CN106645808A - Kelvin probe force microscope synchronously measuring multiple parameters - Google Patents

Kelvin probe force microscope synchronously measuring multiple parameters Download PDF

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CN106645808A
CN106645808A CN201710093420.2A CN201710093420A CN106645808A CN 106645808 A CN106645808 A CN 106645808A CN 201710093420 A CN201710093420 A CN 201710093420A CN 106645808 A CN106645808 A CN 106645808A
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probe
sample
conducting probe
signal
conducting
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CN106645808B (en
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谢晖
张号
孟祥和
宋健民
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Harbin Institute of Technology
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Harbin Institute of Technology
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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
    • G01Q60/30—Scanning potential microscopy

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Abstract

The invention discloses a Kelvin probe force microscope synchronously measuring multiple parameters and relates to a Kelvin probe force microscope. The invention aims to solve the problem that surface appearance, mechanical property and surface local potential of a sample cannot be synchronously represented by using a conventional Kelvin probe force microscope. In the invention, a direct current power supply is used for generating a direct current signal and loads the same between a conductive probe and the sample, a signal generator generates three-path same signals, the frequency of which is the same as a second order resonant frequency of the conductive probe, and the first-path signal is overlaid with a signal generated by an arbitrary waveform generator for controlling a #3 piezoelectric controller, so that the #3 piezoelectric controller drives a piezoelectric ceramic on a probe hand; the second-path signal as a reference signal is sent to a lock phase amplifier; the third-path signal which is shifted by 90 degrees by a phase shifter is loaded between the conductive probe and the sample; and a signal output by the lock phase amplifier is sent to an upper computer. The Kelvin probe force microscope disclosed by the invention is suitable for measuring the surface appearance, the mechanical properties and the surface local potential of the sample.

Description

A kind of Kelvin probe force microscopy of multiparameter synchro measure
Technical field
The present invention relates to Kelvin probe force microscopy.
Background technology
Kelvin probe force microscopy (Kelvin Probe Force Microscopy, KPFM) is that scanning probe is micro- A member in mirror (Scanning probe microscopy, SPM) family, it is by Kelvin probe technology and atomic force microscopy Mirror (Atomic force microscopy, AFM) is combined, and realizes the sign of sample surfaces local potential.Traditional Kelvin Probe force microscopy can realize surface topography, mechanical characteristic and the surface local potential of sample by different measuring methods Characterize.For example " lifting pattern (lift-up mode) " can obtain the surface topography and local electricity of sample by twice sweep Gesture, " resonance mode (tapping mode) " can simultaneously obtain surface topography and the local potential of sample by single pass, And " peak value force mode (peak force mode) " is a kind of discontinuous connection pattern, twice sweep is carried out per line during scanning, first Scanning obtains the surface topography and mechanical characteristic of sample, then utilizes " lifting pattern " to scan the surface office for obtaining sample second Portion's potential.Although existing method can realize the sign of sample surface morphology, mechanical characteristic and surface local potential, not The synchronous sign of these parameters can be realized, that is to say, that surface topography, mechanics that single pass obtains sample simultaneously can not be passed through Characteristic and surface local potential.
The content of the invention
Mechanical characteristic and surface local potential for understand the function of microelectronic component, microbial activity and many machines- Electricity and biological phenomenon are very important, and many measurements have ageing and machine-electromechanical coupling characteristic.In addition, probe and sample Contact potential difference between product will cause error to the measurement of sample surface morphology.Therefore, at the same the surface topography of measuring samples, Mechanical characteristic and surface local potential are significantly.In view of traditional Kelvin probe force microscopy cannot realize sample Surface topography, the synchronous sign of mechanical characteristic and surface local potential, the invention provides a kind of multiparameter synchro measure Kelvin probe force microscopy.
A kind of Kelvin probe force microscopy of multiparameter synchro measure of the present invention include XY microns positioning table 12, XYZ nanometer positionings platform 13, Kelvin scanning sample stage 15, XYZ microns positioning table 8, one-dimensional wide range adjustment microfluidic platform 10, probe Handss support 9, probe handss 7, host computer, DC source, Arbitrary Waveform Generator, capture card, signal generator, phase shifter, lock are mutually put Big device, four-quadrant position detector, semiconductor laser generator, a piezo controller, No. two piezo controllers and No. three pressures Electric controller；
Kelvin's scanning sample stage 15 is fixed on XYZ nanometer positionings platform 13, and XYZ nanometer positionings platform 13 is fixed on XY microns On positioning table 12；Conducting probe 7-4 is installed on probe handss 7 and conducting probe 7-4 vertically i.e. Z-direction shiftings can be driven Dynamic piezoelectric ceramics 7-2, probe handss 7 are fixed on probe handss support 9, and probe handss support 9 is fixed on XYZ microns positioning table 8, XYZ microns positioning table 8 is fixed on one-dimensional wide range adjustment microfluidic platform 10；
Host computer is by the piezoelectric ceramics movement on piezo controller driving Kelvin's scanning sample stage 15, by two Number piezo controller drives piezoelectric ceramics movement on XYZ nanometer positionings platform 13, drives probe handss 7 by No. three piezo controllers On piezoelectric ceramics movement；
To conducting probe 7-4, what Jing conducting probes 7-4 reflected swashs the laser light incident that semiconductor laser generator 18 is produced Light is incident to four-quadrant position detector 4；
The detectable signal of four-quadrant position detector 4 is sent to host computer by capture card, and the detectable signal is also as anti- Feedback signal is sent to lock-in amplifier；
DC source is used to produce direct current signal under the control of host computer, and the direct current signal is loaded into into conducting probe Between 7-4 and sample 15-8；
Signal generator produces three tunnel identical signals (the second-order resonance frequency phase of the signal frequency and conducting probe 7-4 Together), for controlling No. three piezo controllers after the first via is superimposed with the logical adder of the signal that Arbitrary Waveform Generator is produced, No. three are made Piezo controller drives the piezoelectric ceramics 7-2 on probe handss 7；Second tunnel is sent to lock-in amplifier as reference signal；3rd Road is loaded between conducting probe 7-4 and sample 15-8 after 90 degree of phase shifter phase shift；
The signal of lock-in amplifier output is sent to host computer by capture card.
Advantages below of the present invention：1st, breaching traditional KPFM cannot synchronously characterize to the mechanical characteristic of sample and local potential The characteristics of, realize the same pacing of the surface topography, mechanical characteristic and local electric potential difference in the case of single pass to sample Amount；2nd, the Kelvin probe force microscopy device of multiparameter synchro measure, makes AFM can be used for the measuring multiple parameters of sample surfaces, Including pattern, mechanical characteristic and local potential；3rd, the Kelvin probe force microscopy device of multiparameter synchro measure be into One step realizes that the measuring multiple parameters to test object is expanded and provide technical foundation (such as conductivity, resistivity).Open with traditional You compare literary probe force microscopy, and the method can meet the requirement of the ageing and Multi-parameter coupling characteristic in measurement, and mend The error that electrostatic force is caused to topography measurement is repaid, has been had in nanometer manufacture, test, characteristic present and biological field higher Availability and operability, with very high practical value.
Description of the drawings
Fig. 1 is the principle schematic of the Kelvin probe force microscopy described in embodiment one, wherein 21 swash for quasiconductor Optical generator, 22 is four-quadrant position detector,
Fig. 2 be the drive signal that No. three piezo controllers drive piezoelectric ceramics 7-2 on probe handss 7 in embodiment one, The oscillogram of force feedback signal and phase-feedback signal, drive signal is in integrally gaussian-shape, and the sinusoidal wave form of laminated thereto is Um；
Fig. 3 is the structural representation of the mechanical part of the Kelvin probe force microscopy described in embodiment one, wherein,
1：Frame；2：Four-quadrant position detector two-dimension adjustment microfluidic platform；3：One-dimensional adjustment microfluidic platform I；4：Four-quadrant is spacing Put detector；5：Reflection laser convex lenss；6：Laser mirror；7：Probe handss；8：XYZ micron positioning tables；9：Probe handss support； 10：One-dimensional wide range adjusts microfluidic platform；11：Table top；12：XY micron positioning tables；13：XYZ nanometer positioning platforms；14：Sample stage Frame；15：Kelvin scans sample stage；16：Incident laser focuses on convex lenss；17：One-dimensional adjustment microfluidic platform II；18：Quasiconductor swashs Optical generator；19：Laser generator angle-adjusting mechanism；20：Optical microscope；
Fig. 4 is the structural representation of the middle probe handss of embodiment one, wherein, 7-1：Probe handss pedestal；7-2：Piezoelectric ceramics； 7-3：Probe support；7-4：Conducting probe；7-5：Shielding piece；7-6：Conducting probe fixed plate；7-7：Binding post；
Fig. 5 is the structural representation that Kelvin scans sample stage in embodiment one, wherein, (a) scan sample for Kelvin The front view of sample platform, is (b) top view of (a)；15-1：Kelvin scans sample sewing platform base；15-2：Piezoelectric ceramics；15-3：Sample Product seat；15-4：Connecting line；15-5：Screw；15-6：Bunch block；15-7：Copper tabletting；15-8：Sample；15-9：Insulation is solid Determine screw；
Fig. 6 is the measurement result of polystyrene/light binding grating in embodiment two.
Specific embodiment
Specific embodiment one：Present embodiment, the same pacing of a kind of multiparameter described in present embodiment are illustrated with reference to Fig. 1 The Kelvin probe force microscopy of amount, including XY microns positioning table 12, XYZ nanometer positionings platform 13, Kelvin scanning sample stage 15, XYZ microns positioning table 8, one-dimensional wide range adjustment microfluidic platform 10, probe handss support 9, probe handss 7, host computer, DC source, appoint Meaning wave producer, capture card, signal generator, phase shifter, lock-in amplifier, four-quadrant position detector, semiconductor laser are sent out Raw device, piezo controller, No. two piezo controllers and No. three piezo controllers；
Kelvin's scanning sample stage 15 is fixed on XYZ nanometer positionings platform 13, and XYZ nanometer positionings platform 13 is fixed on XY microns On positioning table 12；Conducting probe 7-4 is installed on probe handss 7 and conducting probe 7-4 vertically i.e. Z-direction shiftings can be driven Dynamic piezoelectric ceramics 7-2, probe handss 7 are fixed on probe handss support 9, and probe handss support 9 is fixed on XYZ microns positioning table 8, XYZ microns positioning table 8 is fixed on one-dimensional wide range adjustment microfluidic platform 10；
Host computer is by the piezoelectric ceramics movement on piezo controller driving Kelvin's scanning sample stage 15, by two Number piezo controller drives piezoelectric ceramics movement on XYZ nanometer positionings platform 13, drives probe handss 7 by No. three piezo controllers On piezoelectric ceramics 7-2 movement；
The generator of semiconductor laser 18 produce laser light incident to conducting probe 7-4, Jing conducting probes 7-4 reflection Laser light incident is to four-quadrant position detector 4；
The detectable signal of four-quadrant position detector 4 is sent to host computer by capture card, and the detectable signal is also as anti- Feedback signal is sent to lock-in amplifier；
DC source is used to produce direct current signal under the control of host computer, and the direct current signal is loaded into into conducting probe Between 7-4 and sample 15-8；
Signal generator produces three tunnel identical signals, the second-order resonance frequency phase of the signal frequency and conducting probe 7-4 Together, for controlling No. three piezo controllers after the first via is superimposed with the logical adder of the signal that Arbitrary Waveform Generator is produced, No. three are made Piezo controller drives the piezoelectric ceramics 7-2 on probe handss 7；Second tunnel is sent to lock-in amplifier as reference signal；3rd Road is loaded between conducting probe 7-4 and sample 15-8 after 90 degree of phase shifter phase shift；
The signal of lock-in amplifier output is sent to host computer by capture card.
The present invention carries out the principle of the measuring method of multiparameter synchro measure as shown in Fig. 2 the invention breaches tradition makes The drive signal measured as force-displacement curve with sinusoidal signal, the driving measured as force-displacement curve using gaussian signal Signal, therefore, after probe and sample surfaces depart from, the distance between probe and sample will keep stablizing (only sub- nanometer Second order vibration, between point D to point E), the invention makes full use of the idle stroke in conventional test methodologies to realize many ginsengs to sample Number synchro measure, concrete test process is as follows：
Step 1, the piezoelectric ceramics 7-2 on probe handss 7 is driven by No. three piezo controllers, keep conducting probe 7-4 Move back and forth up and down；
Step 2, XYZ nanometer positionings platforms 13 are driven by No. two piezo controllers, and upwards servo moves closer to sample, makes to lead Electric probe 7-4 is contacted with sample 15-8, and continues to increase the maximum force between conducting probe and sample, until conductive spy Maximum interaction force between pin 7-4 and sample 15-8 reaches setting value and keeps；
Step 3, XYZ nanometer positionings platforms 13 are driven to move down by No. two piezo controllers, displacement is less than Kai Er The range of text scanning sample stage 15；
Step 4, Kelvin's scanning sample stage 15 is driven to replace No. two piezo controllers to drive using piezo controller The repeat step 2 of XYZ nanometer positionings platform 13, makes the maximum interaction force between conducting probe and sample reach setting value, passes through Signal generator gives No. three piezo controller superposition machinery exciting Um, and the phase shifter is spent to loading friendship between conducting probe and sample Stream voltage UACSin (ω t), by DC source between conducting probe and sample load direct current compensation voltage UDC；
Wherein, within a period of motion of conducting probe, the interaction between conducting probe and sample is followed successively by：
Step 4-1, the piezoelectric ceramics 7-2 on probe handss 7 is driven to move downward by No. three piezo controllers, when conductive spy Conducting probe will be attracted down and be contacted with sample surfaces when captivation between pin and sample is more than the rigidity of conducting probe, should Time point is A points；
Step 4-2, after conducting probe is contacted with sample, drive the piezoelectricity on probe handss 7 by No. three piezo controllers Ceramic 7-2 continues to move downward, and continues to increase the maximum force between conducting probe and sample, until conducting probe and sample Maximum interaction force between product reaches setting value, and the time point is B points；
The Z-direction coordinate figure of sample stage 15 is scanned by recording B points Kelvin, the surface topography of sample current scan point is obtained Image；The deformation of record B points conducting probe and displacements of the piezoelectric ceramics 7-2 from equilbrium position point A ' to point B, obtain sample and currently sweep The maximum depth of cup image of described point, displacements of the maximum depth of cup=piezoelectric ceramics 7-2 from equilbrium position point A ' to point B-lead The deformation of electric probe；The equilbrium position point A ' is referred to after A points, in conducting probe and sample contact process, conducting probe Force feedback signal be equal to conducting probe and sample not in contact with when force feedback signal time point；
Step 4-3, control conducting probe adverse movement；
When the deformation force of conducting probe is more than the adhesion between conducting probe and sample surfaces, conducting probe is from sample Surface pops out, and the time point is C points, records the power suffered by C point conducting probes, is working as between sample and conducting probe The maximum adhesion of front scanning element tries hard to picture；
By the power between point B and point C-piezoelectric ceramics 7-2 displacement data converting to force-between conducting probe and sample away from From data, and using DMT models fittings, equivalent Young's modulus image of the sample in the scanning element is just obtained, the power is referred to Power suffered by conducting probe, wherein DMT models are shown below：
In formula, F is the interaction force between probe and sample, FadhFor the maximum adhesion power between sample and probe, R For the needle type radius of probe, δ is depth of cup, E*For equivalent Young's modulus；
Young's moduluss E of sample are obtained according to the Poisson's ratio of the equivalent Young's modulus and sample；
Step 4-4, after conducting probe and sample depart from, conducting probe continues to rise to stop motion after setting height h, The time point is D points, and h is more than 0, and makes conducting probe be kept for a period of time in the height, i.e. D points are to E points；
Between point D and point E, the phase place that lock-in amplifier is exported as feedback signal measure conducting probe and sample it Between surface potential difference；The initial point that wherein surface local potential difference is started compensating for is visited apart from the time interval of C points more than conductive The timeconstantτ of pin 7-4, τ=2Q/ ω, Q are quality factor, and ω is angular frequency, total electric potential difference between conducting probe and sample For：
Δ U=UDC-UCPD+UAC sin(ωt)
In formula, UCPDIt is the intrinsic surface potential difference between probe and sample surfaces；
Now, the electrostatic force between conducting probe and sample surfaces is：
In formula, C and z is respectively the electric capacity between probe and sample and distance.Work as U as can be seen from the above equationDC=UCPDWhen, Impact of the electrostatic force under ω frequencies to conducting probe will be eliminated, and using lock-in amplifier the frequency test can be obtained The phase place and amplitude information of pin feedback signal.The phase signal that lock-in amplifier is exported as feed back input to host computer, on Position machine is by adjusting UDCEliminate the skew of lock-in amplifier output phase.Work as UDC=UCPDWhen, the skew of lock-in amplifier output phase To be eliminated.By record U nowDC, the surface local potential between corresponding conducting probe and sample surfaces is just obtained Difference (UCPD) image.
Step 5, by the mobile example of XYZ nanometer positionings platform 13 to next scanning element, repeat step 4 arrives step 5, obtains The surface topography image of sample, equivalent Young's modulus image and surface potential difference image.
Ideally, U is worked asDC=UCPDWhen, the phase place of lock-in amplifier output is 0 degree in step 4, but under normal circumstances Due to the presence of error, the phase place of lock-in amplifier output is not 0 degree, by the phase place for recording lock-in amplifier output, just may be used Obtain corresponding test phase offset error image.
In order to improve the accuracy of measurement result, each scanning element repeat step more than 4 times chooses middle one group of test data B points Kelvin scanning sample stage 15 Z-direction coordinate figure for sample current scan point final surface topography；Choose correspondence group number According to equivalent Young's modulus E*It is worth the final equivalent Young's modulus as sample current scan point；Choose the surface of correspondence group data Final surface potential difference of the potential difference values as sample current scan point；
Wherein, the moving back and forth up and down of conducting probe 7-4, Kelvin's scanning sample stage 15 keep conducting probe 7-4 and sample Maximum interaction force between product 15-8 for setting value servo motion and the mobile example of XYZ nanometer positionings platform 13 to next Parallel running between the motion three of individual scanning element.
Specific embodiment two：With reference to Fig. 1 and Fig. 2 explanation present embodiments, present embodiment is to the institute of embodiment one The further restriction of the Kelvin probe force microscopy stated, in present embodiment, the host computer is embedded in what is realized by software Measurement module, the measurement module is included with lower unit：
Power detector unit：The deformation quantity of the conducting probe 7-4 that Real-time Collection four-quadrant position detector 4 is detected, and root The active force between conducting probe 7-4 and sample is calculated according to the deformation quantity；The active force is equal to deformation quantity and conducting probe 7-4 The product of rigidity；
Surface topography and maximum depth of cup measuring unit：Kelvin is controlled by a piezo controller and scans sample stage 15 rise, and make the close conducting probe 7-4 of sample, when the maximum force between conducting probe 7-4 and sample reaches setting value, The Z-direction coordinate figure of record sample stage piezoelectric ceramics；Maximum depth of cup is recorded simultaneously, and the maximum depth of cup is made pottery equal to piezoelectricity Porcelain 7-2 is from equilbrium position point A ' to the displacement of point B and the difference of the deformation quantity of conducting probe 7-4；Between conducting probe 7-4 and sample Active force reach time point corresponding during setting value for B points；The equilbrium position point A ' refers to that after A points conduction is visited In pin and sample contact process, the force feedback signal of conducting probe be equal to conducting probe and sample not in contact with when force feedback signal Time point；
Adhesion measuring unit：Piezoelectric ceramics 7-2 is controlled by No. three piezo controllers, conducting probe 7-4 is reversely moved It is dynamic, and conducting probe 7-4 and active force suffered during sample disengaging during reverse movement are recorded, the active force is conduction Maximum adhesion power between probe 7-4 and sample；Now corresponding time point is C points；
Equivalent Young's modulus computing unit：By the power between B points and C points-piezoelectric ceramics 7-2 displacement quantity converting to force- Depth of cup data, and using DMT models fittings, the equivalent Young's modulus of sample are just obtained, the DMT models are：
F is the interaction force between conducting probe 7-4 and sample, FadhFor the maximum between sample and conducting probe 7-4 Adhesion, R for conducting probe 7-4 needle type radius, δ is depth of cup, E*For equivalent Young's modulus；
Surface local potential difference measurements unit：The piezoelectric ceramics 7-2 controlled by No. three piezo controllers on probe handss 7 is moved It is dynamic, make conducting probe 7-4 continue to move up certain altitude h, h>0, conducting probe 7-4 is maintained at height h；Will lock The phase place of phase amplifier output adjusts DC voltage U as feedback signalDCValue, make lock-in amplifier export signal be zero, Record U nowDCValue, the UDCThe surface local potential that is between sample and probe of value it is poor；
Sample mobile unit：XYZ nanometer positionings platform 13 is driven to be moved to next scanning element by No. two piezo controllers.
After above-mentioned measurement module has run once, complete the surface topography of sample current scan point, equivalent Young's modulus with And the measurement of surface local potential difference.
Measuring surface form unit measures the corresponding sample piezoelectric ceramics Z-direction coordinate figure of B point, institute in each scanning element There is the surface topography image of the sample stage piezoelectric ceramics Z-direction coordinate figure synthetic sample of scanning element；
Maximum depth of cup measuring unit measures the corresponding depth of cup of B point, all scanning elements in each scanning element Maximum depth of cup synthetic sample maximum depth of cup image；
Maximum adhesion power measuring unit measures the corresponding adhesion of C point in each scanning element, and all scanning elements are most The maximum adhesion of big adhesion synthetic sample tries hard to picture；
Equivalent Young's modulus computing unit measures an equivalent Young's modulus in each scanning element, all scanning elements it is equivalent The equivalent Young's modulus image of Young's moduluss synthetic sample；
It is poor that surface local potential difference measurements unit measures a surface local potential in each scanning element, all scanning elements The surface local potential difference image of the value synthetic sample of surface local potential difference.
Before using above-mentioned measurement module measurement surface pattern, mechanical characteristic and surface local potential difference, first to carry out Some preparations, to the measurement module relevant parameter setting is carried out.Detailed process is as follows：
1st, system initialization, ready sample 15-8 is fixed on specimen holder 15-3, by copper tabletting 15-7 and sample 15-8 conductive contacts and it is fixed, conducting probe 7-4 is arranged on probe handss 7, by conducting probe 7-4 and conducting probe fixed plate 7-6 is conductively connected, and Kelvin's scanning sample stage 15 and probe handss 7 are separately mounted to into sample platform bracket 14 and probe handss support On 9, and binding post is electrically connected with corresponding equipment；
2nd, PC control XY micron positioning table 12 is moved, and by the Primary Location sample 15-8 of optical microscope 20, is selected Suitable measured zone, and the mobile region is to the field of view center of optical microscope 20；
3rd, the one-dimensional wide range adjustment microfluidic platform 10 of movement and XYZ microns positioning table 8, coarse alignment conducting probe 7-4, make conduction The measured zone top that probe 7-4 is placed in selected in the 2nd step, adjusts laser direction, makes the laser facula on conducting probe 7-4 In the front end center of conducting probe 7-4 cantilever beams；
4th, open scanning frequency excitation device carries out frequency sweep operation to conducting probe 7-4, to obtain the second-order resonance of conducting probe 7-4 Frequencies omega and corresponding quality factor q, and then the timeconstantτ=2Q/ ω of conducting probe 7-4 are obtained, and signal is sent out The frequency configuration of raw device is ω；
5th, by the distance between coarse adjustment conducting probe 7-4 of XYZ microns positioning table 8 and sample 15-8, ready position servo Control, and the laser facula on conducting probe 7-4 is readjusted into the front end center of conducting probe 7-4 cantilever beams；
6th, Arbitrary Waveform Generator produces control signal, and each cycle of the control signal is gaussian signal, the control signal Send to No. three piezo controllers, make No. three piezo controllers drive conducting probe 7-4 to pump according to gaussian signal；
Power on conducting probe 7-4 is detected by four-quadrant position detector 4, starts SERVO CONTROL, control XYZ nanometers are determined Position platform 13 is along Z axis fast approaching conducting probe 7-4 and keeps maximum force to be between the two equal to set active force；
7th, stop SERVO CONTROL after servo success, XYZ nanometer positionings platform 13 is declined into certain altitude (less than Kelvin's scanning The stroke of the piezoelectric ceramics 15-2 installed on sample stage 15), then the piezoelectricity installed on sample stage 15 pottery is scanned by Kelvin Porcelain 15-2 repeats the servo in the 6th step, continues to keep the maximum force between conducting probe 7-4 and sample 15-8 equal to set Fixed active force；Generally servo frequency is 5-10 times of rate of scanning, therefore each scanning element has carried out multiple servo；
8th, the mechanical accumulation signal U under second-order resonance frequency is applied to conducting probe 7-4 by signal generatorm, and will The calculating point of phase place is arranged between point D points and E (as shown in Fig. 2 within a period of motion of conducting probe 7-4, conduction is visited The moment that pin 7-4 comes in contact during moving down with sample is A points, and conducting probe 7-4 is continued to move down until and sample Active force between product reaches setting value, and the moment is B points, and then conducting probe 7-4 starts adverse movement, occurs with sample de- From moment be C points, conducting probe 7-4 continuously rises to stop motion after certain altitude, and is kept for a period of time in the height, That is between E points, the initial point that wherein surface local potential difference is compensated to the time between C points is greater than time long number τ to D points), It is zero to adjust the phase place of Um and make the phase output of lock-in amplifier, wherein, the second order exciting of conducting probe 7-4 is in Subnano-class Not, the stable contact between conducting probe 7-4 and sample 15-8 is not interfered with；
The 9th, 90 degree of phase shifter phase shift is set and is opened, second-order resonance frequency is applied between conducting probe 7-4 and sample 15-8 Electric accumulation signal U under rateACSin (ω t), now due to the work function between conducting probe 7-4 and sample 15-8/surface electricity The difference of gesture, therefore, there is surface potential difference U between themCPD, so as to the phase place for causing lock-in amplifier to export will occur partially Move；
10th, open Kelvin's control program for being embedded in of host computer, the phase place that the program exports lock-in amplifier as Feedback signal, control DC source exports a direct current compensation voltage signal UDCAct on conducting probe 7-4 and sample 15-8 it Between, so as to compensate the poor (U of local potential between conducting probe 7-4 and sample 15-8 surfacesCPD), finally make lock-in amplifier defeated The phase recovery for going out is zero, the voltage (U of DC source outputDC) by equal between conducting probe 7-4 and sample 15-8 surfaces Poor (the U of local potentialCPD)；
11st, Scanning step and number of scan points are set, then start scanning.
The conducting probe of above-mentioned Kelvin probe force microscopy is driven simultaneously by multifrequency state, including：1) low frequency Gauss Signal Mechanical Driven (0.5-2kHz), 2) Mechanical Driven under second-order resonance mode, 3) second-order resonance between probe and sample Electric excitation under mode.Host computer carries out segmentation scaling down processing to the feedback signal of conducting probe and realizes that distance controlling, potential are mended Repay and data fitting, so as to realize the synchro measure to sample surface morphology, mechanical characteristic and surface local potential.
Polystyrene/light binding grating is measured using the Kelvin probe force microscopy of present embodiment, is scanned Scope is 2.56um*2.56um, number of scan points be 256*256. Fig. 6 be polystyrene/light binding grating sample scanogram As a result, wherein (a) is surface topography image, the part of center protrusion is polystyrene, and the sunk part in both sides is light binding, Its difference in height is 60nm；B () tries hard to picture for maximum adhesion；C () is maximum depth of cup image；D () is equivalent Young's modulus figure Picture, the Poisson's ratio of polystyrene takes 0.33, therefore, the Young's moduluss of polystyrene are 1.93 ± 0.28GPa；E () is surface office Portion's potential energy diagram picture；F () phase shift errors image, phase error is -0.05 ± 1.01 degree.Table 1 is measurement result, including Maximum adhesion power, maximum depth of cup, equivalent Young's modulus and surface local potential are poor.
The measurement result data list of table 1

Claims (3)

1. a kind of Kelvin probe force microscopy of multiparameter synchro measure, it is characterised in that including XY micron positioning tables (12), XYZ nanometer positioning platforms (13), Kelvin's scanning sample stage (15), XYZ micron positioning tables (8), one-dimensional wide range adjustment microfluidic platform (10), probe handss support (9), probe handss (7), host computer, DC source, Arbitrary Waveform Generator, capture card, signal generator, Phase shifter, lock-in amplifier, four-quadrant position detector, semiconductor laser generator, piezo controller, No. two voltage controls Device processed and No. three piezo controllers；
Kelvin's scanning sample stage (15) is fixed on XYZ nanometer positioning platforms (13), and it is micro- that XYZ nanometer positioning platforms (13) is fixed on XY On rice positioning table (12)；Conducting probe (7-4) is installed on probe handss (7) and conducting probe (7-4) can be driven along vertically side To the piezoelectric ceramics (7-2) of i.e. Z-direction movement, probe handss (7) are fixed on probe handss support (9), and probe handss support (9) is fixed On XYZ micron positioning tables (8), XYZ micron positioning tables (8) is fixed on one-dimensional wide range adjustment microfluidic platform (10)；
Host computer is by the piezoelectric ceramics movement on piezo controller driving Kelvin's scanning sample stage (15), by No. two Piezo controller drives the piezoelectric ceramics on XYZ nanometer positioning platforms (13) to move, drives probe handss by No. three piezo controllers (7) the piezoelectric ceramics movement on；
Semiconductor laser generator produce laser light incident to conducting probe (7-4), Jing conducting probes (7-4) reflection laser It is incident to four-quadrant position detector；
The detectable signal of four-quadrant position detector is sent to host computer by capture card, and the detectable signal is also as feedback signal Send to lock-in amplifier；
DC source is used to produce direct current signal under the control of host computer, and the direct current signal is loaded into into conducting probe (7- 4) and sample (15-8) between；
Signal generator produces three tunnel identical signals, and the signal frequency is identical with the second-order resonance frequency of conducting probe (7-4), The first via is used to control No. three piezo controllers after being superimposed with the logical adder of the signal that Arbitrary Waveform Generator is produced, and makes No. three piezoelectricity Controller drives the piezoelectric ceramics (7-2) on probe handss (7)；Second tunnel is sent to lock-in amplifier as reference signal；3rd Road is loaded between conducting probe (7-4) and sample (15-8) after 90 degree of phase shifter phase shift；
The signal of lock-in amplifier output is sent to host computer by capture card.
2. Kelvin probe force microscopy according to claim 1, it is characterised in that the host computer is embedded in by software The measurement module of realization, the measurement module is included with lower unit：
Power detector unit：The deformation quantity of the conducting probe (7-4) that Real-time Collection four-quadrant position detector (4) is detected, and root Active force of the conducting probe (7-4) and sample between is calculated according to the deformation quantity；The active force is equal to deformation quantity and conducting probe (7-4) product of rigidity；
Surface topography and maximum depth of cup measuring unit：Kelvin is controlled by a piezo controller and scans sample stage (15) On piezoelectric ceramics rise, the close conducting probe of sample (7-4) is made, when maximum effect of the conducting probe (7-4) and sample between When power reaches setting value, the Z-direction coordinate figure of piezoelectric ceramics on Kelvin's scanning sample stage (15) is recorded；Maximum impression is recorded simultaneously Depth, the maximum depth of cup is equal to piezoelectric ceramics (7-2) from equilbrium position point A ' to the displacement of point B and conducting probe (7- 4) difference of deformation quantity；Active force of the conducting probe (7-4) and sample between reaches time point corresponding during setting value for B Point；The equilbrium position point A ' is referred to after A points, in conducting probe and sample contact process, the force feedback letter of conducting probe Number be equal to conducting probe and sample not in contact with when force feedback signal time point；
Adhesion measuring unit：Piezoelectric ceramics (7-2) is controlled by No. three piezo controllers, conducting probe (7-4) is reversely moved It is dynamic, and conducting probe (7-4) and active force suffered during sample disengaging during reverse movement are recorded, the active force is and leads Maximum adhesion power of the electric probe (7-4) and sample between；Now corresponding time point is C points；
Equivalent Young's modulus computing unit：By the power between B points and C points-piezoelectric ceramics displacement quantity converting to force-depth of cup Data, and using DMT models fittings, the equivalent Young's modulus of sample are just obtained, the DMT models are：
F - F a d h = 4 3 E * Rδ 3
F be interaction force of the conducting probe (7-4) and sample between, FadhFor the maximum between sample and conducting probe (7-4) Adhesion, R for conducting probe (7-4) needle type radius, δ is depth of cup, E*For equivalent Young's modulus；
Surface local potential difference measurements unit：The piezoelectric ceramics movement on probe handss (7) is controlled by No. three piezo controllers, is made Conducting probe (7-4) continues to move up certain altitude h, h>0, conducting probe (7-4) is maintained at height h；Will lock The phase place of phase amplifier output adjusts DC voltage U as feedback signalDCValue, make lock-in amplifier export phase signal be Zero, UDCIt is direct current compensation voltage that DC source is loaded between conducting probe and sample, records U nowDCValue, the UDC The surface local potential that is between sample and conducting probe of value it is poor；
Sample mobile unit：XYZ nanometer positioning platforms (13) is driven to be moved to next scanning element by No. two piezo controllers.
3. Kelvin probe force microscopy according to claim 1 and 2, it is characterised in that the Arbitrary Waveform Generator is produced Raw gaussian signal, controls conducting probe and moves back and forth up and down by the signal.
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