CN106443218B - A kind of surface charge measurement method - Google Patents

A kind of surface charge measurement method Download PDF

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Publication number
CN106443218B
CN106443218B CN201611048902.8A CN201611048902A CN106443218B CN 106443218 B CN106443218 B CN 106443218B CN 201611048902 A CN201611048902 A CN 201611048902A CN 106443218 B CN106443218 B CN 106443218B
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probe
sample
surface charge
flying
moving distance
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CN106443218A (en
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曾慧中
冯杰
何月
张佳玉
张文旭
张万里
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University of Electronic Science and Technology of China
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University of Electronic Science and Technology of China
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01RMEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
    • G01R29/00Arrangements for measuring or indicating electric quantities not covered by groups G01R19/00 - G01R27/00
    • G01R29/24Arrangements for measuring quantities of charge

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  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Investigating Or Analyzing Materials By The Use Of Electric Means (AREA)
  • Length Measuring Devices With Unspecified Measuring Means (AREA)

Abstract

The invention belongs to surface charge measurement technical field, especially a kind of surface charge measurement method using Kelvin probe force microscopy technology.The fibre optic interferometer that the present invention is carried using Kelvin probe force microscopy itself measures the offset of probe by the variation of measurement interference laser intensity, complete the distance correction to needle point to sample, reliable surface charge density is finally obtained using the relationship of the actual range and electrostatic force of needle point and sample, is of great significance for the research of material and device surface charge.

Description

A kind of surface charge measurement method
Technical field
It is especially a kind of using Kelvin probe force microscopy technology the invention belongs to surface charge measurement technical field Surface charge measurement method.
Technical background
Surface charge measurement method is the basis of surface charge research, and the accurate surface charge that measures is for present each electron-like The micromation research of device is of great significance.
Currently, surface charge measurement method has dust figure method, electrostatic probe method and the optics based on Pockels effect to survey Amount method etc..But above method cannot all quantify surface charge, and resolution ratio is not high.
Comparing effective ways for the measurement of surface charge in the prior art is Kelvin probe force microscopy technology, the skill Art calculates surface charge density by the electrostatic force signal between exploratory probe and sample surfaces.Specific method is to utilize Kai Er Literary probe force microscopy, measure the electrostatic force between probe and sample and flying-spot tube moving distance relation curve (i.e. " and power-away from From " curve), then by formula " power-distance " curve is fitted, and then extrapolate the surface charge density of sample.
At document " Mapping and Quantifying Surface Charges on Clay Naoparticles " (Jun Liu;Ravi Gaikwad;Aharnish Hande;Siddhartha Das.Langmuir 2015,31,10469- 10476) in, introduction of authors is a kind of using Kelvin probe force microscopy technology clay material surface charge is carried out it is quantitative The step of method, this method, is described as follows:
1) sample to be tested is fixed on the sample stage of Kelvin probe force microscopy, adjusts instrument parameters;
2) apply alternating voltage between probe and sample, make probe and its cantilever that resonance occur, probe is moved to sample Product region to be measured measures the relation curve of probe vibration frequency and flying-spot tube moving distance;
3) pass through formulaRelation curve is fitted to obtain sample surface charge density σ.
Above-mentioned surface charge measurement method can be realized the surface charge quantitative measurment of nanoscale.But probe with When sample distance is less than 50nm, influence of the power to probe will lead to probe cantilever the effects of Van der Waals force, electrostatic force Deformation, at this point, the distance that actual " power-distance " distance is mobile not equal to flying-spot tube, causes through fitting " power-distance " curve There are large errors for the method for extraction surface charge density.
Therefore, in the prior art using the method for Kelvin probe force microscopy technology measurement surface charge due to actual Distance in " power-distance " is not equal to the mobile distance of flying-spot tube, leads to surface charge measurement there are errors larger, and existing cannot The shortcomings that accurate measurement surface charge.
Summary of the invention
The object of the present invention is to provide a kind of surveys that surface charge is accurately measured using Kelvin probe force microscopy technology Amount method.
In order to solve the above technical problems, the technical solution adopted by the present invention is that a kind of surface charge measurement method, including such as Lower step:
1) sample to be tested is fixed on the sample stage of Kelvin probe force microscopy, it is swashing for λ that laser, which issues wavelength, Light applies DC voltage V on piezoelectric patchesdc, so that probe vertically moves, moving distance is greater than laser wavelength lambda;Meanwhile it recording The relationship for interfering laser intensity and probe moving distance, by the maximum value I for interfering laser intensitymaxWith minimum value Imin, calculate Obtain the sensitivity of interferometer measurement probe offset
2) apply alternating voltage between probe and sample, make probe and its cantilever that resonance occur, probe is moved to sample The top of product tested point, flying-spot tube is mobile to probe direction, using the Oscillation Amplitude R and phase theta of lock-in amplifier monitoring probe, Obtain the relation curve of probe Oscillation Amplitude R and flying-spot tube moving distance Z, the relationship song of phase theta and flying-spot tube moving distance Z Oscillation Amplitude R and phase theta are output to computer by line;Interference laser intensity I is monitored simultaneously, and the interference laser of initial position is strong Degree is I0, obtain the relation curve of interference laser intensity and flying-spot tube moving distance Z;
3) phase theta and Oscillation Amplitude R, the range value with probe in initial position arrived by computer acquisition normalizes meter Calculation obtains normalized amplitude value RN, A=cos θ/R is then calculatedN
4) pass through the changing value Δ I=I-I of interference laser intensity in flying-spot tube moving process0, calculate the deformation quantity of cantilever Δ Z=D × Δ I, amendment obtain the actual range Z*=Z- Δ Z of " tip-sample ", obtain A-Z* curved line relation;
5) pass through formulaA-Z* force curve is fitted, the value of M, B are obtained, M, B are constant;
6) surface charge density is calculated:
Wherein S=π × r2, r is probe tip radius;K is needle point coefficient of elasticity, ε0For permittivity of vacuum.
In order to solve the problems, such as probe offset and bring " tip-sample " distance there are deviations, obtain reliable surface Charge density data, the fibre optic interferometer measurement interference laser intensity that the present invention is carried using Kelvin probe force microscopy itself Variation obtain the offset of probe, complete the distance correction to needle point to sample, the actual range of utilization " tip-sample " Reliable surface charge density is finally obtained with the relationship of electrostatic force.
Detailed description of the invention
Fig. 1 is the schematic diagram of " tip-sample " distance;
Fig. 2 is the system structure diagram of Kelvin probe force microscopy measurement surface charge;
Fig. 3 is the relation curve for interfering laser intensity and probe deflection;
Fig. 4 is relation curve of the needle point close to sample middle probe offset and flying-spot tube moving distance;
Fig. 5 is the power-distance Curve and its corresponding matched curve before and after " tip-sample " distance correction.
Specific embodiment
Invention is further explained with example with reference to the accompanying drawing:
In the present embodiment, conducting probe coefficient of elasticity k=2.18N/m, resonant frequency 75kHz used;S=1 × 10-15m2;Permittivity of vacuum ε0=8.85 × 10-12;Sample to be tested is SiO2, by test macro shown in Fig. 2, specific measurement step It is rapid as follows:
By SiO2Sample is fixed on the sample stage of Kelvin probe force microscopy, and laser issues the laser of 40uw, Apply DC voltage V on piezoelectric patchesdc=3V so that probe vertically moves, while recording interference laser intensity and moving distance Relationship, as shown in figure 3, by the maximum value I of interference laser intensitymaxWith minimum value IminThe probe that interferometer measurement arrives is calculated Deviation sensitivity D=142.1nm/V;
Apply alternating voltage between probe and sample, makes probe and its cantilever that resonance occur, probe is moved to sample The top of tested point, flying-spot tube is mobile to probe direction, using the Oscillation Amplitude R and phase theta of lock-in amplifier monitoring probe, obtains To the relation curve of probe Oscillation Amplitude R and flying-spot tube moving distance Z, the relation curve of phase theta and flying-spot tube moving distance Z, Oscillation Amplitude R and phase theta signal are output to computer;Interference laser intensity I is monitored simultaneously, by the interference laser of initial position Intensity is denoted as I0, obtain the relation curve of monitoring interference laser intensity and flying-spot tube moving distance Z.
The phase theta and Oscillation Amplitude R arrived by computer acquisition is normalized in the range value of initial position with probe and is calculated Obtain normalized amplitude value RN, power A=cos θ/R is then calculatedN;The curve of A-Z can be obtained at this time;
Interfere the changing value Δ I=I-I of laser intensity during sample surfaces by probe0, calculate the shape of cantilever Variable Δ Z=142.1 × Δ I, obtains the relationship of probe offset as shown in Figure 4 Yu flying-spot tube moving distance, and then acquire " needle The actual distance Z*=Z- Δ Z of point-sample ", obtains A-Z* curved line relation as shown in Figure 5;
Pass through formulaThe force curve of amendment front and back is fitted respectively, obtains the value of M, B;M, B are normal Amount;M, B are substituted into formula againSurface charge density is calculated;By the fit solution of Fig. 5 it is found that before amendment The surface charge density σ being calculated is 5.0uCcm-2, revised surface charge density σ is 4.4uCcm-2.Pass through ratio Compared with discovery, obtained surface charge density value increases compared with the value after amendment before " tip-sample " distance correction 10%.

Claims (1)

1. a kind of surface charge measurement method, it is characterised in that include the following steps:
1) sample to be tested being fixed on the sample stage of Kelvin probe force microscopy, laser issues the laser that wavelength is λ, Apply DC voltage V on piezoelectric patchesdc, so that probe vertically moves, moving distance is greater than laser wavelength lambda;Meanwhile it recording interference and swashing The relationship of luminous intensity and probe moving distance, by the maximum value I for interfering laser intensitymaxWith minimum value Imin, it is calculated dry The sensitivity of interferometer measurement probe offset
2) apply alternating voltage between probe and sample, make probe and its cantilever that resonance occur, probe is moved to sample and is waited for The top of measuring point, flying-spot tube is mobile to probe direction, using the Oscillation Amplitude R and phase theta of lock-in amplifier monitoring probe, obtains The relation curve of the relation curve of probe Oscillation Amplitude R and flying-spot tube moving distance Z, phase theta and flying-spot tube moving distance Z, will Oscillation Amplitude R and phase theta are output to computer;Interference laser intensity I is monitored simultaneously, and the interference laser intensity of initial position is I0, obtain the relation curve of interference laser intensity and flying-spot tube moving distance Z;
3) phase theta and Oscillation Amplitude R, the range value normalization with probe in initial position arrived by computer acquisition calculates To normalized amplitude value RN, A=cos θ/R is then calculatedN
4) pass through the changing value Δ I=I-I of interference laser intensity in flying-spot tube moving process0, calculate the deformation quantity Δ Z=D of cantilever × Δ I, amendment obtain the actual range Z*=Z- Δ Z of " tip-sample ", obtain A-Z* curved line relation;
5) pass through formulaA-Z* force curve is fitted, the value of M, B are obtained, M, B are constant;
6) surface charge density is calculated:
Wherein S=π × r2, r is probe tip radius;K is needle point coefficient of elasticity, ε0For permittivity of vacuum.
CN201611048902.8A 2016-11-24 2016-11-24 A kind of surface charge measurement method Expired - Fee Related CN106443218B (en)

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CN108196178B (en) * 2017-12-28 2020-02-14 电子科技大学 Measuring device for surface trap energy level distribution and photoconductive analysis method
CN108362913B (en) * 2018-02-08 2020-05-12 电子科技大学 Ferroelectric domain polarization direction discrimination method of laser interference type piezoelectric power microscope
CN108802442B (en) * 2018-05-30 2020-07-24 中国船舶重工集团公司第七二五研究所青岛分部 Kelvin probe testing device and testing method thereof
CN109917407A (en) * 2019-03-22 2019-06-21 中国科学院重庆绿色智能技术研究院 A kind of near field probe distance measuring method and device based on laser reflection
CN110672882B (en) * 2019-11-07 2022-06-03 南京邮电大学 Method for detecting dielectric constant of material by using scanning probe
CN111273094B (en) * 2020-01-21 2021-12-17 黑龙江大学 Optical fiber sensing probe application system for detecting electrode charge amount of super capacitor and preparation method of optical fiber sensing probe
CN111879451B (en) * 2020-07-30 2021-10-15 合肥工业大学 Microcosmic acting force measuring system and method for judging contact zero point and surface property of microcosmic acting force measuring system
CN112198370A (en) * 2020-09-03 2021-01-08 中山大学 Method and system for measuring local dielectric constant of thin film and storage medium
CN113030602B (en) * 2021-03-02 2022-10-21 北京纳米能源与系统研究所 Method, device, equipment and medium for measuring electrical property of sample material
CN113917221B (en) * 2021-10-09 2023-07-25 重庆师范大学 Optical fiber-based optical high-precision electricity inspection device and system

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CN101281219A (en) * 2007-04-06 2008-10-08 国家纳米科学中心 Method for measuring characteristic capacitance of scanning probe microscope conductive pinpoint
CN101788572A (en) * 2010-01-26 2010-07-28 中山大学 Kelvin probe force microscopy and measuring method thereof
CN102981023A (en) * 2012-11-21 2013-03-20 哈尔滨理工大学 Method for measuring surface potential by using electrostatic force microscope
EP2850412A1 (en) * 2012-05-14 2015-03-25 Optofluidics, Inc. Methods of using near field optical forces

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Publication number Priority date Publication date Assignee Title
CN101281219A (en) * 2007-04-06 2008-10-08 国家纳米科学中心 Method for measuring characteristic capacitance of scanning probe microscope conductive pinpoint
CN101788572A (en) * 2010-01-26 2010-07-28 中山大学 Kelvin probe force microscopy and measuring method thereof
EP2850412A1 (en) * 2012-05-14 2015-03-25 Optofluidics, Inc. Methods of using near field optical forces
CN102981023A (en) * 2012-11-21 2013-03-20 哈尔滨理工大学 Method for measuring surface potential by using electrostatic force microscope

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