing process, the probe tip contacts the surface of a sample to generate an interaction force, so that the probe micro-cantilever is bent, and various information is obtained by detecting the bending size of the micro-cantilever. However, the contact surface of the existing atomic force microscope probe and the tested sample is a non-plane surface, and the actual value and the nominal value of the curvature radius of the contact surface have deviation, so that various properties of the tested sample cannot be accurately tested, and the development of the atomic force microscope is severely limited.
in view of the above, the prior art is obviously inconvenient and disadvantageous in practical use, and needs to be improved.
disclosure of Invention
in view of the above-mentioned drawbacks, an object of the present invention is to provide a method for processing a micro-cantilever probe with ultra-low friction coefficient, which includes establishing a model of the micro-cantilever probe for measuring friction coefficient, determining a dimensional parameter of the micro-cantilever probe according to the model, and processing and manufacturing the probe. The invention establishes a model for measuring the friction coefficient by the micro-cantilever probe and realizes the processing and the manufacturing of the probe by utilizing the high-precision optical imaging system and the high-precision motion control system of the existing atomic force microscope.
in order to achieve the above object, the present invention provides a method for processing a micro-cantilever probe for ultra-low friction coefficient measurement, comprising the following steps:
Step 1: model for establishing micro-cantilever probe to measure friction coefficient
According to the measuring principle of an atomic force microscope, expressions for measuring friction force and positive pressure are respectively established through the torsion and the bending of a probe;
establishing a model for measuring the friction coefficient of the probe by the expression in a simultaneous manner;
step 2: determining the dimensional parameters of the microcantilever probe according to the model
calculating and determining the size of the micro-cantilever probe by using the model established in the step 1 according to the friction coefficient mu resolution mu minn and the constraint conditions of the maximum positive pressure FNmax or the minimum friction FLmin and the characteristics of the atomic force microscope;
the micro-cantilever probe has the dimensions of length l, width w and thickness t;
and step 3: machining probe
and (3) processing the micro-cantilever probe according to the size determined in the step (2), wherein the processing comprises the following steps:
S1, selecting a commercial microcantilever probe with a needle tip, and cutting the sharp front end of the needle tip into a platform with the width of 1-1.5 microns through a focused ion beam flight time secondary ion mass spectrometer to prepare a probe sample for later use;
S2, placing the microspherical particles for preparing the probe tips into an acetone or ethanol solution for ultrasonic cleaning, and sealing and storing the cleaned particles in a dispersion liquid for later use;
S3, placing the silicon wafer template marked with the position in acetone or isopropanol solution for ultrasonic cleaning, and blowing the silicon wafer template for standby after cleaning;
s4, taking a drop of ethanol or deionized water dispersion liquid containing microsphere particles, dropping the drop on the processed silicon wafer template marked with the position, and drying for later use;
The microsphere particles are silicon dioxide spheres or organic medicine particles; the diameter of the microspherical particle is 200-1000 nm.
s5, preparing an epoxy glue tablet; uniformly coating a layer of epoxy glue on a glass slide or a silicon wafer for later use;
S6, scanning and imaging the silicon wafer template prepared in the S4 by using an atomic force microscope to fully disperse particles, and recording the dispersed positions according to marks;
S7, replacing the probe of the atomic force microscope in S6 with the probe sample prepared in S1, and adjusting the position and the reflection value of the laser to ensure the effective needle inserting track of the atomic force microscope;
S8, fixing the prepared epoxy glue piece in the S5 on a sample table, adjusting the atomic force microscope to insert the probe in a contact mode, enabling the probe sample to contact the surface of the epoxy glue and stand for 30 seconds, and enabling the probe sample platform to be fully adhered with the epoxy glue and then withdraw the probe;
s9, replacing the epoxy glue film with the silicon wafer template prepared in S4, enabling the probe sample to be inserted to the position of the recorded particles in S6 again, and standing for 60 seconds to enable the microsphere particles to be bonded on the probe sample;
and S10, taking off the probe sample of S9, and obtaining the micro-cantilever probe after the epoxy glue is completely cured.
according to the method for processing the micro-cantilever probe for measuring the ultralow friction coefficient, the cross section of the micro-cantilever is set to be rectangular.
according to the processing method of the micro-cantilever probe for measuring the ultralow friction coefficient, the width w of the micro-cantilever probe is more than or equal to 20 microns, and the length l of the micro-cantilever probe is more than or equal to 50 microns.
according to the method for processing the micro-cantilever probe for measuring the ultralow friction coefficient, the material of the micro-cantilever probe is preferably silicon or silicon nitride.
According to the processing method of the micro-cantilever probe for measuring the ultralow friction coefficient, the thickness t of the silicon micro-cantilever probe is as follows: 1-7.8 μm.
according to the processing method of the micro-cantilever probe for measuring the ultralow friction coefficient, the thickness t of the silicon nitride micro-cantilever probe is as follows: 0.2-0.6 μm.
according to the processing method of the micro-cantilever probe for measuring the ultralow friction coefficient, the method for preparing the epoxy glue film by S5 in the step 3 comprises the following steps: and (3) dropping epoxy glue on the glass slide or the silicon chip cleaned by acetone or ethanol, uniformly stirring, and scraping redundant glue to obtain the epoxy glue chip.
according to the processing method of the micro-cantilever probe for measuring the ultralow friction coefficient, the two components of the epoxy glue are epoxy glue.
according to the processing method of the micro-cantilever probe for measuring the ultralow friction coefficient, the curing time of the epoxy glue is not less than 30 min.
The invention aims to provide a method for processing a micro-cantilever probe for measuring an ultralow friction coefficient. The invention establishes a model for measuring the friction coefficient by the micro-cantilever probe and realizes the processing and the manufacturing of the probe by utilizing the high-precision optical imaging system and the high-precision motion control system of the existing atomic force microscope.
Detailed Description
in order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
the invention provides a method for processing a micro-cantilever probe for measuring an ultralow friction coefficient, which comprises the following steps:
Step 1: model for establishing micro-cantilever probe to measure friction coefficient
according to the measuring principle of an atomic force microscope, expressions for measuring friction force and positive pressure are respectively established through the torsion and the bending of a probe;
Establishing a model for measuring the friction coefficient of the probe by the expression in a simultaneous manner;
step 2: determining the dimensional parameters of the microcantilever probe according to the model
calculating and determining the size of the micro-cantilever probe by using the model established in the step 1 according to the friction coefficient mu resolution mu minn and the constraint conditions of the maximum positive pressure FNmax or the minimum friction FLmin and the characteristics of the atomic force microscope;
The micro-cantilever probe has the dimensions of length l, width w and thickness t;
And step 3: machining probe
and (3) processing the micro-cantilever probe according to the size determined in the step (2), wherein the processing comprises the following steps:
s1, selecting a commercial microcantilever probe with a needle tip, and cutting the sharp front end of the needle tip into a platform with the width of 1-1.5 microns through a focused ion beam flight time secondary ion mass spectrometer to prepare a probe sample for later use;
S2, placing the microspherical particles for preparing the probe tips into an acetone or ethanol solution for ultrasonic cleaning, and sealing and storing the cleaned particles in a dispersion liquid for later use;
S3, placing the silicon wafer template marked with the position in acetone or isopropanol solution for ultrasonic cleaning, and blowing the silicon wafer template for standby after cleaning;
S4, taking a drop of ethanol or deionized water dispersion liquid containing microsphere particles, dropping the drop on the processed silicon wafer template marked with the position, and drying for later use;
The microsphere particles are silicon dioxide spheres or organic medicine particles; the diameter of the microspherical particle is 200-1000 nm.
S5, preparing an epoxy glue tablet; uniformly coating a layer of epoxy glue on a glass slide or a silicon wafer for later use;
S6, scanning and imaging the silicon wafer template prepared in the S4 by using an atomic force microscope to fully disperse particles, and recording the dispersed positions according to marks;
S7, replacing the probe of the atomic force microscope in S6 with the probe sample prepared in S1, and adjusting the position and the reflection value of the laser to ensure the effective needle inserting track of the atomic force microscope;
S8, fixing the prepared epoxy glue piece in the S5 on a sample table, adjusting the atomic force microscope to insert the probe in a contact mode, enabling the probe sample to contact the surface of the epoxy glue and stand for 30 seconds, and enabling the probe sample platform to be fully adhered with the epoxy glue and then withdraw the probe;
S9, replacing the epoxy glue film with the silicon wafer template prepared in S4, enabling the probe sample to be inserted to the position of the recorded particles in S6 again, and standing for 60 seconds to enable the microsphere particles to be bonded on the probe sample;
and S10, taking off the probe sample of S9, and obtaining the micro-cantilever probe after the epoxy glue is completely cured.
specifically, step 1: model for establishing micro-cantilever probe to measure friction coefficient
According to the measuring principle of atomic force microscope, the friction force and the positive pressure are respectively measured by the torsion and the bending of the micro-cantilever probe, namely
F＝K×InvOLS×U (i)
F＝K×InvOLS×U (ii)
(i) In the formulae (I) and (ii),
FL is friction; FN is positive pressure;
KT is the torsional elasticity coefficient of the micro-cantilever probe; KN is the normal elastic coefficient;
InvOLSL is the inverse of the lateral optical lever sensitivity; InvOLSN is the inverse of the normal optical lever sensitivity;
UL is the lateral output voltage of the photodetector; UN is the normal output voltage;
further establishing a common expression of the friction coefficient measured by the micro-cantilever probe:
Wherein μ is a friction coefficient; the formula is a model for measuring the friction coefficient by the probe.
Preferably, the cross-sectional shape of the micro-cantilever is set to be rectangular
according to the measurement principle of the optical path system, expressions of the inverse number InvOLSL of the lateral optical lever sensitivity and the inverse number InvOLSN of the normal optical lever sensitivity are respectively established as follows:
in the formula, H is the length of a photosensitive surface of the photoelectric detector, d is the length of a light path, L is the length of a micro-cantilever beam, Usum is the total voltage generated by laser in four quadrants of the photoelectric detector, and alpha sum, alpha L and alpha N are the amplification times of the total output current, the transverse output current and the normal output current of the photoelectric detector after passing through a current/voltage converter respectively, and the unit is V/A;
furthermore, the cross section of the micro-cantilever beam is a long and narrow rectangle, namely the width is far larger than the thickness; based on the sheet elasticity mechanics and material mechanics theory, the expressions of the torsional elastic coefficient KT and the normal elastic coefficient KN of the micro-cantilever beam probe are established as follows:
in the formula, G, E is the shear modulus and the elastic modulus of the micro-cantilever beam material respectively, w and t are the width and the thickness of the micro-cantilever beam respectively, and htip is the height of the needle tip;
Substituting the formulas (iv) to (vii) into the general expression (iii) of the friction coefficient measured by the general micro-cantilever probe in the step 1 to obtain a model of the friction coefficient measured by the rectangular micro-cantilever probe, wherein the model is as follows:
IN the formula, IL is the lateral output current of the photodetector, IL is UL/α L, IN is the normal output current of the photodetector, and IN is UN/α N;
step 2: determining the dimensional parameters of the microcantilever probe according to the model
the mu is a friction coefficient resolution ratio mu min, FN is a loadable maximum positive pressure FNmax or FL is a measurable minimum friction force FLmin, and the dimensions of the micro-cantilever beam probe meeting the measurement requirements, including the length l, the width w, the thickness t and the like, are determined through simultaneous (i) to (viii) calculation by combining constraint conditions such as the maximum positive pressure FNmax or the measurable minimum friction force FLmin and the characteristics of an atomic force microscope;
the width w of the micro-cantilever probe is more than or equal to 20 microns, and the length l of the micro-cantilever probe is more than or equal to 50 microns;
The material of the micro-cantilever probe is preferably silicon or silicon nitride;
the thickness t of the silicon micro-cantilever probe is as follows: 1-7.8 μm; the thickness t of the silicon nitride micro-cantilever probe is as follows: 0.2-0.6 μm;
and step 3: machining probe
and (3) processing the micro-cantilever probe according to the size determined in the step (2), wherein the processing comprises the following steps:
s1, selecting a commercial microcantilever probe with a needle tip, and cutting the sharp front end of the needle tip into a platform with the width of 1-1.5 microns through a focused ion beam flight time secondary ion mass spectrometer to prepare a probe sample for later use;
s2, placing the microspherical particles for preparing the probe tips into an acetone or ethanol solution for ultrasonic cleaning, and sealing and storing the cleaned particles in a dispersion liquid for later use;
the dispersion is preferably ethanol or water.
and S3, placing the silicon wafer template marked with the position in acetone or isopropanol solution for ultrasonic cleaning, and drying for later use after cleaning.
The silicon wafer template is dried by adopting pure nitrogen after being cleaned.
s4, taking a drop of ethanol or deionized water dispersion liquid containing microsphere particles, dropping the drop on the processed silicon wafer template marked with the position, and drying for later use;
The microsphere particles are silicon dioxide spheres or organic medicine particles; the diameter of the microspherical particle is 200-1000 nm.
S5, preparing an epoxy glue tablet; uniformly coating a layer of epoxy glue on a glass slide or a silicon wafer for later use;
during preparation, epoxy glue is dropped on a glass slide or a silicon wafer cleaned by acetone or ethanol, after the epoxy glue is uniformly stirred, the side surface of the other cleaned glass slide is used for forcibly scraping redundant glue for many times, and a spin coater can also be used for spin coating at high speed to ensure that the glue on the glass slide or the silicon wafer is as thin as possible.
the double-component epoxy glue is preferably selected, and the curing time is more than 30 min.
S6, scanning and imaging the silicon wafer template prepared in the S4 by using an atomic force microscope to fully disperse particles, and recording the dispersed positions according to marks;
and (3) sequentially opening a controller and supporting software (with high-precision optical and position control accessories, such as Bruker division Icon) of the atomic force microscope, selecting a commercial sharp probe (with the curvature radius of about 2-50 nm), scanning and imaging the silicon wafer template marked with the position prepared in the step S4 to obtain the position with good particle dispersibility, and recording the position according to the mark (the position among the particles is far enough to avoid mutual influence when the particles are adhered to the probe).
S7, replacing the probe of the atomic force microscope in S6 with the probe sample prepared in S1, and adjusting the position and the reflection value of the laser to ensure the effective needle inserting track of the atomic force microscope;
S8, fixing the prepared epoxy glue piece in the S5 on a sample table, adjusting the atomic force microscope to insert the probe in a contact mode, enabling the probe sample to contact the surface of the epoxy glue and stand for 30 seconds, and enabling the probe sample platform to be fully adhered with the epoxy glue and then withdraw the probe;
fixing a glass slide or a silicon wafer with an epoxy glue layer on a sample platform, moving the glass slide or the silicon wafer to a relatively thin area of the epoxy glue layer by using a high-resolution optical microscope and a position control system which are carried by the instrument, adjusting the automatic needle insertion under the contact mode of the atomic force microscope, standing for 30 seconds after a probe is contacted with the surface of the epoxy glue, fully sticking the epoxy glue on the platform obtained in step 1, and then automatically withdrawing the needle.
S9, replacing the epoxy glue film with the silicon wafer template prepared in S4, enabling the probe sample to be inserted to the position of the recorded particles in S6 again, and standing for 60 seconds to enable the microsphere particles to be bonded on the probe sample;
And replacing the glass slide or the silicon wafer with the epoxy glue water layer with the silicon wafer template which is prepared in S4 and is dispersed with the microsphere particles and marked with the positions, searching the positions of the microsphere particles recorded in the step 6 by using a high-resolution optical microscope and a position control system which are arranged on the instrument, accurately positioning the needle, and standing for 60 seconds after the probe is contacted with the surface of the epoxy glue to ensure that the microsphere particles can be bonded on the probe.
And S10, taking off the probe sample of S9, and placing the probe sample in a clean environment for 24 hours to completely cure the epoxy glue to obtain the probe.
In summary, the present invention provides a method for processing a micro-cantilever probe with an ultra-low friction coefficient, which comprises establishing a model of the micro-cantilever probe for measuring the friction coefficient, determining the dimensional parameters of the micro-cantilever probe according to the model, and processing and manufacturing the probe. The invention establishes a model for measuring the friction coefficient by the micro-cantilever probe and realizes the processing and the manufacturing of the probe by utilizing the high-precision optical imaging system and the high-precision motion control system of the existing atomic force microscope.
The present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof, and it should be understood that various changes and modifications can be effected therein by one skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (9)
1. A method for processing a micro-cantilever probe for measuring ultralow friction coefficient is characterized by comprising the following steps:
step 1: model for establishing micro-cantilever probe to measure friction coefficient
According to the measuring principle of an atomic force microscope, expressions for measuring friction force and positive pressure are respectively established through the torsion and the bending of a probe;
Establishing a model for measuring the friction coefficient of the probe by the expression in a simultaneous manner;
step 2: determining the dimensional parameters of the microcantilever probe according to the model
calculating and determining the size of the micro-cantilever probe by using the model established in the step 1 according to the friction coefficient mu resolution mu minn and the constraint conditions of the maximum positive pressure FNmax or the minimum friction FLmin and the characteristics of the atomic force microscope;
The micro-cantilever probe has the dimensions of length l, width w and thickness t;
And step 3: machining probe
And (3) processing the micro-cantilever probe according to the size determined in the step (2), wherein the processing comprises the following steps:
S1, selecting a commercial microcantilever probe with a needle tip, and cutting the sharp front end of the needle tip into a platform with the width of 1-1.5 microns through a focused ion beam flight time secondary ion mass spectrometer to prepare a probe sample for later use;
s2, placing the microspherical particles for preparing the probe tips into an acetone or ethanol solution for ultrasonic cleaning, and sealing and storing the cleaned particles in a dispersion liquid for later use;
s3, placing the silicon wafer template marked with the position in acetone or isopropanol solution for ultrasonic cleaning, and blowing the silicon wafer template for standby after cleaning;
S4, taking a drop of ethanol or deionized water dispersion liquid containing microsphere particles, dropping the drop on the processed silicon wafer template marked with the position, and drying for later use;
The microsphere particles are silicon dioxide spheres or organic medicine particles; the diameter of the microspherical particle is 200-1000 nm.
S5, preparing an epoxy glue tablet; uniformly coating a layer of epoxy glue on a glass slide or a silicon wafer for later use;
S6, scanning and imaging the silicon wafer template prepared in the S4 by using an atomic force microscope to fully disperse particles, and recording the dispersed positions according to marks;
S7, replacing the probe of the atomic force microscope in S6 with the probe sample prepared in S1, and adjusting the position and the reflection value of the laser to ensure the effective needle inserting track of the atomic force microscope;
S8, fixing the prepared epoxy glue piece in the S5 on a sample table, adjusting the atomic force microscope to insert the probe in a contact mode, enabling the probe sample to contact the surface of the epoxy glue and stand for 30 seconds, and enabling the probe sample platform to be fully adhered with the epoxy glue and then withdraw the probe;
S9, replacing the epoxy glue film with the silicon wafer template prepared in S4, enabling the probe sample to be inserted to the position of the recorded particles in S6 again, and standing for 60 seconds to enable the microsphere particles to be bonded on the probe sample;
and S10, taking off the probe sample of S9, and obtaining the micro-cantilever probe after the epoxy glue is completely cured.
2. the method as claimed in claim 1, wherein the micro-cantilever is rectangular in cross-section.
3. The method for processing the micro-cantilever probe for ultra-low friction coefficient measurement according to claim 2, wherein the width w of the micro-cantilever probe is greater than or equal to 20 μm, and the length l of the micro-cantilever probe is greater than or equal to 50 μm.
4. The method as claimed in claim 3, wherein the micro-cantilever probe is preferably made of silicon or silicon nitride.
5. the method for processing the micro-cantilever probe for ultra-low friction coefficient measurement according to claim 4, wherein the thickness t of the silicon micro-cantilever probe is: 1-7.8 μm.
6. The method for processing the micro-cantilever probe with ultra-low friction coefficient measurement according to claim 4, wherein the thickness t of the silicon nitride micro-cantilever probe is as follows: 0.2-0.6 μm.
7. the method for processing the micro-cantilever probe for measuring ultralow friction coefficient according to any one of claims 1 to 6, wherein the method for preparing the epoxy glue film at S5 in the step 3 comprises the following steps: and (3) dropping epoxy glue on the glass slide or the silicon chip cleaned by acetone or ethanol, uniformly stirring, and scraping redundant glue to obtain the epoxy glue chip.
8. the method of claim 7, wherein the epoxy glue is a two-component epoxy glue.
9. The method of claim 8, wherein the epoxy glue is cured for at least 30 min.
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