Microscopy

Scanning Probe Microscopy (SPM)

Monitor the interactions between a probe and a sample surface

Types of SPM

Scanning Probe Microscopy

History: The Scanning Tunneling Microscope (STM)
was invented by G. Binnig and H. Rohrer, for which
they were awarded the Nobel Prize in 1984
A few years later, the first Atomic Force Microscope
(AFM) was developed by G. Binnig, Ch. Gerber, and
C. Quate at Stanford University by gluing a tiny
shard of diamond onto one end of a tiny strip of gold
foil
TYPES OF SPM ?

 Atomic Force Microscopy (AFM)-Monitors the forces

of attraction and repulsion between a probe and a
sample surface
Scanning Tunneling Microscopy (STM). Tunneling of
electrons through air between probe and surface
Lateral Force Microscopy (LFM) Frictional forces
measured by twisting or sideways forces on
cantilever.
Magnetic Force Microscopy (MFM)-Magnetic tip
detects magnetic fields/measures magnetic properties
of the sample.
Electrostatic Force Microscopy (EFM)-Electrically
charged Pt tip detects electric fields/measures
dielectric and electrostatic properties of the sample

Chemical Force Microscopy (CFM)-Chemically

functionalized tip can interact with molecules on
the 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 quartz
fiber pulled to a sharp point and coated with
aluminum to give a sub-wavelength aperture (~100
nm), A brief introduction of few techniques is given
below

STM: scanning tunneling microscope

piezoelement

tunneling of electrons through

air between probe and surface
ee-

nA

e-

e-

probe
e-

e-

< 1nm

ee-

e-

x-y stage

only conducting material

Scanning Tunneling Microscopes (STMs)

Monitors the electron
tunneling current
between a probe and a
sample surface
What is electron
tunneling?
Classical versus
quantum mechanical
model
Occurs over very
short distances

Scanning Probe

Tip and surface and electron tunneling

STM Tips
Tunneling current
depends on the
distance between
the STM probe and
the sample

Tip

Surface
Tunneling current depends on distance between tip and surface

STM Tips

How do you
make an
STM tip
one atom
sharp?

Lets Zoom In!

ex
106

x 108

x 108

Putting It All Together

The human hand

cannot precisely
manipulate at the
nanoscale level
Therefore,
specialized
materials are used
to control the
movement of the
tip

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

STM: scanning tunneling microscope

piezo-element (changes
length at different
voltages)

Itip

nA
R

Icontrol

MFM: magnetic force microscope

photodiode

laser

AFM with magnetic probe

magnetic tip

piezo-element

e.g. hard disc, tape

SNOM: scanning near-field optical microscope

fiber

metal-coated
fiber tip

tunneling of photons between

probe and surface

sample

lens
filter

shows the amount of light

that is
absorbed/transmitted for
different colors

detector

e.g. fluorescent molecules

Atomic Force Microscopy

Objectives
General Applications
Background and History
How Does AFM Work?
3 Modes:
Contact mode
Non-contact mode
Tapping Mode

Figures of Merit
Advantages of AFM
Biological Applications
Future Work

General Applications
Materials Investigated: Thin and thick film
coatings, 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 in
atomic resolution and also measure force
at the nano-Newton scale.

How Does AFM Work?

Parts of AFM
1. Laser deflected off
cantilever
2. Mirror reflects laser beam
to photodetector
3. Photodetector dual
element photodiode that
measures differences in light
intensity and converts to voltage
4. Amplifier
5. Register
6. Sample
7. Probe tip that scans
sample made of Si
8. Cantilever moves as
scanned over sample and
deflects laser beam

Necessary Components

Indirect detection of force

Vibration Isolation
Flexibility of Cantilever

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)

Force Measurement
The cantilever is designed with
a very low spring constant (easy
to bend) so it is very sensitive to
force.
The laser is focused to reflect off
the cantilever and onto the
sensor
The position of the beam in the
sensor measures the deflection
of the cantilever and in turn the
force between the tip and the
sample.

Contact Mode

Measures repulsion between tip and sample

Force of tip against sample remains constant
Feedback regulation keeps cantilever
deflection constant
Voltage required indicates height of sample
Problems: excessive tracking forces applied
by probe to sample

Contact Mode
Contact mode operates in the repulsive regime
of the van der Waals curve
Tip attached to cantilever with low spring
constant (lower than effective spring constant
binding the atoms of the sample together).
In ambient conditions there is also a capillary
force exerted by the thin water layer present
(2-50 nm thick).

How It Works

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

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

Non-Contact Mode

Measures attractive forces between tip and

sample
Tip doesnt touch sample
Van der Waals forces between tip and
sample detected
Problems: Cant use with samples in fluid
Used to analyze semiconductors
Doesnt degrade or interfere with samplebetter for soft samples

Non-Contact Mode
Uses attractive forces to interact surface with tip
Operates within the van der Waal radii of the
atoms
Oscillates cantilever near its resonant frequency
(~ 200 kHz) to improve sensitivity
Advantages over contact: no lateral forces,
non-destructive/no contamination to sample, etc.

Tapping (Intermittent-Contact) Mode

Tip vertically oscillates between contacting

sample surface and lifting of at frequency of
50,000 to 500,000 cycles/sec.
Oscillation amplitude reduced as probe
contacts surface due to loss of energy caused
by tip contacting surface
Advantages: overcomes problems associated
with friction, adhesion, electrostatic forces
More effective for larger scan sizes

Figures of Merit

Can measure surface features with

dimensions ranging from inter-atomic
spacing to 0.1mm
Resolution limited by size of tip (2-3 nm)
Resolution of imaging 5 nm lateral and
0.01nm vertical

Advantages of AFM
AFM versus STM (scanning tunneling
microscope): both conductors and
insulators
AFM versus SEM (scanning electron
microscope): greater topographic
contrast
AFM versus TEM (transmission electron
microscope): no expensive sample
prep.

Biological Applications
Used to analyze DNA, RNA, protein-nucleic acid
complexes, chromosomes, cell membranes, proteins
and peptides, molecular crystals, polymers,
biomaterials, ligand-receptor binding
Little sample prep required
Nanometer resolved images of nucleic acids
Imaging of cells
Quantification of molecular interactions in biological
systems
Quantification of electrical surface charge

Polymer surface modification

Raster Motion

Scanning Tip

Raster the Tip: Generating an Image

The tip passes back and forth in
a straight line across the sample
(think old typewriter or CRT)
In the typical imaging mode, the
tip-sample force is held constant
by adjusting the vertical position
of the tip (feedback).
A topographic image is built up
by the computer by recording the
vertical position as the tip is
rastered across the sample.

Scanning the Sample

Tip brought within nanometers of
the sample (van der Waals)
Radius of tip limits the accuracy of
analysis/ resolution
Stiffer cantilevers protect against
sample damage because they
deflect less in response to a small
force
This means a more sensitive
detection scheme is needed
measure change in resonance
frequency and amplitude of
oscillation

Some of Pictures
2D topographical image of
Atomic Step

3D Image

Screw dislocations on InSb grown by MBE

The Bad Examples

Histogram shows level surface, but
scan is very streaky

The horizontal lines are due to tip hops

where the tip picks up or loses a small
nanodust

Typically the sample will have a

slight tilt with respect to the AFM.
The AFM can compensate for this
tilt.

In this image the tilt have not

yet been removed.

So What Do We See?

Nickel from an STM

ZnO from an AFM

AFM - atomic force microscopy

CD stamper

AlGaN/GaN quantum well waveguide

surface atoms on Si single crystal

polymer growth

Teeny little dust mites, ultra tiny dust mites

about 2,000 in the average bed

Topography Scanning

Example of
generated
image upon
scanning
Pd thermally evaporated on Si

Surface Roughness

Roughness typically measured as root mean squared (RMS)

Million Cantilever Wafer

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

 Dip Pen Lithography.

SPM Lithography

SPM Lithography
Electrochemistry: carbon nanotube used as a conducting AFM tip for local
oxidation of Si.

Millipede Memory

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 Microelectromechanical systems (MEMS)-based probe.

Millipede Memory

Cantilever Gas Sensors (Noses)