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CN110095637A - The test method of atomic force microscope and sample surfaces property - Google Patents

The test method of atomic force microscope and sample surfaces property Download PDF

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Publication number
CN110095637A
CN110095637A CN201910381546.9A CN201910381546A CN110095637A CN 110095637 A CN110095637 A CN 110095637A CN 201910381546 A CN201910381546 A CN 201910381546A CN 110095637 A CN110095637 A CN 110095637A
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CN
China
Prior art keywords
signal
probe
cantilever beam
atomic force
force microscope
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CN201910381546.9A
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Chinese (zh)
Inventor
李鹏
裘晓辉
邵永健
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National Center for Nanosccience and Technology China
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National Center for Nanosccience and Technology China
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Priority to CN201910381546.9A priority Critical patent/CN110095637A/en
Publication of CN110095637A publication Critical patent/CN110095637A/en
Pending legal-status Critical Current

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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01QSCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
    • G01Q60/00Particular types of SPM [Scanning Probe Microscopy] or microscopes; Essential components thereof
    • G01Q60/24AFM [Atomic Force Microscopy] or apparatus therefor, e.g. AFM probes
    • G01Q60/32AC mode
    • G01Q60/34Tapping mode
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01QSCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
    • G01Q60/00Particular types of SPM [Scanning Probe Microscopy] or microscopes; Essential components thereof
    • G01Q60/24AFM [Atomic Force Microscopy] or apparatus therefor, e.g. AFM probes
    • G01Q60/38Probes, their manufacture, or their related instrumentation, e.g. holders
    • G01Q60/42Functionalisation

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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • Radiology & Medical Imaging (AREA)
  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Length Measuring Devices With Unspecified Measuring Means (AREA)

Abstract

The invention discloses a kind of atomic force microscope and the test methods of sample surfaces property.The atomic force microscope includes: signal generator, probe assembly, Z-direction piezoelectric ceramics, laser generator, photodetector, displacement coarse adjustment unit, controller and sample stage, wherein, probe assembly includes probe and excitation module, probe includes cantilever beam and the needle point positioned at cantilever beam first end, excitation module is connect with signal generator, for receiving pumping signal, and driving probe to deflect in a first direction under the action of pumping signal, excitation module is non-laser light thermal excitation module.Technical solution provided in an embodiment of the present invention, to effectively accelerate speed when testing surface nature to be measured using off-resonance tapping-mode, shortens the testing time on same surface to be measured so that the vibration frequency of probe greatly improves.

Description

The test method of atomic force microscope and sample surfaces property
Technical field
The present embodiments relate to surface nature measuring technology more particularly to a kind of atomic force microscope and sample surfaces The test method of matter.
Background technique
Atomic force microscope (Atomic Force Microscope, AFM) has high resolution and applied widely etc. Advantage is widely used in the important tool of micro-nano scale topography characterization, physical measurement and micro-nano operation.
Common imaging pattern specifically includes that contact mode, tapping-mode and off-resonance tapping-mode in AFM at present.Its Middle contact mode continues to contact with sample in imaging process middle probe, and biggish lateral force easily damages probe and sample; Tapping-mode vibrates at its resonant frequency in imaging process middle probe cantilever beam, probe and sample Intermittent Contact, though lateral force It so reduces, but directly power is not controlled, so that when soft sample is imaged, due to can not accurately carry out The control of power and sample may be damaged;Off-resonance tapping-mode is in imaging process middle probe cantilever beam lower than at its resonant frequency The active force of vibration, each period middle probe and sample room can be measured, and then can accurately be controlled the active force, and non- The relation curve that can get active force and distance under resonance tapping-mode, therefrom analyzes adhesion strength, deformation and the Young of sample The mechanical properties information such as modulus.
Fig. 1 is probe motion schematic diagram under off-resonance tapping-mode in the prior art.As shown in Figure 1, probe 101 passes through spy Needle folder 103 is connected on Z-direction piezoelectric ceramics 102, and in test process, Z-direction piezoelectric ceramics 102 is in the direction perpendicular to sample surfaces The upper back and forth movement of Z, driving Probe clip 103 and probe 101, back and forth movement, Fig. 1 are illustrated above-mentioned in this direction with dashed lines The position of back and forth movement process middle probe 101 and Z-direction piezoelectric ceramics 102, and probe 101 and Z are illustrated in a manner of solid line To the current location of piezoelectric ceramics 102.Since the weight of Probe clip 103 and probe 101 is larger so that drive this on the whole under Vibration is more difficult, so when leading to its test it vibration frequency it is lower, cannot achieve high speed test.
Summary of the invention
The present invention provides the test method of a kind of atomic force microscope and sample surfaces property, to effectively improve using non-total Vibration tapping-mode tests speed when surface topography to be measured.
In a first aspect, the embodiment of the invention provides a kind of atomic force microscope, which includes:
Signal generator, for generating simultaneously output drive signal and synchronization signal;
Probe assembly, the probe assembly include probe and excitation module, and the probe includes cantilever beam and is located at The needle point of the cantilever beam first end, the excitation module are connect with the signal generator, for receiving the pumping signal, And the probe is driven to deflect under the action of the pumping signal in a first direction, the first direction is perpendicular to table to be measured Face;
The second end of Z-direction piezoelectric ceramics, the cantilever beam is connect by Probe clip with the Z-direction piezoelectric ceramics, the Z-direction Piezoelectric ceramics for moving the probe in said first direction at the nanoscale;
Laser generator, for emitting laser to the cantilever beam;
Received optical signal for receiving the laser reflected from the cantilever beam, and is converted to telecommunications by photodetector Number;
It is displaced coarse adjustment unit, the displacement coarse adjustment unit is connect with the Z-direction piezoelectric ceramics, for Z-direction pressure described in coarse adjustment The position of electroceramics, with the position of coarse adjustment Probe clip and probe;
Controller, the controller and the signal generator, the photodetector, the position coarse adjustment unit and Z-direction piezoelectric ceramics connection, for obtaining background signal and live signal according to the electric signal, by the live signal with The difference signal of the background signal obtains the needle point according to the synchronization signal and the detection signal as detection signal Maximum interaction force with the surface to be measured is as peak force, using the peak force as feed back input, and judging It states feed back input and when preset value has difference, controls the position that the Z-direction piezoelectric ceramics adjusts the probe;
Sample stage, for carrying sample to be tested, the surface to be measured of the sample to be tested is towards the probe;
Wherein, the excitation module is non-laser light thermal excitation module.
Second aspect, the embodiment of the invention also provides a kind of test methods of sample surfaces property, using above-mentioned first Atomic force microscope described in aspect, the test method include:
Step 1, the controller adjust the position of the Z-direction piezoelectric ceramics by the displacement coarse adjustment unit, so that institute It states probe and is located at the surface to be measured;
Step 2, the signal generator generate the pumping signal and the synchronization signal, and by the pumping signal and The synchronization signal is transmitted separately to the excitation module and the controller;
Step 3, the excitation module motivate the cantilever beam in the first direction under the action of pumping signal Upper round-trip deflection;
The laser that step 4, the laser detector real-time reception are reflected from the cantilever beam, and multiple periodic signals are asked Be averaged after store into the controller as background signal, wherein the periodic signal is a synchronous signal cycle The optical signal received is carried out conversion acquisition for the laser detector by interior cantilever deflection signal, the cantilever deflection signal Electric signal;
Step 5 obtains pumping signal delay according to the cantilever deflection signal and the pumping signal, using the excitation Signal delay calibrates the synchronization signal;
Step 6, the controller control the position of the displacement coarse adjustment unit and the Z-direction piezoelectric ceramics to adjust probe Position so that the needle point approaches the surface to be measured;
The laser that step 7, the laser detector real-time reception are reflected from the cantilever beam, and optical signal is converted and is obtained Electric signal be transferred to the controller as the actual deflection signal of cantilever beam;
Step 8, the controller using the difference signal of the actual deflection signal and the background signal as detecting signal, And according to the detection signal and the synchronization signal, the maximum interaction on needle point and sample to be tested surface is obtained as peak value Power, and using the peak force as feed back input, the size relation of the feed back input and preset value is judged, if the feedback is defeated Enter to be greater than or equal to preset value, then skips to step 9, be otherwise back to above-mentioned steps 6;
Step 9, the sample to be tested surface horizontal grid shape traverse scanning, the controller is using the peak force as instead The position of Z-direction piezoelectric ceramics described in input control is presented, to obtain the three-dimensional appearance of sample and the relation curve of power and distance.
The probe assembly of atomic force microscope provided in an embodiment of the present invention includes probe and excitation module, and probe includes Cantilever beam and needle point positioned at cantilever beam first end, excitation module is connect with signal generator, for receiving pumping signal, and Probe is driven to deflect in a first direction under the action of pumping signal.Above-mentioned atomic force microscope can directly excitation quality compared with Light cantilever beam so that the vibration frequency of probe greatly improves, thus effectively accelerate using the test of off-resonance tapping-mode to Speed when surface nature is surveyed, the testing time on same surface to be measured is shortened.
Detailed description of the invention
In order to more clearly illustrate the technical scheme of the exemplary embodiment of the present invention, below to required in description embodiment The attached drawing to be used does a simple introduction.Obviously, the attached drawing introduced is present invention a part of the embodiment to be described Attached drawing, rather than whole attached drawings without creative efforts, may be used also for those of ordinary skill in the art To obtain other attached drawings according to these attached drawings.
Fig. 1 is probe motion schematic diagram under off-resonance tapping-mode in the prior art;
Fig. 2 is a kind of structural schematic diagram of atomic force microscope provided in an embodiment of the present invention;
Fig. 3 is probe motion schematic diagram under a kind of off-resonance tapping-mode provided in an embodiment of the present invention;
Fig. 4 is a kind of partial structural diagram of atomic force microscope provided in an embodiment of the present invention;
Fig. 5 is the partial structural diagram of another atomic force microscope provided in an embodiment of the present invention;
Fig. 6 is the partial structural diagram of another atomic force microscope provided in an embodiment of the present invention;
Fig. 7 is the partial structural diagram of another atomic force microscope provided in an embodiment of the present invention;
Fig. 8 is the partial structural diagram of another atomic force microscope provided in an embodiment of the present invention;
Fig. 9 is a kind of flow diagram of the test method of sample surfaces property provided in an embodiment of the present invention;
Figure 10 is one group of background signal, actual signal and the measured drawing for detecting signal provided in an embodiment of the present invention;
Figure 11 is a kind of distance change schematic diagram of the probe stress provided in an embodiment of the present invention with probe motion;
Figure 12 is the corresponding detection signal schematic representation in surface to be measured of unlike material provided in an embodiment of the present invention;
Figure 13 is a kind of shape appearance figure of sample being made of PS and LDPE material provided in an embodiment of the present invention;
Figure 14 is the adhesion strength measured drawing on surface to be measured corresponding with Figure 13.
Specific embodiment
It is of the invention to reach the technical means and efficacy that predetermined goal of the invention is taken further to illustrate, below in conjunction with Attached drawing and preferred embodiment, to the test method of a kind of atomic force microscope proposed according to the present invention and sample surfaces property Specific embodiment, structure, feature and its effect, detailed description is as follows.
The embodiment of the invention provides a kind of atomic force microscope, which includes:
Signal generator, for generating simultaneously output drive signal and synchronization signal;
Probe assembly, the probe assembly include probe and excitation module, and the probe includes cantilever beam and is located at The needle point of the cantilever beam first end, the excitation module are connect with the signal generator, for receiving the pumping signal, And the probe is driven to deflect under the action of the pumping signal in a first direction, the first direction is perpendicular to table to be measured Face;
The second end of Z-direction piezoelectric ceramics, the cantilever beam is connect by Probe clip with the Z-direction piezoelectric ceramics, the Z-direction Piezoelectric ceramics for moving the probe in said first direction at the nanoscale;
Laser generator, for emitting laser to the cantilever beam;
Received optical signal for receiving the laser reflected from the cantilever beam, and is converted to telecommunications by photodetector Number;
It is displaced coarse adjustment unit, the displacement coarse adjustment unit is connect with the Z-direction piezoelectric ceramics, for Z-direction pressure described in coarse adjustment The position of electroceramics, with the position of coarse adjustment Probe clip and probe;
Controller, the controller and the signal generator, the photodetector, the position coarse adjustment unit and Z-direction piezoelectric ceramics connection, for obtaining background signal and live signal according to the electric signal, by the live signal with The difference signal of the background signal obtains the needle point according to the synchronization signal and the detection signal as detection signal Maximum interaction force with the surface to be measured is as peak force, using the peak force as feed back input, and judging It states feed back input and when preset value has difference, controls the position that the Z-direction piezoelectric ceramics adjusts the probe;
Sample stage, for carrying sample to be tested, the surface to be measured of the sample to be tested is towards the probe;
Wherein, the driver unit is non-laser light thermal excitation component.
The probe assembly of atomic force microscope provided in an embodiment of the present invention includes probe and excitation module, and probe includes Cantilever beam and needle point positioned at cantilever beam first end, excitation module is connect with signal generator, for receiving pumping signal, and Probe is driven to deflect in a first direction under the action of pumping signal.Above-mentioned atomic force microscope can directly excitation quality compared with Light cantilever beam so that the vibration frequency of probe greatly improves, thus effectively accelerate using the test of off-resonance tapping-mode to Speed when surface nature is surveyed, the testing time on same surface to be measured is shortened.
It is the core concept of the application above, following will be combined with the drawings in the embodiments of the present invention, to the embodiment of the present invention In technical solution be clearly and completely described, it is clear that described embodiments are only a part of the embodiments of the present invention, Instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not making creative labor Under the premise of dynamic, every other embodiment obtained be shall fall within the protection scope of the present invention.
In the following description, numerous specific details are set forth in order to facilitate a full understanding of the present invention, but the present invention can be with Implemented using other than the one described here other embodiments, those skilled in the art can be without prejudice in the present invention Similar popularization is done in the case where culvert, therefore the present invention is not limited by the specific embodiments disclosed below.
Secondly, combination schematic diagram of the present invention is described in detail, when describing the embodiments of the present invention, for purposes of illustration only, table The schematic diagram of showing device device architecture not makees partial enlargement according to general proportion, and the schematic diagram is example, This should not limit the scope of protection of the invention.In addition, the three-dimensional space of length, width and height should be included in actual fabrication Size.
Fig. 2 is a kind of structural schematic diagram of atomic force microscope provided in an embodiment of the present invention.The atomic force microscope is suitable For the test of solid structure surface nature, test pattern includes at least off-resonance tapping-mode, and the application is mainly for above-mentioned Test pattern.As shown in Fig. 2, atomic force microscope include signal generator 700, probe assembly 800, Z-direction piezoelectric ceramics 600, Laser generator 300, photodetector 200, displacement coarse adjustment unit 500, controller 100 and sample stage 900.
Wherein, signal generator 700 includes visiting for generating simultaneously output drive signal and synchronization signal, probe assembly 800 Needle 830 and excitation module 810, probe 830 include cantilever beam 831 and the needle point 832 positioned at 831 first end of cantilever beam, are swashed It encourages module 810 to connect with signal generator 700, for receiving pumping signal, and drives probe 830 under the action of pumping signal It is deflected on Z in a first direction, first direction Z is perpendicular to surface to be measured, and excitation module 810 is non-laser light thermal excitation module. The second end of cantilever beam 831 is connect by Probe clip with Z-direction piezoelectric ceramics 600, and laser generator 300 is used for cantilever beam 831 Emit laser, photodetector 200 is used to receive the laser reflected from cantilever beam 831, and received optical signal is converted to electricity Signal, displacement coarse adjustment unit 500 are connect with Z-direction piezoelectric ceramics 600, the position for coarse adjustment Z-direction piezoelectric ceramics 600.Controller 100 connect with signal generator 700, photodetector 200, position coarse adjustment unit 500 and Z-direction piezoelectric ceramics 600, are used for root Background signal and live signal are obtained according to electric signal, using the difference signal of live signal and background signal as detecting signal, according to Synchronization signal and detection signal obtain the maximum interaction force on needle point 832 and surface to be measured as peak force, by peak value masterpiece For feed back input, and when judging that feed back input and preset value have difference, control Z-direction piezoelectric ceramics 600 adjusts the position of probe 830 It sets, sample stage 900 is for carrying sample to be tested, and the surface to be measured of sample to be tested is towards probe 830.
Fig. 3 is probe motion schematic diagram under a kind of off-resonance tapping-mode provided in an embodiment of the present invention.As shown in figure 3, In test process, the round-trip deflection of the Z in a first direction of probe 830, and the position of Z-direction piezoelectric ceramics 600 is fixed, 830 matter of probe Amount is smaller, and relative to mode in the prior art shown in Fig. 1, the vibration of mode middle probe shown in Fig. 3 830 easily reaches very high Frequency, and then effectively promote sweep test speed.
Fig. 4 is a kind of partial structural diagram of atomic force microscope provided in an embodiment of the present invention.Fig. 4 illustrates original Photodetector 200, laser generator 300, probe 830, Z-direction piezoelectric ceramics 600 and sample stage in sub- force microscope 900.As shown in figure 4, one far from sample to be tested in probe 830 can be set in photodetector 200 and laser generator 300 Side, it is to be understood that all setting positions for meeting the photodetector 200 and laser generator 300 that require as follows exist In the protection scope of the present embodiment: in 830 deflection process of probe, the laser that laser generator 300 issues can be exposed to On cantilever beam 831, and it can be received from the laser that cantilever beam 831 reflects by photodetector 200.
It should be noted that the output valve on the direction photodetector 200Y changes, photoelectricity when probe 830 deflects Detector 200 converts optical signals to electric signal transmission to controller.It is worth noting that, the excitation letter that signal generator generates It number is usually sinusoidal signal, and then driver unit drives probe 830 Z is upper in a first direction and deflects back and forth, so that photodetector 200 electric signals generated are also sinusoidal signal, and the period is identical as pumping signal and synchronization signal.
It should also be noted that, during actual test, Z is upper in a first direction deflects back and forth for probe 830, and towards sample Contacted when product side deflects near maximum angle with surface to be measured, when above-mentioned contact, photodetector 200 detect first Signal includes that the second signal that needle point 832 and surface contact force to be measured generate and the third that probe 830 itself deflection generates are believed Number, but judge to use when whether needle point 832 damages sample to be tested surface is only second signal, therefore be so that accuracy of judgement, Third signal in first signal need to be removed.Probe 830 back and forth deflection and when needle point 832 and contactless surface to be measured, can be obtained Single third signal, probe deflected at surface remote position to be measured multiple periods sum again be averaged it is available Third signal then approaches in surface process to be measured in probe, can believe the signal and third that photodetector real-time detection arrives Number difference signal as detection signal, at this time detect signal only include above-mentioned second signal.And what photodetector 200 generated Electric signal relationship proportional to active force.Therefore corresponding peak can be obtained by the signal parameter of the peak position of second signal It is worth power, i.e. active force of the signal between the peak value moment needle point 832 and surface to be measured.It is worth noting that, second signal packet Include delay etc. and increase peak position and judge the disturbing factor of difficulty, and the peak value of second signal with synchronization signal be it is corresponding, Therefore the position that synchronization signal accurately finds peak value in second signal can be used.
In the present embodiment, displacement coarse adjustment unit adjusts the position of Z-direction piezoelectric ceramics 600 under millimeter to micro-meter scale, And then drive the position for adjusting probe 830.Needle point 832 apart from surface to be measured farther out when, can be used displacement coarse adjustment unit to spy The position of needle 830 is adjusted, and when needle point 832 is closer apart from surface to be measured, the displacement to avoid needle point 832 excessive leads to needle Point 832, to bump against compared with noticeable effort, damages probe 830 with surface to be measured, needs to make the mobile lesser displacement of needle point 832, at this time Z-direction piezoelectric ceramics 600 can be used the position of probe 830 is adjusted.
Excitation module 810 is non-laser light thermal excitation module in the present embodiment, avoids the laser of relatively high power to sample The phenomenon that heating and damaging sample, to expand the application range of atomic force microscope.In addition, the present embodiment is to sharp Encourage the specific structure of module 810 without limitation, it is all can excitation probe 830 structure of back and forth movement is equal on Z in a first direction In the protection scope of the present embodiment.
The probe assembly 800 of atomic force microscope provided in this embodiment includes probe 830 and excitation module 810, is visited Needle includes cantilever beam 831 and the needle point 832 positioned at 831 first end of cantilever beam, and excitation module 810 and signal generator 700 connect It connects, drives probe 830 to deflect in a first direction for receiving pumping signal, and under the action of pumping signal.Above-mentioned atom Force microscope is capable of the cantilever beam 831 of directly excitation lighter weight, so that the vibration frequency of probe 830 greatly improves, to have Effect accelerates speed when testing surface nature to be measured using off-resonance tapping-mode, when shortening the test on same surface to be measured Between.
Optionally, signal generator can be for external signal generator or by the digital-analog convertor group in controller At built-in signal generator.
It should be noted that the controller in atomic force microscope in the present embodiment can use digital-to-analog conversion Device realizes the function of signal generator, for generating the signals such as pumping signal and synchronization signal.
Preferably, signal generator can be external signal generator, to reach the beneficial effect for the burden for mitigating controller Fruit.
Fig. 5 is the partial structural diagram of another atomic force microscope provided in an embodiment of the present invention.Knot shown in Fig. 4 On the basis of structure, Fig. 5 further illustrates excitation module.As shown in figure 5, excitation module 810 may include functional film layer 820 With driver unit 840, functional film layer 820 is located on cantilever beam 831, and driver unit 840 is connect with signal generator 700.
Illustratively, the material of functional film layer 820 can be piezoelectric material.
Optionally, piezoelectric material can be zinc oxide.It is understood that piezoelectric material can also be its outside zinc oxide His piezoelectric material, the present embodiment are not especially limited this.
Correspondingly, driver unit 810 may include positive electrode 841 and negative electrode 842, positive electrode 841 with continued reference to Fig. 5 It is electrically connected with functional film layer 820 with negative electrode 842, and is electrically connected the output end of the pumping signal of signal generator 700.
It should be noted that positive/negative voltage signal is applied in functional film layer 820 by positive electrode 841 and negative electrode 842, So that functional film layer 820 is excited, deformation occurs, and then probe 830 is driven to deflect.
Illustratively, the material of functional film layer 820 may be conductive material.
The present embodiment to formed functional film layer 820 conductive material specific type without limitation, all conductive materials are equal In the protection scope of the present embodiment.
Correspondingly, Fig. 6 is the partial structural diagram of another atomic force microscope provided in an embodiment of the present invention.Fig. 6 Shown structure is similar to structure shown in Fig. 5, unlike, in Fig. 6 driver unit 810 include excitation electrode, excitation electrode with The setting of 820 relative spacing of functional film layer, the output end of the pumping signal of excitation electrode electrical connection signal generator 700.
It should be noted that excitation electrode and functional film layer 820 apply varying voltage signal, there is phase interaction between the two Firmly, when motivating the voltage change on electrode, under the action of above-mentioned effect, functional film layer 820 drives probe 830 to make correspondence Yaw motion.
Illustratively, the material of driver unit 810 can also be magnetic material.
The present embodiment to formed functional film layer 820 magnetic material specific type without limitation, all magnetic materials are equal In the protection scope of the present embodiment.
Correspondingly, Fig. 7 is the partial structural diagram of another atomic force microscope provided in an embodiment of the present invention.Fig. 7 Shown structure is similar to structure shown in Fig. 5, unlike, driver unit 810 includes excitation coil in Fig. 7, excitation coil Central axes are electrically connected the output end of the pumping signal of signal generator 700 perpendicular to surface to be measured, excitation coil.
It should be noted that excitation coil generates magnetic field under the action of pumping signal, functional film layer 820 is in above-mentioned magnetic field Round-trip deflection on Z in a first direction under effect, drives probe 830 Z is upper in a first direction and deflect back and forth.
Optionally, atomic force microscope can also include host computer, and host computer is connect with controller.Host computer for realizing Integration of user interaction functionality allows users to the working condition by PC control atomic force microscope, and can pass through interface Observe test image.
Fig. 8 is the partial structural diagram of another atomic force microscope provided in an embodiment of the present invention.Knot shown in Fig. 4 On the basis of structure, Fig. 8 further illustrates excitation module.As shown in figure 8, excitation module 810 is heating wire, heating wire is located at On cantilever beam 831, heating wire 810 is electrically connected the output end of the pumping signal of signal photophore 700.
It should be noted that heating wire is directly contacted with cantilever beam 831, when the pumping signal that signal generator 700 issues When being applied on heating wire, 831 expanded by heating of cantilever beam, with being moved on probe 830 in a first direction Z.
Fig. 9 is a kind of flow diagram of the test method of sample surfaces property provided in an embodiment of the present invention.The test Method is applied to the atomic force microscope that any embodiment of that present invention provides, and the test method of the sample surfaces property is specifically wrapped It includes as follows:
Step 1, controller adjust the position of Z-direction piezoelectric ceramics by displacement coarse adjustment unit, so that probe is located at table to be measured Above face.
Illustratively, the distance between probe and surface to be measured can be several microns, such as 1~3 micron.This hour hand Sharp larger with the distance between surface to be measured, the round-trip deflection of probe in a first direction will not make needle point connect with surface to be measured Touching.
Step 2, signal generator generate pumping signal and synchronization signal, and pumping signal and synchronization signal are transmitted respectively To excitation module and controller.
Significantly, since the application is directed to off-resonance tapping-mode, therefore, need so that probe is far from its resonance It is vibrated at frequency.
It is understood that pumping signal is identical as the period of synchronization signal, illustratively, pumping signal can be sine Signal, for example, pumping signal can be AC signal, synchronization signal can be pulse signal.
Under the action of pumping signal, excitation cantilever arm beam deflects back and forth in a first direction for step 3, excitation module.
It is understood that since the distance between probe and surface to be measured are farther out, as above, usually several micro- at this time Rice, therefore, needle point will not be contacted with surface to be measured in the deflection process of probe.
The laser that step 4, laser detector real-time reception are reflected from cantilever beam, and the summation of multiple periodic signals is averaged It storing afterwards as background signal into controller, wherein periodic signal is the cantilever deflection signal in a synchronous signal cycle, Cantilever deflection signal is the electric signal that the optical signal received is carried out conversion acquisition by laser detector.
It is understood that the third signal referred in above content is background signal, related description can be found in above-mentioned Related content, details are not described herein again.
Step 5 obtains pumping signal delay according to cantilever deflection signal and pumping signal, postpones to calibrate using pumping signal Synchronization signal.
It should be noted that probe has certain quality, and signal transmission needs the regular hour, and above-mentioned factor is led It causes when detecting cantilever beam deflection, the signal that photodetector detects has delay relative to pumping signal, subsequent based on excitation The synchronization signal that signal determines has error, and then error even mistake can therefore occurs during finding peak position, Therefore the signal acquisition amount of delay first detected according to pumping signal and photodetector before being operated is based on the delay Amount calibration synchronization signal, detected in the synchronization signal that actually uses.
The position of step 6, controller command displacement coarse adjustment unit and Z-direction piezoelectric ceramics adjusts the position of probe, so that Needle point approaches surface to be measured.
The laser that step 7, laser detector real-time reception are reflected from cantilever beam, and the electric signal that optical signal conversion is obtained Actual deflection signal as cantilever beam is transferred to controller.
It is understood that the first signal referred in above content is actual signal, related description can be found in above-mentioned Related content, details are not described herein again.
Step 8, controller are believed using the difference signal of actual deflection signal and background signal as detection signal according to detection Number and synchronization signal, obtain the maximum interaction on needle point and sample to be tested surface as peak force, and using peak force as instead Feedback input, judges the size relation of feed back input and preset value, if feed back input is greater than or equal to preset value, skips to step 9, Otherwise above-mentioned steps 6 are back to.
Illustratively, Figure 10 is one group of background signal, actual signal and detection signal provided in an embodiment of the present invention Measured drawing.Each schematic diagram in Figure 10 obtains under the cantilever beam vibration frequency of 10kHz.As shown in Figure 10, it is located at Figure 10 most The signal schematic representation of upside is the measured drawing of background signal, is located in the middle the measured drawing that signal schematic representation is actual signal, position Signal schematic representation in the lower side Figure 10 is the measured drawing for detecting signal.
Optionally, preset value can contact between needle point and surface to be measured, but when contact force will not damage surface to be measured Active force.Specifically, controlling probe towards to be measured by Z-direction piezoelectric ceramics when controller judges that peak force is less than preset value Apparent motion when controller judges that peak force is greater than preset value, leads to so that the active force between needle point and surface to be measured increases Z-direction piezoelectric ceramics control probe is crossed away from apparent motion to be measured, so that the active force between needle point and surface to be measured reduces, into And can be to the close of pre set force, eventually equal to pre set force.
Step 9, sample to be tested surface horizontal grid shape traverse scanning, controller control Z using peak force as feed back input To the position of piezoelectric ceramics, to obtain the three-dimensional appearance of sample and the relation curve of power and distance.
Technical solution provided in this embodiment drives probe to deflect in a first direction by excitation module, and by swashing Deflection detection is realized in light device and photodetector cooperation, and obtaining needle point and surface to be measured in deflection process respectively, there is no when contacting Background signal and deflection process in needle point approach the live actual signal in surface process to be measured, by actual signal and back The difference signal of scape signal is obtaining peak force according to detection signal, is comparing the size of peak force and preset value as detection signal Relationship, and adjusted according to comparison result and probe location or be scanned test, enables atomic force microscope directly excitation matter Lighter cantilever beam is measured, so that the vibration frequency of probe greatly improves, is surveyed to effectively accelerate using off-resonance tapping-mode Speed when surface nature to be measured is tried, the testing time on same surface to be measured is shortened.
It illustratively provides and is obtained using atomic force microscope provided by the present application and surface topography test method below Testing result.Specifically, Figure 11 is that a kind of probe stress provided in an embodiment of the present invention is shown with the distance change of probe motion It is intended to.Figure 11 illustrates above-mentioned variation schematic diagram of the probe in surface process to be measured with dotted line, and illustrates spy with solid line Needle has been specifically identified out peak force and adhesion strength far from the above-mentioned variation schematic diagram in surface process to be measured.Figure 12 is this hair The corresponding detection signal schematic representation in surface to be measured for the unlike material that bright embodiment provides.Illustrated in Figure 12 PS material and The corresponding above-mentioned detection signal schematic representation in the surface to be measured of LDPE material, wherein dotted line corresponds to PS material, and solid line corresponds to LDPE material Matter.Figure 13 is a kind of shape appearance figure of sample being made of PS and LDPE material provided in an embodiment of the present invention.Figure 14 is and Figure 13 The adhesion strength measured drawing on corresponding surface to be measured.Figure 13 and Figure 14 is swept in the row of the cantilever beam vibration frequency of 5KHz and 5.5Hz Retouch the test result that frequency down-sweep imaging obtains.
Note that the above is only a better embodiment of the present invention and the applied technical principle.It will be appreciated by those skilled in the art that The invention is not limited to the specific embodiments described herein, be able to carry out for a person skilled in the art it is various it is apparent variation, It readjusts and substitutes without departing from protection scope of the present invention.Therefore, although being carried out by above embodiments to the present invention It is described in further detail, but the present invention is not limited to the above embodiments only, without departing from the inventive concept, also It may include more other equivalent embodiments, and the scope of the invention is determined by the scope of the appended claims.

Claims (11)

1. a kind of atomic force microscope characterized by comprising
Signal generator, for generating simultaneously output drive signal and synchronization signal;
Probe assembly, the probe assembly include probe and excitation module, and the probe includes cantilever beam and is located at described The needle point of cantilever beam first end, the excitation module are connect with the signal generator, for receiving the pumping signal, and The probe is driven to deflect under the action of the pumping signal in a first direction, the first direction is perpendicular to surface to be measured;
The second end of Z-direction piezoelectric ceramics, the cantilever beam is connect by Probe clip with the Z-direction piezoelectric ceramics, the Z-direction piezoelectricity Ceramics for moving the probe in said first direction at the nanoscale;
Laser generator, for emitting laser to the cantilever beam;
Received optical signal for receiving the laser reflected from the cantilever beam, and is converted to electric signal by photodetector;
It is displaced coarse adjustment unit, the displacement coarse adjustment unit is connect with the Z-direction piezoelectric ceramics, for the pottery of Z-direction piezoelectricity described in coarse adjustment The position of porcelain, with the position of coarse adjustment Probe clip and probe;
Controller, the controller and the signal generator, the photodetector, the position coarse adjustment unit and described The connection of Z-direction piezoelectric ceramics, for obtaining background signal and live signal according to the electric signal, by the live signal with it is described The difference signal of background signal obtains the needle point and institute according to the synchronization signal and the detection signal as detection signal The maximum interaction force on surface to be measured is stated as peak force, using the peak force as feed back input, and judge it is described anti- When feedback input and preset value have difference, the position that the Z-direction piezoelectric ceramics adjusts the probe is controlled;
Sample stage, for carrying sample to be tested, the surface to be measured of the sample to be tested is towards the probe;
Wherein, the excitation module is non-laser light thermal excitation module.
2. atomic force microscope according to claim 1, which is characterized in that the signal generator is external signal Device or the built-in signal generator being made of the digital-analog convertor in the controller.
3. atomic force microscope according to claim 1, which is characterized in that the excitation module includes functional film layer and swashs Component is encouraged, the functional film layer is located on the cantilever beam, and the driver unit is connect with the signal generator.
4. atomic force microscope according to claim 3, which is characterized in that the material of the functional film layer is piezoresistive material Material.
5. atomic force microscope according to claim 4, which is characterized in that the driver unit includes positive electrode and negative electricity Pole, the positive electrode and the negative electrode are electrically connected with the functional film layer, and are electrically connected swashing for the signal generator Encourage the output end of signal.
6. atomic force microscope according to claim 3, which is characterized in that the material of the functional film layer is conduction material Material.
7. atomic force microscope according to claim 6, which is characterized in that the driver unit includes excitation electrode, institute It states excitation electrode and the functional film layer relative spacing is arranged, the excitation electrode is electrically connected the excitation letter of the signal generator Number output end.
8. atomic force microscope according to claim 3, which is characterized in that the material of the functional film layer is magnetic material Material.
9. atomic force microscope according to claim 8, which is characterized in that the driver unit includes excitation coil, institute The central axes of excitation coil are stated perpendicular to the surface to be measured, the excitation coil is electrically connected the excitation letter of the signal generator Number output end.
10. atomic force microscope according to claim 1, which is characterized in that the excitation module is heating wire, the electricity Heated filament is located on the cantilever beam, and the heating wire is electrically connected the output end of the pumping signal of the signal photophore.
11. a kind of test method of sample surfaces property is applied to the described in any item atomic force microscope of claim 1-10, It is characterised by comprising:
Step 1, the controller adjust the position of the Z-direction piezoelectric ceramics by the displacement coarse adjustment unit, so that the spy Needle is located at the surface to be measured;
Step 2, the signal generator generate the pumping signal and the synchronization signal, and by the pumping signal and described Synchronization signal is transmitted separately to the excitation module and the controller;
Step 3, the excitation module motivate the cantilever beam past in said first direction under the action of the pumping signal Return deflection;
The laser that step 4, the laser detector real-time reception are reflected from the cantilever beam, and the summation of multiple periodic signals is taken It is stored as background signal into the controller after average, wherein the periodic signal is in a synchronous signal cycle Cantilever deflection signal, the cantilever deflection signal are the electricity that the optical signal received is carried out conversion acquisition by the laser detector Signal;
Step 5 obtains pumping signal delay according to the cantilever deflection signal and the pumping signal, using the pumping signal The synchronization signal is calibrated in delay;
Step 6, the controller control the position of the displacement coarse adjustment unit and the Z-direction piezoelectric ceramics to adjust the position of probe It sets, so that the needle point approaches the surface to be measured;
The laser that step 7, the laser detector real-time reception are reflected from the cantilever beam, and the electricity that optical signal conversion is obtained Signal is transferred to the controller as the actual deflection signal of cantilever beam;
Step 8, the controller are using the difference signal of the actual deflection signal and the background signal as detecting signal, and root According to the detection signal and the synchronization signal, the maximum interaction for obtaining needle point and sample to be tested surface is used as peak force, And using the peak force as feed back input, the size relation of the feed back input and preset value is judged, if the feed back input More than or equal to preset value, then step 9 is skipped to, is otherwise back to above-mentioned steps 6;
Step 9, the sample to be tested surface horizontal grid shape traverse scanning, the controller are defeated using the peak force as feeding back Enter the position for controlling the Z-direction piezoelectric ceramics, to obtain the three-dimensional appearance of sample and the relation curve of power and distance.
CN201910381546.9A 2019-05-08 2019-05-08 The test method of atomic force microscope and sample surfaces property Pending CN110095637A (en)

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