3 AFM Lecture

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     Microscopy

    1

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    2

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    Scanning Probe Microscopy (SPM)

    y x

    Moni tor the interactions between a probe and a sample surface

    Types of SPM

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    Scanning Probe Microscopy

    History: The Scanning Tunneling Microscope (STM)was invented by G. Binnig and H. Rohrer, for whichthey were awarded the Nobel Prize in 1984

     A few years later, the first Atomic Force Microscope

    (AFM) was developed by G. Binnig, Ch. Gerber, andC. Quate at Stanford University by gluing a tinyshard of diamond onto one end of a tiny strip of goldfoil

    TYPES OF SPM ?

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    •  Atomic Force Microscopy (AFM)-Monitors the forcesof attraction and repulsion between a probe and asample surface

    • Scanning Tunneling Microscopy (STM). Tunneling ofelectrons through air between probe and surface

    • Lateral Force Microscopy (LFM) Frictional forcesmeasured by twisting or “sideways” forces on

    cantilever.• Magnetic Force Microscopy (MFM)-Magnetic tip

    detects magnetic fields/measures magnetic propertiesof the sample.

    • Electrostatic Force Microscopy (EFM)-Electricallycharged Pt tip detects electric fields/measuresdielectric and electrostatic properties of the sample

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    •Chemical Force Microscopy (CFM)-Chemically

    functionalized tip can interact with molecules onthe surface – giving info on bond strengths, etc.•Near Field Scanning Optical Microscopy (NSOM)-Optical technique in which a very small aperture is

    scanned very close to sample, Probe is a quartzfiber pulled to a sharp point and coated withaluminum to give a sub-wavelength aperture (~100nm), A brief introduction of few techniques is given

    below  

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    STM: scanning tunneling microscope

    nA

    R

     piezo-

    element

    e-  e- 

    e- 

    e- e- 

    e- 

    e- 

    e- 

    e- 

    < 1nm

    tunneling of electrons through

    air between probe and surface

    only conducting material

     probe

     x-y stage

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    Scanning Tunneling Microscopes (STMs)

    Monitors the electrontunneling current  between a probe and asample surface

    What is electrontunneling?

    Classical versus

    quantum mechanicalmodel

    Occurs over veryshort distances

    Scanning Probe

    Tip and surface and electron tunneling  

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    STM Tips

    Tunneling current

    depends on the

    distance between

    the STM probe andthe sample Tip

    Surface

    Tunneling current depends on distance between tip and surface 

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     x

    10 6   x 10 8    x 10 8

    STM Tips

    How do you

    make an

    STM tip

    “one atom”

    sharp?

    Let’s Zoom In!  

    e-

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    Putting It All Together

    The human hand

    cannot precisely

    manipulate at the

    nanoscale level

    Therefore,

    specialized

    materials are used

    to control the

    movement of thetip

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    AFM Tips

    The size of an

     AFM tip must

    be carefully

    chosen

     Interatomic interaction for STM

    (top) and AFM (bottom).Shading shows interaction

     strength.

    STM tip

     AFM tip

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    STM: scanning tunneling microscope

    nA

    I control  

    I tip 

    ∆I  

    R

    ∆V  

     piezo-element (changes

    length at different

    voltages)

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    MFM: magnetic force microscope

     AFM with magnetic probe

    e.g. hard disc, tape

    magnetic tip

    laser photodiode

     piezo-element

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    SNOM: scanning near-field optical microscope

    fiber tunneling of photons between

     probe and surface

    shows the amount of lightthat is

    absorbed/transmitted for

    different colors

    sample

    lens

    detector

    filter

    e.g. fluorescent molecules

    metal-coated

    fiber tip

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    Atomic Force Microscopy

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    General Applications

    Materials Investigated: Thin and thick filmcoatings, ceramics, composites, glasses,synthetic and biological membranes,metals, polymers, and semiconductors.

    Used to study phenomena of: Abrasion,adhesion, cleaning, corrosion, etching,friction, lubricating, plating, and polishing.

     AFM can image surface of material inatomic resolution and also measure forceat the nano-Newton scale.

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    How Does AFM Work?

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    Parts of AFM

    1. Laser   – 

     deflected offcantilever

    2. Mirror   – reflects laser beamto photodetector

    3. Photodetector  – dualelement photodiode that

    measures differences in lightintensity and converts to voltage

    4. Amplifier  

    5. Register  

    6. Sample

    7. Probe  – 

    tip that scanssample made of Si

    8. Cantilever   – moves asscanned over sample anddeflects laser beam

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    Necessary Components

    Indirect detection of force

    Vibration Isolation

    Flexibility of Cantilever

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     Modes of AFM

    (1) Contact Mode,

    Prob –surface separation< 0.5 nm

    (2) Non-Contact Mode

    Prob – surface separation< 0.5-2 nm

    (3)Tapping Mode (Intermittent contact),

    Prob –surface separation< 0.1-10 nm)

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    Force Measurement

    The cantilever is designed witha very low spring constant (easy

    to bend) so it is very sensitive to

    force.

    The laser is focused to reflect offthe cantilever and onto the

    sensor

    The position of the beam in the

    sensor measures the deflectionof the cantilever and in turn the

    force between the tip and the

    sample.

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    Contact Mode

    Measures repulsion between tip and sample

    Force of tip against sample remains constant

    Feedback regulation keeps cantileverdeflection constant

    Voltage required indicates height of sample

    Problems: excessive tracking forces appliedby probe to sample

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    Contact Mode

    Contact mode operates in the repulsive regime

    of the van der Waals curve

    Tip attached to cantilever with low springconstant (lower than effective spring constant

    binding the atoms of the sample together).

    In ambient conditions there is also a capillaryforce exerted by the thin water layer present

    (2-50 nm thick).

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    How It Works

    Three common types of AFM tip. (a) normal tip (3

     µm tall); (b) supertip; (c) Ultralever (also 3 µm tall)

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    Non-Contact Mode

    Uses attractive forces to interact surface with tipOperates within the van der Waal radii of theatoms

    Oscillates cantilever near its resonant frequency

    (~ 200 kHz) to improve sensitivity Advantages over contact: no lateral forces,non-destructive/no contamination to sample, etc.

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    Tapping (Intermittent-Contact) Mode

    Tip vertically oscillates between contactingsample surface and lifting of at frequency of50,000 to 500,000 cycles/sec.

    Oscillation amplitude reduced as probecontacts surface due to loss of energy causedby tip contacting surface

     Advantages: overcomes problems associatedwith friction, adhesion, electrostatic forces

    More effective for larger scan sizes

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    Figures of Merit

    Can measure surface features with

    dimensions ranging from inter-atomic

    spacing to 0.1mmResolution limited by size of tip (2-3 nm)

    Resolution of imaging 5 nm lateral and

    0.01nm vertical

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    Advantages of AFM

     AFM versus STM (scanning tunnelingmicroscope): both conductors and

    insulators AFM versus SEM (scanning electronmicroscope): greater topographiccontrast

     AFM versus TEM (transmission electronmicroscope): no expensive sampleprep.

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    Biological Applications

    Used to analyze DNA, RNA, protein-nucleic acidcomplexes, chromosomes, cell membranes, proteinsand peptides, molecular crystals, polymers,

    biomaterials, ligand-receptor bindingLittle sample prep required

    Nanometer resolved images of nucleic acids

    Imaging of cells

    Quantification of molecular interactions in biologicalsystems

    Quantification of electrical surface charge

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    P l f difi ti

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    Polymer surface modification

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    Raster the Tip: Generating an Image

    The tip passes back and forth ina straight line across the sample(think old typewriter or CRT)

    In the typical imaging mode, thetip-sample force is held constant

    by adjusting the vertical positionof the tip (feedback).

     A topographic image is built upby the computer by recording thevertical position as the tip is

    rastered across the sample.

       S  c  a  n  n   i  n  g   T   i  p

       R  a  s   t  e  r   M  o   t   i  o  n

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    Scanning the Sample

    Tip brought within nanometers ofthe sample (van der Waals)

    Radius of tip limits the accuracy ofanalysis/ resolution

    Stiffer cantilevers protect againstsample damage because theydeflect less in response to a smallforce

    This means a more sensitivedetection scheme is needed

    measure change in resonancefrequency and amplitude ofoscillation

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    Some of Pictures

    2D topographical image of Atomic Step 3D Image

    Screw dislocations on InSb grown by MBE

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    The Bad Examples

    Histogram shows level surface, butscan is very streaky

    Typically the sample will have aslight tilt with respect to the AFM.

    The AFM can compensate for this

    tilt.

    The horizontal lines are due to tip hops – 

    where the tip picks up or loses a small

    “nanodust”  

    In this image the tilt have not

    yet been removed.

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    So What Do We See?

     Nickel from an STM    ZnO from an AFM  

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    Teeny little dust mites, ultra tiny dust mites

    about 2,000 in the average bed

    http://www.micropix.demon.co.uk/sem/dustmite/article/12664_2.gif

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    Surface Roughness

    Roughness typically measured as root mean squared (RMS)

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    Carbon Nanotube Tips

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    Carbon Nanotube Tips  

    Well defined shape and composition.

     High aspect ratio and small radius of curvature.

     Mechanically robust. Chemical functionalization at tip.

    DNA

    CNT Tips

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    SPM Lithography

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     Electrochemistry: carbon nanotube used as a conducting AFM tip for localoxidation of Si.

    SPM L ithography

    M il li pede Memory

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    Millipede  is a non-volatile computer memory stored on nanoscopic pits burned into

    the surface of a thin polymer layer, read and written

    by a M icroelectromechani cal systems  (MEMS)-based probe. 

    Mil l ipede Memory

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    Mil l ipede Memory

    Canti lever Gas Sensors (Noses)

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    Canti lever Gas Sensors (Noses)