CN109884347A - The method for delaying probe tip to wear under AFM tapping-mode - Google Patents
The method for delaying probe tip to wear under AFM tapping-mode Download PDFInfo
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- CN109884347A CN109884347A CN201910138130.4A CN201910138130A CN109884347A CN 109884347 A CN109884347 A CN 109884347A CN 201910138130 A CN201910138130 A CN 201910138130A CN 109884347 A CN109884347 A CN 109884347A
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Abstract
The present invention relates to a kind of methods for delaying probe tip to wear under AFM tapping-mode, it is by characterizing depressed phenomenon when tip wear is aggravated using SPA sudden phase anomalies, that is null phenomenon mainly comprises the steps that (1) obtains the phase change figure in probe vibration processes using AFM high-Speed Data-Acquisition Module.(2) observing in phase diagram whether there is SPA sudden phase anomalies (the instantaneous increase of phase value).(3) appropriate to increase amplitude set point, increase free amplitude, reduce scanning speed if there are non-accidental SPA sudden phase anomalies in figure.(4) step 1, step 2 and step 3 are repeated, until SPA sudden phase anomalies are eliminated in tip phase figure.(5) optimization is completed, sample surfaces are scanned with sweep parameter at this time.The present invention can real-time online observe the abrasion condition of probe tip, and sweep parameter can be adjusted in real time to reduce the rate of wear of needle point.To reduce the rate of wear of needle point, extend the service life of probe, saves experimental cost.
Description
Technical field
The present invention relates to delay probe tip to grind under ultraprecise detection technique field more particularly to a kind of AFM tapping-mode
The method of damage.
Background technique
With the development of micro-/ nano technology, people gradually enter micro-scale from macro-scale to the understanding of things.For
Have a better understanding to microcosmos, " imaging " under micro-nano-scale become ever more important.Atomic force microscope
Ultraprecise detection instrument (atomic force microscopes abbreviation AFM) practical as one kind, without vacuum environment, sample
The requirement of product conduction, compared with optical microscopy, electron microscope, it can obtain real three-dimensional appearance information, can survey
The information such as microstructure height, the roughness at side inclination angle and Ultra-precision Turning surface are measured, thus are widely used in aviation boat
It, the fields such as material science, microelectronics.Tapping-mode is one of main operation modes of AFM.Compared to contact mode, tapping
Probe is discontinuously contacted with sample under mode, significantly reduces the interaction force between needle point and sample.For to probe
Protection, tapping-mode receives more and more attention.
The nanometer resolution of AFM depend on fine probe, but unreasonable parameter setting can change probe tip with
Active force between sample surfaces can aggravate the damage of probe, even result in needle point and be broken when active force increase is larger
Abrasion.Since the image that probe scanning sample surfaces obtain is actually needle point and sample surface morphology convolution as a result, needle point
Damage necessarily lead to the distortion of measurement result.Also, probe is expensive, can not repair to it after abrasion.Therefore,
Tip wear is reduced, the service life for improving probe has great importance to raising image quality, reduction experimental cost.
Summary of the invention
Aiming at the problems existing in the prior art, the purpose of the present invention is to provide delay to visit under a kind of AFM tapping-mode
The method of needle tip wear is provided by optimization sweep parameter, for example, amplitude set point, free amplitude, scanning speed, disappear
Except depressed phenomenon, to reduce the rate of wear of needle point, extends the service life of probe, save experimental cost.The present invention utilizes
SPA sudden phase anomalies characterize depressed phenomenon when tip wear aggravation, that is, null phenomenon passes through phase in observation tip phase variation diagram
The number of position mutation, to observe tip wear situation in real time.
The technical solution adopted by the present invention to solve the technical problems is:
A kind of method for delaying probe tip to wear under AFM tapping-mode comprising following steps:
Step 1: bimorph vibratory driver drive probe sample surfaces with preset frequency do damping by
Compel vibration, vibration frequency when preset frequency refers to probe face herein；
Probe is discontinuously contacted with sample surfaces according to preset interval, is acquired piezoelectric scanning pipe at each data collection point and is existed
X, the bias voltage in the direction y obtains the location information of each contact point；
Step 2: the phase change figure in probe vibration processes is obtained using AFM high-Speed Data-Acquisition Module；
Step 3: it whether there is SPA sudden phase anomalies in observation phase diagram；
Step 4: if there are SPA sudden phase anomalies in figure, just suboptimization sweep parameter is appropriate to increase amplitude set point, increase
Free amplitude reduces scanning speed, obtains the phase change figure of AFM probe；The working amplitude is equal to free amplitude and amplitude
The product of set point；
Step 5: optimizing sweep parameter again, according to respective preset single regulated quantity successively to amplitude set point, freedom
Amplitude, scanning speed are adjusted, and repeat step 1 to step 4, obtain the phase change figure of corresponding AFM probe, phase is prominent
Change gradually decreases, until SPA sudden phase anomalies are eliminated in tip phase figure；
Step 6: it determines that phase is prominent from the phase change figure of the AFM probe after final optimization pass and disappears, then depressed phenomenon quilt
It eliminates, is at this time ideal working condition, completes the optimization of sweep parameter, sample surfaces are scanned with sweep parameter at this time.
Preferably, when the phase value of probe is more than 50 °, determine that there are SPA sudden phase anomalies at this.
Preferably, each increment of the amplitude set point is 0.2.
Preferably, each fixed increment of the free amplitude is 50mV.
Preferably, the reduction amount of each scanning speed is 0.2Hz.
Preferably, when the phase value of probe is less than 50 °, determine that the mutation in tip phase figure is eliminated.
Preferably, it is sequentially increased amplitude set point, increase free amplitude and reduces scanning speed, sweep parameter is adjusted
Section.
Preferably, the preset interval in step 1 is 1s/ (10KHz)~1s/ (40KHz).
Preferably, the preset interval in step 1 is 1s/ (30KHz), that is, scanning speed can be improved, and is avoided that probe is sent out
Raw resonance.
The beneficial effects of the present invention are:
Compared with prior art, the method for delaying probe tip to wear under AFM tapping-mode of the invention is prominent using phase
Become depressed phenomenon when characterization tip wear aggravation, the abrasion condition of probe tip, and energy are observed so as to real-time online
Enough sweep parameters that adjusts in real time are to reduce the rate of wear of needle point.
Detailed description of the invention
Fig. 1 is AFM high-speed data acquisition in the method for delaying probe tip to wear under AFM tapping-mode according to the present invention
The phase change figure of the collected AFM probe of module；
Fig. 2 is AFM in the method for delaying probe tip to wear under AFM tapping-mode according to the present invention after just suboptimization
The phase change figure of probe；
Fig. 3 is AFM in the method for delaying probe tip to wear under AFM tapping-mode according to the present invention again after suboptimization
The phase change figure of probe；
Fig. 4 be delay under AFM tapping-mode according to the present invention probe tip wear method eliminate SPA sudden phase anomalies after,
The phase change figure of AFM probe；In above-mentioned each figure: 1 indicates SPA sudden phase anomalies；
Fig. 5 be delay under AFM tapping-mode according to the present invention probe tip wear method first embodiment in
Amplitude set point: 0.2；Free amplitude: 300mV；Scanning speed: 1.0Hz scans the phase for the AFM probe that hard sample surfaces obtain
Position variation diagram；
Fig. 6 be delay under AFM tapping-mode according to the present invention probe tip wear method first embodiment in
Amplitude set point: 0.4；Free amplitude: 350mV；Scanning speed: 0.8Hz scans the phase for the AFM probe that hard sample surfaces obtain
Position variation diagram；
Fig. 7 be delay under AFM tapping-mode according to the present invention probe tip wear method first embodiment in
Amplitude set point: 0.6；Free amplitude: 400mV；Scanning speed: 0.6Hz scans the phase for the AFM probe that hard sample surfaces obtain
Position variation diagram；
Fig. 8 be delay under AFM tapping-mode according to the present invention probe tip wear method first embodiment in
Amplitude set point: 0.8；Free amplitude: 450mV；Scanning speed: 0.4Hz scans the phase for the AFM probe that hard sample surfaces obtain
Position variation diagram；And
Fig. 9 be delay under AFM tapping-mode according to the present invention probe tip wear method 3rd embodiment in
Amplitude set point: 0.2；Free amplitude: 300mV；Scanning speed: 1.0Hz scans the phase for the AFM probe that soft sample surfaces obtain
Position variation diagram.
Figure 10 is the flow chart for the method for delaying probe tip to wear under AFM tapping-mode according to the present invention.
Specific embodiment
The method for delaying probe tip to wear under AFM tapping-mode according to the present invention is provided through optimization scanning ginseng
Number, to reduce the rate of wear of needle point, extends for example, amplitude set point, free amplitude, scanning speed, eliminate depressed phenomenon
The service life of probe saves experimental cost.Depressed phenomenon when the present invention is aggravated using SPA sudden phase anomalies characterization tip wear,
That is, null phenomenon, by the number of SPA sudden phase anomalies in observation tip phase variation diagram, to observe tip wear in real time
Situation, as shown in Figures 1 to 10, the specific steps of which are as follows:
Step 1: bimorph vibratory driver drive probe sample surfaces with preset frequency do damping by
Compel vibration, vibration frequency when preset frequency refers to probe face herein.
Probe is discontinuously contacted with sample surfaces according to preset interval, is acquired piezoelectric scanning pipe at each data collection point and is existed
X, the bias voltage in the direction y obtains the location information of each contact point；
Preferably, information all acquisition probes vibration hundreds of thousands per second of not each contact point, there is hundreds of thousands in contact point
It is a, but data collection point only has several hundred.
Preferably, which changes with probe model and structure.
Preferably, the preset interval in step 1 is 1s/ (10KHz)~1s/ (40KHz).
Preferably, the preset interval in step 1 is 1s/ (30KHz), that is, scanning speed can be improved, and is avoided that probe is sent out
Raw resonance.
Step 2: the phase change figure in probe vibration processes is obtained using AFM high-Speed Data-Acquisition Module；
Step 3: it whether there is SPA sudden phase anomalies in observation phase diagram；
Preferably, it is shown in Fig. 1 and utilizes the phase change in AFM high-Speed Data-Acquisition Module acquisition probe vibration processes
Figure, wherein abscissa is the acquisition time of AFM high-Speed Data-Acquisition Module, and ordinate is phase value.Fig. 2, Fig. 3 are identical as Fig. 1,
From fig. 1, it can be seen that wherein there are more SPA sudden phase anomalies 1, figure middle probe phase value is more than 50 ° of point, is that phase is prominent
Become, illustrates that depressed phenomenon is more serious, tip wear fast speed.
Preferably, when tip phase value is more than 50 °, determine that there are SPA sudden phase anomalies at this.
Step 4: appropriate to increase amplitude set point, increase free amplitude, reduce scanning if there are SPA sudden phase anomalies in figure
Speed；
Preferably, working amplitude is equal to the product of free amplitude and amplitude set point.
Preferably, each increment of amplitude set point is 0.2.
Preferably, each fixed increment of free amplitude is 50mV.
Preferably, the reduction amount of each scanning speed is 0.2Hz.
Specifically, first suboptimization sweep parameter, it is appropriate to increase amplitude set point, increase free amplitude, reduce scanning speed,
The phase change figure of AFM probe is as shown in Figure 2 at this time.Compared to Figure 1, the number of SPA sudden phase anomalies significantly reduces in Fig. 2, phase value
It significantly reduces.But phase angle is still greater than 50 °, it is therefore desirable to continue to optimize sweep parameter.
From Fig. 2 it can be found that SPA sudden phase anomalies 1 time number is reduced, illustrate that depressed phenomenon is alleviated, tip wear situation is
Improve.
Step 5: optimizing sweep parameter again, appropriate to increase amplitude set point, increase free amplitude, reduce scanning speed,
Step 1 is repeated to step 4, until SPA sudden phase anomalies are eliminated in tip phase figure.
Preferably, when the phase value of probe is less than 50 °, determine that the mutation in tip phase figure is eliminated.
The phase change figure of AFM probe is as shown in Figure 3 at this time；Observation Fig. 3 can be found that SPA sudden phase anomalies 1 time number is reduced, and says
Bright depressed phenomenon is further alleviated, and tip wear situation has been greatly improved.
Step 6: when the optimization for completing sweep parameter, sample surfaces are scanned with sweep parameter at this time.
The phase change figure of AFM probe after final optimization pass is as shown in Figure 4.
Observation Fig. 4 can be found that SPA sudden phase anomalies 1 disappear, and illustrates that depressed phenomenon is eliminated, tip wear situation significantly mitigates.
Below with reference to specific example, the present invention will be further described.
Embodiment 1
When the hard sample surfaces of probe scanning, tip wear is more serious, and when scanning soft sample surfaces, tip wear compared with
Gently.Two groups of experiments are set, scan hard sample respectively, for example, polycrystalline titanium film, model: RS-12M and soft sample, for example, poly- diformazan
Radical siloxane film, model: the surface of PDMS-SOFT-1-12.
Scan hard sample surfaces
Sweep parameter is provided that
Scanning range: 30 μm；
Probe vibration frequency: 30KHz；
Sampling number: 512*512；
Amplitude set point: 0.2；
Free amplitude: 300mV；
Scanning speed: 1.0Hz；
Sampling time when acquisition phase figure is set as 0.85s.
Hard sample (polycrystalline titanium film, model: RS-12M) surface is scanned with above-mentioned sweep parameter, obtains phase as shown in Figure 5
Position variation diagram.It can be seen from the figure that the point that phase value is more than 50 ° has very much, it is mutual between probe tip and sample at this time
Active force is very big, and tip wear is more serious.
Adjustment sweep parameter is amplitude set point: 0.4；Free amplitude: 350mV；Scanning speed: 0.8Hz.Other parameters are set
It sets constant, scans hard sample surfaces same position and obtain phase change figure as shown in FIG. 6.It can be seen from the figure that phase value
Point more than 50 ° has reduced much compared with Fig. 5, illustrates that the abrasion condition of needle point is alleviated, but phase value is more than 50 °
Point still have very much, need to continue optimize sweep parameter.
Adjustment sweep parameter is amplitude set point: 0.6；Free amplitude: 400mV；Scanning speed: 0.6Hz.Other parameters are set
It sets constant, scans hard sample surfaces same position and obtain phase change figure as shown in Figure 7.It can be seen from the figure that phase value
Point more than 50 ° reduces much again compared with Fig. 5, illustrates that the abrasion condition of needle point is alleviated, but phase value is more than 50 °
Point do not eliminate also, need to continue optimize sweep parameter.
Adjustment sweep parameter is amplitude set point: 0.8；Free amplitude: 450mV；Scanning speed: 0.4Hz.Other parameters are set
It sets constant, scans hard sample surfaces same position and obtain phase change figure as shown in Figure 8.It can be seen from the figure that phase value
Point more than 50 ° has substantially eliminated, and very little, tip wear are lighter for the interaction force between probe tip and sample at this time.
Therefore, can sweep parameter at this time scan sample.
Embodiment 2
Tip wear experiment
With amplitude set point: 0.2；Free amplitude: 300mV；Scanning speed: 0.8Hz, other sweep parameters are constant.Scanning
Hard sample surfaces same position 20 times.After the completion of scanning, needle point electron microscope is obtained using scanning electron microscope, and probe needle is estimated with this
The blunt round radius of point, with the abrasion condition of the size characterization needle point of probe tip blunt round radius, (blunt round radius is bigger, tip wear
It is more serious).It is 79nm using the probe tip blunt round radius that electron microscope is estimated.
Again with amplitude set point: 0.8；Free amplitude: 450mV；Scanning speed: 0.4Hz scans the same position of hard sample surfaces
It sets 20 times.It is 17.6nm using the probe tip blunt round radius that electron microscope is estimated.
According to the experimental results, when SPA sudden phase anomalies are more, tip wear is more serious.When there is no SPA sudden phase anomalies, needle point mill
It damages lighter.Illustrate present invention adjustment sweep parameter, eliminates SPA sudden phase anomalies, the method for mitigating tip wear has apparent effect.
Embodiment 3
Scan soft sample surfaces
Sweep parameter is provided that
Scanning range: 30 μm；
Probe vibration frequency: 30KHz；
Sampling number: 512*512；
Amplitude set point: 0.2；
Free amplitude: 300mV；
Scanning speed: 1.0Hz；
Sampling time when acquisition phase figure is set as 0.85s.
Soft sample (PDMS membrane, model: PDMS-SOFT-1-12) surface is scanned with above-mentioned sweep parameter, is obtained
To phase change figure as shown in Figure 9.It can be seen from the figure that not occurring the point that phase value is more than 50 °, this is soft with scanning
The lighter experiment law of tip wear is consistent when sample surfaces, also demonstrates the relationship of SPA sudden phase anomalies and tip wear.
The above is the preferred embodiment of the application, it is noted that for those skilled in the art
For, under the premise of not departing from this technology principle, several improvements and modifications can also be made, these improvements and modifications also should be regarded as
The protection scope of the application.
Claims (9)
1. a kind of method for delaying probe tip to wear under AFM tapping-mode, which is characterized in that it includes the following steps:
Step 1: bimorph vibratory driver drive probe does the forced oscillation of damping in sample surfaces with preset frequency
Dynamic, when preset frequency refers to probe face herein vibration frequency；
Probe is discontinuously contacted with sample surfaces according to preset interval, acquires at each data collection point piezoelectric scanning pipe in x, y
The bias voltage in direction obtains the location information of each contact point；
Step 2: the phase change figure in probe vibration processes is obtained using AFM high-Speed Data-Acquisition Module；
Step 3: it whether there is SPA sudden phase anomalies in observation phase diagram；
Step 4: if there are SPA sudden phase anomalies in figure, just suboptimization sweep parameter is appropriate to increase amplitude set point, increase freely
Amplitude reduces scanning speed, obtains the phase change figure of AFM probe；Working amplitude is equal to free amplitude and amplitude set point
Product；
Step 5: optimizing sweep parameter again, successively shakes to amplitude set point, freely according to respective preset single regulated quantity
Width, scanning speed are adjusted, and repeat step 1 to step 4, obtain the phase change figure of corresponding AFM probe, SPA sudden phase anomalies
It gradually decreases, until SPA sudden phase anomalies are eliminated in tip phase figure；
Step 6: it determines that phase is prominent from the phase change figure of the AFM probe after final optimization pass and disappears, then depressed phenomenon is disappeared
It removes, is at this time ideal working condition, completes the optimization of sweep parameter, sample surfaces are scanned with sweep parameter at this time.
2. the method for delaying probe tip to wear under AFM tapping-mode as described in claim 1, which is characterized in that work as probe
Phase value when being more than 50 °, determine that there are SPA sudden phase anomalies at this.
3. the method for delaying probe tip to wear under AFM tapping-mode as claimed in claim 2, which is characterized in that the width
Being worth each increment of set point is 0.2.
4. delay under AFM tapping-mode as claimed in claim 3 probe tip wear method, which is characterized in that it is described from
It is 50mV by each fixed increment of amplitude.
5. the method for delaying probe tip to wear under AFM tapping-mode as claimed in claim 4, which is characterized in that sweep every time
The reduction amount for retouching speed is 0.2Hz.
6. the method for delaying probe tip to wear under AFM tapping-mode as described in claim 1, which is characterized in that work as probe
Phase value be lower than 50 ° when, determine tip phase figure in mutation be eliminated.
7. the method for delaying probe tip to wear under the AFM tapping-mode as described in claim 1 to 6, which is characterized in that according to
Secondary increase amplitude set point increases free amplitude and reduces scanning speed, and sweep parameter is adjusted.
8. the method for delaying probe tip to wear under AFM tapping-mode as described in claim 7, which is characterized in that step
Preset interval in one is 1s/ (10KHz)~1s/ (40KHz).
9. the method for delaying probe tip to wear under AFM tapping-mode as described in claim 7, which is characterized in that step
Preset interval in one is 1s/ (30KHz), that is, scanning speed can be improved, and be avoided that probe resonates.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112305264A (en) * | 2020-10-30 | 2021-02-02 | 燕山大学 | Method for obtaining hardness and elastic modulus measurement values based on AFM nano indentation experiment |
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| CN1624452A (en) * | 2003-08-25 | 2005-06-08 | 精工电子纳米科技术有限公司 | Scanning probe microscope and scanning method |
| CN102439462A (en) * | 2008-11-13 | 2012-05-02 | 布鲁克纳米公司 | Method and apparatus of operating a scanning probe microscope |
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2019
- 2019-02-25 CN CN201910138130.4A patent/CN109884347A/en not_active Withdrawn
Patent Citations (4)
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|---|---|---|---|---|
| JPH06241762A (en) * | 1993-02-18 | 1994-09-02 | Seiko Instr Inc | Frictional force microscope |
| CN1624452A (en) * | 2003-08-25 | 2005-06-08 | 精工电子纳米科技术有限公司 | Scanning probe microscope and scanning method |
| CN102439462A (en) * | 2008-11-13 | 2012-05-02 | 布鲁克纳米公司 | Method and apparatus of operating a scanning probe microscope |
| CN105319396A (en) * | 2008-11-13 | 2016-02-10 | 布鲁克纳米公司 | Method and apparatus of using a peak force tapping mode to measure the physical properties of a sample |
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| 杨延婷: "基于AFM和DIC的探针纳米尺度磨损实验研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅱ辑》 * |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112305264A (en) * | 2020-10-30 | 2021-02-02 | 燕山大学 | Method for obtaining hardness and elastic modulus measurement values based on AFM nano indentation experiment |
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Application publication date: 20190614 |