CN106526242A - AFM probe lateral force calibrating coefficient measurement method and lateral force calibrating method - Google Patents
AFM probe lateral force calibrating coefficient measurement method and lateral force calibrating method Download PDFInfo
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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]
- G01Q40/00—Calibration, e.g. of probes
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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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Abstract
The invention provides an AFM probe lateral force calibrating coefficient measurement method and a lateral force calibrating method, and belongs to the crossing field of nano-technology and nano-tribology. The measurement method is conducted in the environment condition of a standard laboratory. By means of an AFM, the friction electrical signal Uf and the surface adhesion Fad of a test specimen in the same region under the effects of different normal loads are measured. After that, the measured values are substituted into Uf beta = k (Fn + Fad). In this way, a lateral force calibrating coefficient beta is figured out through the optimal parameter estimation method, so that the calibrating process of the lateral force is realized. According to the technical scheme of the invention, the materials of the above method are optional, convenient to obtain, low in cost and free from being processed. Meanwhile, the above method is provided based on the law of Amontons, so that the influence of the adhesion on the calibration is fully considered. The calculation process is simple, quick and accurate, so that the method can be widely used for calibrating the lateral forces of various AFM probes and micro-cantilevers.
Description
Technical field
The invention discloses a kind of AFM probe cross force calibration coefficient measuring method and cross force scaling method, more specifically
It is a kind of side for measuring AFM probe cross force calibration coefficient based on Amontons (A Mengdong) law using frictional force device for measuring force
Method and AFM probe cross force scaling method.Belong to nanosecond science and technology and Nanotribology technology crossing domain.
Background technology
Past 20 years the insides, with the development of scanning probe microscopy, particularly atomic force microscope technology, to receive
The mechanical property of materials research of metrical scale brings great convenience.Bhushan of such as Ohio State University etc. utilizes AFM
(atomic force microscope) done the mechanics of series of experiment research nanometer sized materials, tribological property (Wear, 2005,259
(7):1507-1531), the AFM such as Wen Shizhu, Qian Linmao of domestic Tsing-Hua University's tribology National Key Laboratory has carried out various
Nano material friction and wear research (mechanical engineering journal, 2007,43 (10):7-8.).
AFM has a wide range of applications in Nanotribology and nanometer mechanics research, but due to atomic force microscope technology
The power problem of calibrating of limitation, particularly AFM probe so that the material mechanical or frictional behaviour ten of quantitative analyses nanoscale
Divide difficulty.Force curve of atomic force microscope causes photoelectric reactor on electricity using probe deformations back reflection laser with frictional force module
Pressure deflection relation come reaction material surface mechanical property (Surface science reports, 2005,59 (1):1-
152.), such as adhesive force, frictional force etc., and the voltage signal measured by AFM can not be converted directly into power by instrument, each spy
Pin could change after being required for demarcating the physical parameter of itself (Langmuir, 2006,22 (5):2340-2350.),
It is divided into normal force to demarcate and cross force demarcation.
In terms of atomic force microscope probe cross force demarcation, scholars propose some solutions, for example Australia
Wedges method that the Huabin Wang of University of Melbourne are proposed (Ultramicroscopy, 2014,136:193-200.) demarcate and visit
Pin cross force.But this method needs specially to process specific slope grating sample, whole test is very numerous and diverse with analysis process,
Demarcate inefficiency high cost；The two-step method that Hamburg, Germany university Applied Physics institute and Study on Microstructure center propose
(Review of scientific instruments,1996,67(7):2560-2567.) probe cross force is demarcated, by visiting
The geometric parameter and physical parameter of pin itself calculates complicated and calibrated error up to 30% to 50% calculating cross force, it is clear that
It is less accurate；The Yu Jiaxin and Qian Linmao of domestic Southwest Jiaotong University propose a kind of improved wedges method (tribology journal,
2007,27(5):472-476.), it is contemplated that trend of the calibration coefficient with load change, but there is no innovation substantially.
Therefore demarcate in the urgent need to introducing a kind of AFM probe cross force that calibration cost is cheap and efficiency and accuracy are higher
Method is meeting the mechanics and tribology research needs of nanoscale.
The content of the invention
It is an object of the invention to overcome the deficiency of prior art and provide a kind of AFM probe cross force calibration coefficient measurement
Method and cross force scaling method.
The present invention measures AFM probe cross force calibration coefficient using frictional force device for measuring force based on Amontons laws,
Simple, the easy-operating advantage with step, and calibrated error is little, is widely portable to various types of probes or micro-cantilever
The measurement of cross force calibration coefficient.
The present invention is based on Amontons laws, it is considered to AFM frictional force dynamometry principles, using standard material, it is proposed that measurement
The experimental technique principle model of AFM probe cross force calibration coefficient；
(1) the Amontons law constitutive equations of micro/nano-scale are：
Ff=k (Fn+Fad)……(3)
Wherein, parameter FfFor frictional force；Parameter k is the coefficient of friction between probe and sample；Parameter FnFor shorting pin loaded
In the normal load of sample surfaces, parameter FadFor sample surfaces adhesive force.
(2) AFM frictional force dynamometry principle is：
Ff=Uf×β……(2)
Wherein, parameter FfFor frictional force；Parameter UfFor the signal of telecommunication that frictional experiment is measured；Parameter beta is that cross force demarcates system
Number.
Simultaneous equations (2), (3) can measure the experimental technique principle model of AFM probe cross force calibration coefficient：
Utβ=k (Fn+Fad)……(1)
AFM probe cross force calibration coefficient measuring method of the present invention, be under the conditions of standard laboratory atmosphere, using AFM,
Measurement sample the same area bears different normal load FnUnder friction force electrical signal UfAnd surface adhesion power Fad；Substitution formula (1)
In, cross force calibration coefficient β is solved using the optimized parameter estimation technique；
Ufβ=k (Fn+Fad)……….(1)
In formula (1), K is the coefficient of friction between probe and sample.
In AFM probe cross force calibration coefficient measuring method of the present invention, standard laboratory atmosphere condition refers to that temperature is 21
DEG C, humidity is 50% super-clean environment.
In AFM probe cross force calibration coefficient measuring method of the present invention, normal load FnDemarcated using thermal constant method.
In AFM probe cross force calibration coefficient measuring method of the present invention, at least 5 kinds different normal direction are applied to AFM probe
Load Fn, for each normal load Fn, using the frictional force module of AFM, scanned sample surface selection area, obtain the area
Domain is in corresponding normal load FnMantle friction under effect is tried hard to, and resulting mantle friction is tried hard to adopt Gaussian statistics, is obtained
To corresponding normal load FnFriction force electrical signal U under effectf。
In AFM probe cross force calibration coefficient measuring method of the present invention, apply the different normal direction of 5-20 kinds to AFM probe and carry
Lotus Fn；Front and back stages normal load FnDifference it is equal.
In AFM probe cross force calibration coefficient measuring method of the present invention, module, the same area of measurement sample are tried hard to using AFM
The adhesive force in domain, obtains specimen surface adhesive force F through Gaussian statisticsad。
In AFM probe cross force calibration coefficient measuring method of the present invention, when adhesive force is measured, module is tried hard to using AFM, survey
At least 1024 points of amount sample the same area.
In AFM probe cross force calibration coefficient measuring method of the present invention, sample is selected from standard materials such as monocrystalline silicon piece, mica sheets
Material or MoS2In the non-standard materials such as nanometer sheet any one.
In AFM probe cross force calibration coefficient measuring method of the present invention, the optimized parameter estimation technique is wheat quart optimized algorithm；
Using the optimized parameter assessment function of " one stop " numerical analysis software of Beijing 7 degree of freedom high-tech company limited, it is based on
Amontons laws are with AFM frictional force dynamometry principles with equation Utβ-k(Fn+Fad) for numerical model, substitute into the glutinous of material surface
Attached power, two constant values of coefficient of friction, with load frictional force electrical signal data as independent variable, dependent variable be input in software, adopt
Cross force calibration coefficient β is estimated with wheat quart optimized algorithm.
AFM probe cross force scaling method of the present invention, is, under the conditions of standard laboratory atmosphere, using AFM, to measure sample
The same area bears different normal load FnUnder friction force electrical signal UfAnd surface adhesion power Fad；In substitution formula (1), using most
Excellent Parameter Estimation Method solves cross force calibration coefficient β；
β is substituted in formula (2), the demarcation of AFM probe cross force is completed；
Ff=Uf×β……(2)
In formula (2), FfThe frictional force of specimen surface is acted on for AFM probe, meanwhile, and probe carried it is horizontal
Power.
Probe cross force scaling method of the present invention based on Amontons laws, based on Amontons laws, it is considered to which AFM rubs
Power dynamometry principle is wiped, the experimental technique principle model of measurement AFM probe cross force calibration coefficient is proposed；
Experimental technique principle utilizes Amontons laws and AFM frictional force dynamometry principles；
The friction signal refers to the friction signal measured under multigroup different normal loads；
The surface adhesion power is that Jing Gauss curve fitting takes after the kinetic measurement sample surfaces at least adhesive force of 1024 points
It is worth to；
Friction and adhesive force test area are less than 1 μm of 1 μ m；
The coefficient of friction of the material is the coefficient of friction under tip flakes friction conditions；
The approximating method is the optimized parameter estimation technique.
The present invention has advantages below：(a) this method using sample material there is arbitrariness, be not required to processing, the side of drawing materials
Just, low cost；B () this method is based on Amontons laws, it is contemplated that impact of the adhesive force to demarcating, calculating process are simple, fast
Fast, accurate, the cross force for being widely portable to all kinds of AFM probes and micro-cantilever is demarcated.
Description of the drawings
Accompanying drawing 1 is the flow chart that utilization Nanotribology linear relationship of the present invention demarcates AFM probe cross force；
Accompanying drawing 2 is the surface adhesion power afm image of 1 Plays sample monocrystal silicon of embodiment；
Accompanying drawing 3 is the surface adhesion power Gauss distribution figure of 1 Plays sample monocrystal silicon of embodiment；
Accompanying drawing 4 is the surface adhesion power afm image of 2 Plays sample mica sheet of embodiment；
Accompanying drawing 5 is the surface adhesion power Gauss distribution figure of 2 Plays sample mica sheet of embodiment；
Accompanying drawing 6 is non-standard samples MoS in embodiment 32The surface adhesion power afm image of nanometer sheet；
Accompanying drawing 7 is non-standard samples MoS in embodiment 32The surface adhesion power Gauss distribution figure of nanometer sheet；
Accompanying drawing 8 is non-standard samples MoS in embodiment 32AFM surface topography images；
Accompanying drawing 9 is non-standard samples MoS in embodiment 32Cross section AFM height maps；
From accompanying drawing 8 as can be seen that MoS2For nano-sheet；
From accompanying drawing 9 as can be seen that used MoS2For two-dimension nano materials.
Specific embodiment
A kind of probe cross force scaling method based on Amontons laws, it is characterised in that including following step：
1st, based on Amontons laws, it is considered to AFM frictional force dynamometry principles, using standard material, propose measurement AFM probe
The experimental technique principle model of cross force calibration coefficient；
The Amontons law constitutive equations of micro/nano-scale are：
Ff=k (Fn+Fad)….(3)
Wherein, parameter FfFor frictional force；Parameter k is the coefficient of friction between probe and sample；Parameter FnFor shorting pin loaded
In the normal load of sample surfaces, parameter FadFor sample surfaces adhesive force.
AFM frictional force dynamometry principles are：
Ff=Uf×β……(2)
Wherein, parameter FfFor frictional force；Parameter UfFor the signal of telecommunication that frictional experiment is measured；Parameter beta is that cross force demarcates system
Number.
Simultaneous equations (2), (3) can measure the experiment of AFM probe cross force calibration coefficient
Method And Principle model：
Ufβ=k (Fn+Fad)……(1)
2nd, the friction signal of measurement standard material and surface adhesion power under the conditions of standard laboratory atmosphere：
(1) sample after cleaning is positioned under AFM, using frictional force module, scan area is 200nm × 200nm.
The friction that 10 web material surfaces are measured under the normal load of 10nN to 100nN is tried hard to, and tries hard to used method per width friction
Uniformly increase to load (set point values), friction force electrical signal takes average Jing after Gaussian statistics, and wherein normal load is using warm
Constant method is demarcated；
(2) adhesive force of 1024 points is measured in the same area that measurement friction signal is located using AFM Massa Medicata Fermentata wire module,
Its average is taken Jing after Gaussian statistics as surface adhesion power F of the samplead。
3rd, by the coefficient of friction of friction signal data and material under different loads obtained by frictional experiment, surface adhesion power generation
Enter principle model, the cross force calibration coefficient of probe is calculated using optimized parameter method of estimation.
(1) search pertinent literature or data obtains the tip flakes type coefficient of frictions of material；
(2) during gained friction signal, normal load and material surface adhesive force, coefficient of friction substitution equation will be tested 3.,
The method estimated using optimized parameter calculates the value of cross force calibration coefficient β.
4., in order to verify the stability and effectiveness of scaling method, same probe is carried out demarcating laggard using multiple material
Row analysis contrast.
Embodiment 1：
Used atomic force microscope model in embodiment 1：Cypher ES,Asylum Research,CA；Marked
Fixed probe model：AC160TS,Olympus；Demarcate monocrystalline silicon piece of the utilized standard material for 1cm × 1cm；Check in
Silicon chip coefficient of friction be 0.050 (Materials Letters, 2015,142:207-210.).Whole calibration process is in ultra-clean chamber
Complete, temperature is 21 DEG C, and humidity is 50%.
By step 2, the silicon chip after clean drying is positioned on AFM sample stages, using frictional force module, scan area is
200nm×200nm.The friction that 10 width silicon chip surfaces are measured under the normal load of 10nN to 100nN is tried hard to, every width frictional force
The used normal load (set point values) of figure uniformly increases, and friction force electrical signal is shown in Table 1 Jing after Gaussian statistics.
By step 2, in the same area for carrying out friction testing, we try hard to module using AFM and uniformly measure silicon
The adhesive force of 1024 points on piece, after Gaussian statistics, its average is 130nN (Fig. 2).
By step 3, estimated using the optimized parameter of " one stop " numerical analysis software of Beijing 7 degree of freedom high-tech company limited
Meter function, based on Amontons laws with AFM frictional force dynamometry principles with equation Ufβ=k (Fn+Fad) for numerical model, substitute into
The adhesive force of material surface, two constant values of coefficient of friction, with ten groups of load frictional force electrical signal datas as independent variable, because becoming
Amount is input in software, estimates cross force calibration coefficient β using wheat quart optimized algorithm1Value be 0.522nN/mV.
Embodiment 2：
Used atomic force microscope model in embodiment 2：Cypher ES,Asylum Research,CA；Marked
Fixed probe model：AC160TS,Olympus；Demarcate mica sheet of the utilized material for 1cm × 1cm；Check in mica sheet
Coefficient of friction be 0.094 (Langmuir, 1999,15 (22):7662‐7669.).Whole calibration process is completed in ultra-clean chamber, temperature
Spend for 21 DEG C, humidity is 50%.
By step 2, the mica sheet of firm cleavage is positioned on AFM sample stages, using frictional force module, scan area is
200nm×200nm.The friction that 10 width mica surfaces are measured under the normal load of 10nN to 100nN is tried hard to, every width frictional force
The used normal load (set point values) of figure uniformly increases, and friction force electrical signal is shown in Table 2 Jing after Gaussian statistics.
By step 2, in the same area for carrying out friction testing, we try hard to module using AFM and uniformly measure cloud
The adhesive force of 1024 points on master slice, after Gaussian statistics, its average is 3nN (Fig. 2).
By step 3, estimated using the optimized parameter of " one stop " numerical analysis software of Beijing 7 degree of freedom high-tech company limited
Meter function, based on Amontons laws with AFM frictional force dynamometry principles with equation Ufβ=k (Fn+Fad) for numerical model, substitute into
The adhesive force of material surface, two constant values of coefficient of friction, with ten groups of load frictional force electrical signal datas as independent variable, because becoming
Amount is input in software, estimates cross force calibration coefficient β using wheat quart optimized algorithm2Value be 0.520nN/mV.
Embodiment 3：
Used atomic force microscope model in embodiment 3：Cypher ES,Asylum Research,CA；Marked
Fixed probe model：AC160TS,Olympus；Demarcate the MoS that utilized material is prepared by mechanical stripping method2Nanometer sheet,
Thickness is about 18nm and sees Fig. 3；Check in MoS2Nanometer sheet coefficient of friction be 0.003 (Euro physics Letters, 2002,58
(4):610.).Whole calibration process is completed in ultra-clean chamber, and temperature is 21 DEG C, and humidity is 50%.
By step 2, the silicon chip after clean drying is positioned on AFM sample stages, using frictional force module, scan area is
200nm×200nm.10 width MoS are measured under the normal load of 10nN to 100nN2The friction on surface is tried hard to, every width frictional force
The used normal load (set point values) of figure uniformly increases, and friction force electrical signal is shown in Table 3 Jing after Gaussian statistics.
By step 2, in the same area for carrying out friction testing, we try hard to module using AFM and uniformly measure
MoS2The adhesive force of 1024 points on surface, after Gaussian statistics, its average is 130nN (Fig. 2).
By step 3, estimated using the optimized parameter of " one stop " numerical analysis software of Beijing 7 degree of freedom high-tech company limited
Meter function, based on Amontons laws with AFM frictional force dynamometry principles with equation Utβ=k (Fn+Fad) for numerical model, substitute into
The adhesive force of material surface, two constant values of coefficient of friction, with ten groups of load frictional force electrical signal datas as independent variable, because becoming
Amount is input in software, estimates cross force calibration coefficient β using wheat quart optimized algorithm1Value be 0.502nN/mV.
The probe cross force calibration coefficient β drawn by embodiment 1,2,31、β2、β3It is compared, demarcates relative error little
In 4%, illustrate that this scaling method is effective and stable.
1. silicon chip varying load friction signal of table
2 mica sheet varying load friction signal of table
Table 3.MoS2Nanometer sheet varying load friction signal
Claims (10)
1.AFM probe cross force calibration coefficient measuring methods, are, under the conditions of standard laboratory atmosphere, using AFM, to measure sample
The same area bears different normal load FnUnder friction force electrical signal UfAnd surface adhesion power Fad；In substitution formula (1), using most
Excellent Parameter Estimation Method solves cross force calibration coefficient β；
Ufβ=k (Fn+Fad)..........(1)
In formula (1), K is the coefficient of friction between probe and sample.
2. AFM probe cross force calibration coefficient measuring method according to claim 1, it is characterised in that：Standard laboratory
Environmental condition refers to temperature for 21 DEG C, and humidity is 50% super-clean environment.
3. AFM probe cross force calibration coefficient measuring method according to claim 1, it is characterised in that：Normal load FnAdopt
Demarcated with thermal constant method.
4. AFM probe cross force calibration coefficient measuring method according to claim 1, it is characterised in that：AFM probe is applied
Add to few 5 kinds of different normal load Fn, for each normal load Fn, using the frictional force module of AFM, scanned sample table
Face selection area, obtains the region in corresponding normal load FnMantle friction under effect is tried hard to, to resulting mantle friction
Try hard to adopt Gaussian statistics, obtain corresponding normal load FnFriction force electrical signal U under effectf。
5. AFM probe cross force calibration coefficient measuring method according to claim 4, it is characterised in that：AFM probe is applied
Plus the normal load F that 5-20 kinds are differentn；Front and back stages normal load FnDifference it is equal.
6. AFM probe cross force calibration coefficient measuring method according to claim 1, it is characterised in that：Tried hard to using AFM
Module, measures the adhesive force of sample the same area, obtains specimen surface adhesive force F through Gaussian statisticsad。
7. AFM probe cross force calibration coefficient measuring method according to claim 6, it is characterised in that：Adhesive force is measured
When, module is tried hard to using AFM, measure at least 1024 points of sample the same area.
8. AFM probe cross force calibration coefficient measuring method according to claim 1, it is characterised in that：Sample is selected from single
Crystal silicon chip, mica sheet, MoS2Any one in nanometer sheet.
9. the AFM probe cross force calibration coefficient measuring method according to 8 any one of claim 1, it is characterised in that：
The optimized parameter estimation technique is wheat quart optimized algorithm.
10.AFM probe cross force scaling methods, are, under the conditions of standard laboratory atmosphere, using AFM, to measure the same area of sample
Bear different normal load F in domainnUnder friction force electrical signal UfAnd surface adhesion power Fad；In substitution formula (1), using optimized parameter
The estimation technique solves cross force calibration coefficient β；β is substituted in formula (2), the demarcation of AFM probe cross force is completed；
Ff=Uf×β......(2)
In formula (2), FfThe cross force that produce is scanned in material surface for AFM probe.
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| CN114446402A (en) * | 2022-03-04 | 2022-05-06 | 兰州理工大学 | Research method for phonon friction between graphene layers under coupling of layer number and load |
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| CN106979897A (en) * | 2017-05-10 | 2017-07-25 | 湘潭大学 | A kind of measuring method of nano material limiting shearing stress |
| CN107192856A (en) * | 2017-06-26 | 2017-09-22 | 湘潭大学 | A kind of cross force scaling method based on AFM probe structural parameters |
| CN109406386A (en) * | 2017-10-30 | 2019-03-01 | 西南交通大学 | The design of profiled cross-section micro-cantilever beam probe and processing method applied to the measurement of nanoscale single-contact ultralow friction coefficient |
| WO2019084983A1 (en) * | 2017-10-30 | 2019-05-09 | 西南交通大学 | Methods for designing and processing micro-cantilever probe with special-shaped cross section applied to ultra-low friction coefficient measurement in nanoscale single point contact |
| US10739379B2 (en) | 2017-10-30 | 2020-08-11 | Southwest Jiaotong University | Methods for designing and processing a microcantilever-based probe with an irregular cross section applied in an ultra-low friction coefficient measurement at a nanoscale single-point contact |
| CN109406386B (en) * | 2017-10-30 | 2020-10-23 | 西南交通大学 | Design and processing method of special-shaped section cantilever beam probe for measuring ultralow friction coefficient |
| CN111190031A (en) * | 2020-01-21 | 2020-05-22 | 湘潭大学 | Method for correcting friction performance of probe abrasion of atomic force microscope |
| CN111190031B (en) * | 2020-01-21 | 2022-10-25 | 湘潭大学 | Method for correcting friction performance of probe abrasion of atomic force microscope |
| CN114446402A (en) * | 2022-03-04 | 2022-05-06 | 兰州理工大学 | Research method for phonon friction between graphene layers under coupling of layer number and load |
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