Scanning Probe Microscopy (SPM)

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Scanning Probe Microscopy (SPM)

• A family of microscopy forms where a sharp probe is scanned


across a surface and some tip/sample interactions are monitored
• Scanning tunneling Microscopy (STM)
• Atomic Force Microscopy (AFM)
• contact mode
• non-contact mode
• TappingMode
• Other forms of SPM
• Lateral force
• Force modulation
• Magnetic or electric force
• surface potential
• scanning thermal
• phase imaging
Atomic Force Microscopy
AFM works by scanning a probe over the
sample surface, building up a map of the
height or topography of the surface as it goes
along.

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General AFM
“Beam Deflection” Detection
A Solid State
B Laser Diode

Cantilever and Tip

• Used for Contact Mode, Non-contact and TappingMode AFM


• Laser light from a solid state diode is reflected off the back of the
cantilever and collected by a position sensitive detector (PSD). This
consists of two closely spaced photodiodes. The output is then collected
by a differential amplifier
• Angular displacement of the cantilever results in one photodiode
collecting more light than the other. The resulting output signal is
proportional to the deflection of the cantilever.
• Detects cantilever deflection <1A
Different From other Microscopy
 No need of focusing, illumination, Depth of field.
 It also have height information that make it simple
to quickly measure the height, volume, width of
any feature in the sample.
 It physically feels the sample’s surface with a
sharp probe, building up a map of the height of
samples surface.
 It provides single atomic level structure so provide
high resolution.
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2. General Applications

1 2 3

Materials Used to study AFM can image


Investigated: Thin and phenomena of: surface of
thick film coatings, Abrasion, corrosion,
ceramics, composites, material in
etching (scratch), atomic resolution
glasses, synthetic and
friction, lubricating, and also measure
biological
membranes, metals, plating, and force at the
polymers, and polishing. nano-Newton
semiconductors. scale.
Further Applications
3. How Does AFM Work?
3. Continued…

Tip vibrates (105 Hz) close to specimen surface (50-150


Å) with amplitude 10-100 nm, May at times lightly
contact surface
Two ways - 'constant force' ……. feedback system
moves tip in z direction to keep force
constant.
'constant height'……. no feedback system -
usually used when surface roughness small
higher scan speeds possible.
Hooke’s Law

Hooke’s Law

F = the force acting


On the cantilever

k = the cantilever
F = -kx spring constant

x= the vertical
displacement of the
end of the cantilever.
AFM Tips
4. Parts of AFM

1. Laser – deflected off cantilever


2. Mirror –reflects laser beam to
photo detector
3. Photo detector –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
Calibration Every month

1. Z-Piezo Calibration: by scanning a sample of known height


(calibration grating)
In contact mode
2. Cantilever deflection calibration
3. Cantilever stiffness, k, calibration
Basic concept of AFM Instrumentation

The piezoelectric transducer moves the tip


over the sample surface, the force transducer
senses the force between the tip and the
surface, and the feedback control feeds the
signal from the force transducer back in to the
piezoelectric, to maintain a fixed force
between the tip and the sample.

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Piezoelectric transducers

Convert electrical potential into mechanical


motion. amorphous lead barium titanate,
PdBaTiO3 or lead zirconate titanate,
Pb[ZrxTi1–x]O3,0<x<1

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Force transducers

It may be constructed that measure forces as low as 10


piconewtons. 17
Feedback control
Feedback control is used to maintain a set
force between the probe and the sample.

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Scanning Modes
There are different imaging modes of AFM
 Contact Mode
 Non Contact Mode
 Tapping Mode

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Different modes of operation

Mode of Operation Force of Interaction

Contact mode strong (repulsive) - constant force or constant


distance.

Non-contact mode weak (attractive) - vibrating probe

Tapping mode strong (repulsive) - vibrating probe


A. 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
B. Non-Contact Mode

 Measures attractive forces between tip and


sample
 Tip doesn’t touch sample
 Van der Waals forces between tip and sample
detected
 Problems: Can’t use with samples in fluid
 Used to analyze semiconductors
 Doesn’t degrade or interfere with sample- better
for soft samples
C. 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


6. What are the limitations
of AFM?
 AFM imaging is not ideally sharp
Adv: Dis-adv:
 Easy sample preparation  Limited vertical range
 Non-destructive imaging  Limited magnification range
 Accurate height information  Highly Dependent on AFM probes.
 Works in vacuum, air, and liquids  Tip or sample can be damaged
 Living systems can be studied
 Sample not required to be conductive
Polymers, ceramics, glass
Metals
Biological samples
Application
• Digitally image a topographical surface

• Determine the roughness of a surface sample or to measure the thickness of a crystal


growth layer
• Any sample like ceramic material, human cells or individual molecules of DNA.

• In biological applications: Image non-conducting surfaces such as proteins and DNA


 Study Unfolding Of Proteins
 Imagining Of Biomolecules
 Force Measurements In Real Solvent Environments
 Antibody-Antigen Binding Studies
 Ligand-Receptor Binding Studies
 Binding Forces Of Complimentary DNA Strands

OU NanoLab/NSF
NUE/Bumm & Johnson
Example of contact mode

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Tapping mode

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Non- contact mode

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