Gioi Thieu Kinh Hien Vi Luc Nguyen Tu

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    Scanning Probe Microscopy

    Junior Research Seminar

    Spring 2004

    6 April 2004

    Junior Research Seminar: Nanoscale Patterning and Systems

    Teri W. Odom

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    Fundamental Principles

    Imaging and Spectroscopy

    Instrumentation

    Atomic Force Microscopy

    Junior Research Seminar: Nanoscale Patterning and Systems

    Teri W. Odom

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    Surface force history and measurements

    Surface force apparatus

    Studies of van der waals (VDW) interactions

    Force between mica surfaces (molecules, liquid layers) fromdeflection of spring upon contact

    Separation measured to 1 A; force sensitivity 10-8

    N Surface profi lometers

    Roughness of materials

    Stylus tip in mechanical contact with surface (10-4 N)

    1 m radius of curvature Forces and their range of influence

    Long range

    Electrostatic force in air (100 nm)

    Magneto-electrostatic forces (100 nm)

    Double layer electrostatic (fluid) (100 nm) Short range

    Van der Waals (10 nm)

    Surface-induced solvent ordering (5 nm)

    Hydrogen-bonding force (0.2 nm)

    Contact (0.1 nm)

    Junior Research Seminar: Nanoscale Patterning and Systems

    Teri W. Odom

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    AFM tip and sample interaction

    (1) Large tip-sample separations nodetectable interaction force

    1

    (2) Separation distance decreases

    2

    (3) Separation where the gradient of

    interaction energy exceeds the

    restoring force of the cantilever

    jump to contact point

    3

    (4) Tip pushes farther into surface, a

    positive linear cantilever deflection isobserved; tip retracts from surface,

    a similar cantilever deflection line is

    traced and the tip and sample

    remain in contact

    4

    (5) Separation where restoring force

    exerted by the bending of the

    cantilever overcomes the adhesive

    force of the tip-sample force of

    interaction

    5

    (6) Non-interacting, equilibrium position

    6

    http://www.ntmdt.ru/SPM-Techniques/Spectroscopies/Force-distance_curves_mode20.html

    Junior Research Seminar: Nanoscale Patterning and Systems

    Teri W. Odom

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    Fundamental Principles

    Imaging and Spectroscopy

    Instrumentation

    Atomic Force Microscopy

    Junior Research Seminar: Nanoscale Patterning and Systems

    Teri W. Odom

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    AFM: General Overview

    Junior Research Seminar: Nanoscale Patterning and Systems

    Teri W. Odom

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    Force feedback

    stm2.nrl.navy.mil/how-afm/how-afm.html

    Junior Research Seminar: Nanoscale Patterning and Systems

    Teri W. Odom

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    Optical detection of cantilever changes

    (A+B)-(C+D)

    A B

    C D

    (A+C)-(B+D)

    Junior Research Seminar: Nanoscale Patterning and Systems

    Teri W. Odom

    http://images.google.com/imgres?imgurl=www.spmtips.com/app/Subjects/pics/lateral_deflection.gif&imgrefurl=http://www.spmtips.com/app/Subjects/probes_cantilevers.htm&h=240&w=300&prev=/images%3Fq%3Dafm%2Bschematic%26start%3D40%26svnum%3D10%26hl%3Den%26lr%3D%26ie%3DUTF-8%26oe%3DUTF-8%26sa%3DNhttp://images.google.com/imgres?imgurl=www.spmtips.com/app/Subjects/pics/vertical_deflection.gif&imgrefurl=http://www.spmtips.com/app/Subjects/probes_cantilevers.htm&h=240&w=300&prev=/images%3Fq%3Dafm%2Bschematic%26start%3D40%26svnum%3D10%26hl%3Den%26lr%3D%26ie%3DUTF-8%26oe%3DUTF-8%26sa%3DN
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    Lateral resolution

    Tip effects

    Radius of curvature of tip

    Cone angle and depth of tip

    Aspect ratio of tip

    Force interaction

    Repulsive region can damagesample

    Attractive region not enoughresolution

    Junior Research Seminar: Nanoscale Patterning and Systems

    Teri W. Odom

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    Vibration Isolation Typical frequencies

    1 Hz building vibrations (people

    walking, etc.)

    10 - 100 Hz building vibrations

    (electronics, ventilation, etc.)

    1 - 10 kHz resonant frequency

    of most STMs

    Ideal vibration contributions

    Building vibrational amplitude of

    1 m translates to 1 pm at the

    STM junction

    Solution

    Make STM has rigid as

    possible so that internal

    resonance is high

    Mount it on a low resonant

    frequency support

    Ai r suppor t tables

    Spring suspensions

    PICO SPM solutions

    Junior Research Seminar: Nanoscale Patterning and Systems

    Teri W. Odom

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    Fundamental Principles

    Imaging and Spectroscopy

    Instrumentation

    Atomic Force Microscopy

    Junior Research Seminar: Nanoscale Patterning and Systems

    Teri W. Odom

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    Contact mode imaging Constant force image

    Constant deflection

    Strong repulsive regime

    Tip makes physical contact with the

    surface

    Stiffness of cantilever less than springs

    holding atoms (10 nN/nm)

    VDW forces dominate

    Well-suited for

    Hard and shallow samples Samples with periodicity

    Samples in liquid environments

    Shao, U. Virginia

    2.5m

    Q. Xu, U. Virginia R. Bley, U. Virginia

    80 nm

    http://www.ntmdt.ru/SPM-Techniques/SFM/dc_Contact_techniques/Constant_Force_mode_mode9.html

    Junior Research Seminar: Nanoscale Patterning and Systems

    Teri W. Odom

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    Lateral force microscopy

    -COOH

    -CH3

    25 nN

    C.M. Lieber, J. Am. Chem. Soc. 117, 7943 (1995)http://www.ntmdt.ru/SPM-Techniques/SFM/dc_Contact_techniques/Lateral_Force_Imaging_mode11.html

    Junior Research Seminar: Nanoscale Patterning and Systems

    Teri W. Odom

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    Noncontact mode imaging Constant force gradient image

    Amplitude or resonance frequency

    feedback

    Weak attractive regime

    Tip oscillated 1-10 nm above thesurface

    Stiff cantilever

    Tip-sample forces ~ pN

    Using for imaging

    Soft surfaces Samples in ultra-high vacuum

    2 m

    Raspberry polymer, DI

    10 m

    5 m

    Polystyrene spheres, DI

    http://www.ntmdt.ru/SPM-Techniques/SFM/Non-Contact_techniques/Non-Contact_mode_mode57.html

    Junior Research Seminar: Nanoscale Patterning and Systems

    Teri W. Odom

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    Tapping mode imaging

    Constant force gradient image

    Amplitude feedback

    Weak repulsive force

    Stiff cantilever makes intermittent

    contact with the surface Well-suited for

    Soft samples (biomolecules, polymers)

    Samples with poor surface adhesion

    Arene on graphite, T. Nguyen, Columbia

    B. Stine, Northwesternhttp://www.ntmdt.ru/SPM-Techniques/SFM/Semicontact_techniques/Semicontact_mode_mode28.html

    Junior Research Seminar: Nanoscale Patterning and Systems

    Teri W. Odom

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    Force spectroscopy

    C.M. Lieber, J. Am. Chem. Soc. 117, 7943 (1995)C.M. Lieber, J. Am. Chem. Soc. 119, 2006 (1997)

    http://www.ntmdt.ru/SPM-Techniques/Spectroscopies/Force-distance_curves_mode20.html

    Titration curves

    Junior Research Seminar: Nanoscale Patterning and Systems

    Teri W. Odom

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    Dip Pen Nanolithography

    Junior Research Seminar: Nanoscale Patterning and Systems

    Teri W. Odom

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    Dip-Pen Nanolithography (DPN)

    http://www.chem.northwestern.edu/~mkngrp/timeref.html#dpn

    Junior Research Seminar: Nanoscale Patterning and Systems

    Teri W. Odom

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    DPN Writing

    Junior Research Seminar: Nanoscale Patterning and Systems

    Teri W. Odom

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    Instrumentation

    Junior Research Seminar: Nanoscale Patterning and Systems

    Teri W. Odom

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    Contact Time with Molecular Ink

    C.A. Mirkin, Science 283, 661-663 (1999)

    ODT tip MHA tip

    10, 20, 40 s2, 4, 16 min

    Probe

    Ink diffusion

    2

    A r C t= =

    2 time

    units

    3 time

    units1 time

    unit

    Junior Research Seminar: Nanoscale Patterning and Systems

    Teri W. Odom

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    Towards Parallel Patterning

    C. Mirkin, Science 288, 1808-1811 (2000)

    Junior Research Seminar: Nanoscale Patterning and Systems

    Teri W. Odom

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    Labs 2 and 3: Atomic Force Microscopy

    andDip-pen Nanolithography

    Training on atomic force microscope

    Writing patterns using DPN

    Wet chemical etching

    Lab report on both DPN and AFM due on

    26 April

    Junior Research Seminar: Nanoscale Patterning and Systems

    Teri W. Odom