CN112362909A - Pressure sensing method for projecting AFM probe on surface of nanowire in scanning electron microscope - Google Patents

Pressure sensing method for projecting AFM probe on surface of nanowire in scanning electron microscope Download PDF

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CN112362909A
CN112362909A CN202011187548.3A CN202011187548A CN112362909A CN 112362909 A CN112362909 A CN 112362909A CN 202011187548 A CN202011187548 A CN 202011187548A CN 112362909 A CN112362909 A CN 112362909A
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afm
sensing method
nanowire
electron microscope
scanning electron
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CN112362909B (en
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曲钧天
张震
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Tsinghua University
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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
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
    • G01Q60/00—Particular types of SPM [Scanning Probe Microscopy] or microscopes; Essential components thereof
    • G01Q60/24—AFM [Atomic Force Microscopy] or apparatus therefor, e.g. AFM probes
    • G01Q60/38—Probes, their manufacture, or their related instrumentation, e.g. holders

Abstract

The invention relates to a surface pressure sensing method for a single nanowire, in particular to a pressure sensing method for a protruding AFM probe on the surface of the nanowire in a scanning electron microscope. The pressure sensing method comprises the following three steps: 1) AFM cantilever beam bending deflection calculation based on visual tracking, 2) AFM rigidity correction, and 3) AFM torque correction. The pressure sensing method provided by the invention can be combined with the advantage that the protruding AFM has a visual probe (overlooking angle), is effectively applied to the fields of nano material control and characterization in a scanning electron microscope and the like, and provides real-time pressure feedback for quantitatively and accurately applying pressure to a single nanowire. The sensing method is simple and efficient in calculation process, wide in application range and suitable for surface pressure sensing of single nanowires with different sizes.

Description

Pressure sensing method for projecting AFM probe on surface of nanowire in scanning electron microscope
Technical Field
The invention relates to a surface pressure sensing method for a single nanowire, in particular to a pressure sensing method for a protruded AFM probe on the surface of the nanowire in a scanning electron microscope.
Background
In recent years, one-dimensional nanowire materials have been widely used in various fields such as high-performance new materials, aerospace, micro-electro-mechanical systems, new energy sources, and the like due to superior physical and chemical properties and high-strength mechanical properties. Therefore, how to accurately characterize the advanced mechanical properties of nanowires through experimental methods plays a crucial role in these practical applications as described above.
To date, a variety of experimental techniques have been applied to in situ mechanical characterization of nanowires. For example, bending test and tensile test are performed on silicon nanowires using an Atomic Force Microscope (AFM). Compared with the traditional nanowire experimental characterization technology, the recently emerging Scanning Electron Microscope (SEM) -based nano manipulation technology can provide stronger support for in-situ characterization of mechanical properties of nanowires. For example, in the field of in-situ characterization of mechanical properties, an AFM probe is embedded in an SEM vacuum chamber to perform in-situ tensile testing on a single silicon nanowire, so as to characterize mechanical properties such as young's modulus and yield stress of the nanowire. Also, the elastic modulus of the nanowires can be measured in situ in a scanning electron microscope using an electro-vibration method.
However, how to apply precisely quantified pressure/stress to the nanowire by using the nanoprobe or the AFM probe in the scanning electron microscope still remains a challenge, which involves complex problems such as nanomechanical modeling and control, and furthermore, the problem of effective probe-nanowire contact detection is caused by the problems that the SEM cannot provide depth information and the tip of the AFM probe cannot be observed in a top view angle. In recent years, an AFM probe with a novel structure, namely, a protruding AFM probe is gradually applied to the control of a nanowire, and the tip of the AFM probe can be clearly observed at the overlooking angle of a scanning electron microscope because the tip of the probe protrudes out of an AFM cantilever structure, so that the AFM is more easily controlled to be in contact with the nanowire. But the method for applying pressure to the surface of a single nanowire and sensing the pressure by using the probe is still effective at present.
Disclosure of Invention
The invention aims to establish a pressure sensing method of a protruded AFM probe on the surface of a nanowire in a scanning electron microscope, which can provide a basis for applying quantitative pressure to a single nanowire by using the protruded AFM probe in the scanning electron microscope. The pressure sensing method comprises the following three steps: 1) AFM cantilever beam bending deflection calculation based on visual tracking, 2) AFM rigidity correction, and 3) AFM torque correction. The pressure sensing method provided by the invention can be combined with the advantage that the protruding AFM has a visual probe (overlooking angle), is effectively applied to the fields of nano material control and characterization in a scanning electron microscope and the like, and provides real-time pressure feedback for quantitatively and accurately applying pressure to a single nanowire. The sensing method is simple and efficient in calculation process, wide in application range and suitable for surface pressure sensing of single nanowires with different sizes.
Firstly, the structure of the protruding AFM probe is as shown in fig. 2, because the probe tip protrudes from the cantilever, the protruding probe tip can be seen from a top view angle, so the AFM probe with the structure has the advantages that the conventional AFM probe (the probe tip is below the cantilever, and cannot be seen from the top view angle) does not have, for example, when the structure is applied to nano control and other applications, the position of the AFM probe tip can be clearly observed, and the control probe can conveniently operate and contact nano materials. Therefore, the invention provides a method for performing pressure sensing on the surface of a nanowire by using a protruded AFM probe in a scanning electron microscope.
The protruding AFM probe is embedded in a nano-positioning platform in a scanning electron microscope, so that the AFM probe can be controlled in three degrees of freedom and contacted with the upper surface of a single nanowire, and vertical downward pressure is applied to the nanowire. The invention provides a method for quantitatively sensing the surface pressure of a nanowire, which comprises the following three steps (as shown in figure 1): 1) AFM cantilever beam bending deflection calculation based on visual tracking to obtain deltazAnd 2) AFM rigidity correction to obtain a corrected rigidity coefficient kzAnd 3) AFM torque correction to obtain corrected torque Tz. Pressure (F) of projecting AFM probe on the surface of nanowire in scanning electron microscopez) The sensing method comprises the following steps: pressure-AFM cantilever bending deflection multiplied by corrective stiffness factor multiplied by corrective torque, i.e. Fz＝kz·Tz·Δz。
The following describes the specific implementation of the above three steps.
Step 1) of the sensing method is AFM cantilever beam bending deflection calculation based on visual tracking, and the specific calculation flow is shown in FIG. 3:
(1) setting the AFM cantilever root moving displacement as Z;
(2) controlling the nano positioning platform to move and displace Z (the root of the AFM probe is connected to the nano positioner);
(3) detecting the displacement of the AFM cantilever tip by using a computer vision algorithm, and setting the displacement as z0Wherein the inclination angle of the nano control platform is theta;
(4) obtaining the displacement z 'of the AFM cantilever beam tip on the axis where the vertical cantilever beam is located through coordinate system transformation'0，z′0＝z0/sinθ；
(5) Finally obtaining the bending deflection delta of the AFM cantilever beamz＝Z-z′0。
Step 2) of the sensing method is AFM stiffness correction, and the correction is needed because the AFM probe is usually fixed on the nanopositioner at an inclination angle (θ, relative to the horizontal sample plane), which affects the effective cantilever stiffness, so that the effective AFM cantilever stiffness coefficient (set as k) needs to be accurately determined when calculating the pressurez) As shown in FIG. 4, the corrected stiffness coefficient
Figure BDA0002751768670000031
Wherein
Figure BDA0002751768670000032
The parameter meaning can refer to fig. 2.
Step 3) of the sensing method is AFM torque correction, and when the surface pressure of the AFM probe on the nanowire is calculated, the torque (set as T) after effective AFM correction needs to be accurately determinedz) As shown in fig. 4, the corrected torque is
Figure BDA0002751768670000033
Wherein
Figure BDA0002751768670000034
The parameter meaning can refer to fig. 2.
Through the three calculation steps, the pressure (F) of the AFM probe protruding from the surface of the nanowire in the final scanning electron microscope can be obtainedz) The sensing method comprises the following steps: pressure-AFM cantilever bending deflection multiplied by corrective stiffness factor multiplied by corrective torque, i.e. Fz＝kz·Tz·Δz。
Compared with the prior art, the method has the following advantages:
the pressure sensing method provided by the invention can be combined with the advantage that the protruding AFM has a visual probe (overlooking angle), is effectively applied to the fields of nano material control and characterization in a scanning electron microscope and the like, and provides real-time pressure feedback for quantitatively and accurately applying pressure to a single nanowire. The sensing method is simple and efficient in calculation process, wide in application range and suitable for surface pressure sensing of single nanowires with different sizes.
Detailed Description
In order to illustrate in detail the effectiveness of the method of the present invention in sensing the pressure of the protruding AFM probe on the surface of the nanowire in the implementation of the scanning electron microscope, the present invention is further described in detail with reference to the following specific examples.
Example (b): single nanowire surface pressure sensing and calibration of different diameters
Firstly, a protruding AFM probe is fixed on a nano positioning platform in a scanning electron microscope, and the protruding AFM probe is controlled in three degrees of freedom by controlling a nano positioner.
Then, nanowire sample preparation is performed. The InGaN/GaN quantum dot LED semiconductor nanowire is prepared by a plasma-assisted epitaxial molecular beam (PA-MBE) growth method, the height is about 650nm, the diameter range is 200-700nm, then the nanowire is packaged and protected by Polyimide (PI), and Ni/Au and Ti/Au electrodes are plated on the upper surface of the nanowire and the lower surface of a substrate.
Subsequently, to verify that the sensing method of the present invention can be effectively applied to single nanowires with different sizes, 4 single nanowires with different diameters are selected within the diameter range of 200-700nm, which is 645nm, 470nm, 325nm and 223nm respectively. Respectively controlling the nanometer positioner to vertically move downwards, applying the protruding AFM probe to apply pressure to the four nanowires with different diameters (as shown in FIG. 5), recording the downward given displacement of the nanometer positioner (namely Z in the sensing method of the invention), respectively calculating the pressure of the protruding AFM probe to the surfaces of the four nanowires through the Z (3 calculation steps in the method of the invention), and finally drawing corresponding 4 pressure-nanometer positioner displacement data graphs (as shown in FIG. 6).
It can be seen from the four data graphs in fig. 6 that when the sensing method of the present invention is applied to single nanowires with different diameters, almost the same linear quantitative relationship between pressure and displacement of the nano-positioner can be obtained, and the effectiveness of the sensing method of the present invention in surface pressure sensing of single nanowires with different dimensions can be verified.
The protection scope of the present invention is not limited to the above embodiments, and the protection scope of the present invention should be subject to the protection scope of the claims.
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In order to more clearly illustrate the embodiments of the present disclosure or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present disclosure, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a schematic diagram of a step of a pressure sensing method of a protruding AFM probe on a surface of a nanowire in a scanning electron microscope according to the present invention;
FIG. 2 is a schematic diagram of the protruding AFM probe structure of the present invention, wherein the parameters are as follows:
AFM cantilever Length L
AFM cantilever Width
AFM cantilever thickness
Angle between AFM cantilever and horizontal sample plane
Alpha is the angle between the extension line of the AFM probe tip and the normal vector of the sample plane
AFM Probe tip Length
Z-axis-axis perpendicular to the sample plane
·zcAxis perpendicular to the plane of the cantilever beam
·kcAFM cantilever beam has inherent elastic coefficient and action direction perpendicular to the plane of the cantilever beamNoodle
·kzAFM cantilever effective modulus of elasticity (correction), perpendicular to the horizontal sample plane
·FzPressure applied by AFM probe to single nanowire
·ΔzAFM cantilever bending deflection
E: young's modulus of silicon
·kzθAFM cantilever beam elastic coefficient (longitudinal torque direction)
·TzAFM torque correction perpendicular to the sample plane
FIG. 3 is a flow chart of step 1) AFM cantilever bending deflection calculation based on visual tracking of the sensing method of the present invention;
FIG. 4 is a flowchart of the calculation of AFM stiffness correction in step 2) and AFM torque correction in step 3) of the sensing method of the present invention;
FIG. 5 is a scanning electron microscope image of the application of pressure to the surface of four different sized individual nanowires using a protruding AFM probe in an embodiment of the present invention;
fig. 6 is a graph of 4 sets of pressure-nanopositioner displacement data obtained by applying pressure to the surface of four single nanowires of different sizes and performing pressure sensing using a protruding AFM probe in the embodiment of the present invention.

Claims (4)

1. A pressure sensing method for projecting AFM probe on the surface of a nanowire in a scanning electron microscope is characterized by comprising three steps (as shown in figure 1): 1) AFM cantilever beam bending deflection calculation based on visual tracking to obtain deltazAnd 2) AFM rigidity correction to obtain a corrected rigidity coefficient kzAnd 3) AFM torque correction to obtain corrected torque Tz. Pressure (F) of projecting AFM probe on the surface of nanowire in scanning electron microscopeZ) The sensing method comprises the following steps: pressure-AFM cantilever bending deflection multiplied by corrective stiffness factor multiplied by corrective torque, i.e. FZ＝kz·TZ·ΔZ。
2. The pressure sensing method for the protruding AFM probe on the surface of the nanowire in the scanning electron microscope according to claim 1, wherein the step 1) of the sensing method is a flow of calculating the bending deflection of the AFM cantilever based on visual tracking as shown in FIG. 3, and the flow is as follows:
(1) setting the AFM cantilever root moving displacement as Z;
(2) controlling the nano positioning platform to move and displace Z (the root of the AFM probe is connected to the nano positioner);
(3) detecting the displacement of the AFM cantilever tip by using a computer vision algorithm, and setting the displacement as z0Wherein the inclination angle of the nano control platform is theta;
(4) obtaining the displacement z 'of the AFM cantilever beam tip on the axis where the vertical cantilever beam is located through coordinate system transformation'0，z′0＝z0/sinθ；
(5) Finally obtaining the bending deflection delta of the AFM cantilever beamz＝Z-z′0。
3. The pressure sensing method for the protruding AFM probe on the surface of the nanowire in the scanning electron microscope according to claim 1, wherein the calculation process of AFM stiffness correction in step 2) of the sensing method is shown in FIG. 4, and the corrected stiffness coefficient is
Figure FDA0002751768660000011
Wherein
Figure FDA0002751768660000012
The parameter meaning can refer to fig. 2.
4. The pressure sensing method for the protruding AFM probe on the surface of the nanowire in the scanning electron microscope according to claim 1, wherein the calculation process of AFM torque correction in step 3) of the sensing method is shown in FIG. 4, and the corrected torque is
Figure FDA0002751768660000013
Wherein
Figure FDA0002751768660000014
The parameter meaning can refer to fig. 2.
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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5193383A (en) * 1990-07-11 1993-03-16 The United States Of America As Represented By The Secretary Of The Navy Mechanical and surface force nanoprobe
CN1699960A (en) * 2005-05-25 2005-11-23 中国科学院上海微系统与信息技术研究所 Improved method for testing micro-cantilever beam elasticity coefficient
CN1755345A (en) * 2004-09-30 2006-04-05 中国科学院沈阳自动化研究所 Little acting force modeling method based on the deformation of nano scanning probe
US20060243036A1 (en) * 2004-01-05 2006-11-02 Hak-Joo Lee Atomic force microscope with probe with improved tip movement
CN202256050U (en) * 2011-10-11 2012-05-30 吉林大学 In-situ stretch/compression material mechanical test platform based on quasi-static loaded scanning electron microscope
CN111505346A (en) * 2020-05-15 2020-08-07 大连理工大学 AFM probe for quantitative measurement, modification method and application thereof

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5193383A (en) * 1990-07-11 1993-03-16 The United States Of America As Represented By The Secretary Of The Navy Mechanical and surface force nanoprobe
US20060243036A1 (en) * 2004-01-05 2006-11-02 Hak-Joo Lee Atomic force microscope with probe with improved tip movement
CN1755345A (en) * 2004-09-30 2006-04-05 中国科学院沈阳自动化研究所 Little acting force modeling method based on the deformation of nano scanning probe
CN1699960A (en) * 2005-05-25 2005-11-23 中国科学院上海微系统与信息技术研究所 Improved method for testing micro-cantilever beam elasticity coefficient
CN202256050U (en) * 2011-10-11 2012-05-30 吉林大学 In-situ stretch/compression material mechanical test platform based on quasi-static loaded scanning electron microscope
CN111505346A (en) * 2020-05-15 2020-08-07 大连理工大学 AFM probe for quantitative measurement, modification method and application thereof

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