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ATOMIC FORCE MICROSCOPY

PRESENTED BY
VijAY S Khoiwal

BRANCHES OF MICROSCOPY
There are three well-known branches of
microscopy,
Optical microscopy,
Electron microscopy, and
scanning probe microscopy.

TYPES OF SCANNING PROBE MICROSCOPY


Atomic Force Microscopy (AFM)
Scanning Tunneling Microscopy (STM)
Lateral Force Microscopy (LFM)
Magnetic Force Microscopy (MFM)
Electrostatic Force Microscopy (EFM)
Chemical Force Microscopy (CFM)
Near Field Scanning Optical Microscopy (NSOM)

CHARACTERISTICS OF COMMON
MICROSCOPIC TECHNIQUES

SCANNING PROBE MICROSCOPY


PRINCIPLE
Scans an extremely sharp tip (3-50 nm
radius of curvature) across the object
surface.
Tip mounted on a flexible cantilever,
allowing it to follow the surface profile
Forces of interaction between the tip
and the surface influence the
movement of the cantilever.
These movements are detected by
selective sensors.

PRINCIPLEOFAFM
The AFM brings a probe in
close proximity to the surface
The force is detected by the
deflection of a spring, usually
a cantilever.
Forces between the probe
tip and the sample are
sensed to control the
distance between the the tip
and the sample.

Schematic of AFM operation

AFM TIP
Tips have a pyramidal
geometry.

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


tall); (b) supertip; (c) Ultralever (also 3 m tall).
Electron micrographs by Jean-Paul Revel, Caltech.
Tips from Park Scientific Instruments; supertip made
by Jean-Paul Revel.

AFM TIP
One of the most important factors influencing the resolution which may be
achieved with an AFM is the sharpness of the scanning tip. Best tips may
have a radius of curvature of only around 5nm.

The tip is rounded off so the end radius is taken.

CANTILEVERS
AFM Cantilevers are specified by their width, length, and
thickness.
These parameters determine important factors like
resonance frequency and spring constant.

MODES IN AFM
MODES OF OPERATION

FORCES OF INTERACTION

CONTACT MODE

strong (repulsive) constant force or


constant distance

NON CONTACT MODE

weak (attractive)-vibrating probe.

INTERMITTENT CONTACT
MODE/TAPPING MODE

strong (repulsive) - vibrating probe.

Contact Mode
High resolution
Damage to sample
Can measure frictional forces
Non-Contact Mode
Lower resolution
No damage to sample
Tapping Mode
Better resolution
Minimal damage to sample

Contact(repulsive) Non-contact (attractive)

Tapping

Working mode
Sliding the probe tip across surface, heavily influenced by
frictional and adhesive forces, which can damage samples
and distort image data.
Sensing Van der Waals attractive forces between surface
and probe tip held above surface (50 - 150 ), low
resolution and can also be hampered by the contaminant
layer which can interfere with oscillation.
Tapping the surface with an oscillating probe tip,
eliminates frictional forces by intermittently contacting
the surface and oscillating with sufficient amplitude to
prevent the tip from being trapped by adhesive meniscus
forces from the contaminant layer.

Sample Preparation for AFM Particle


Characterization

METHOD OF SAMPLE PRREPARATION DEPENDS ON ENVIRONMENTAL


MEDIA

Medium
Imaging
in air

Imaging
in liquids
Imaging
of
embedde
d
particles

Example
Dry powder
Carbon nano tube

Method
substrate is chemically treated and dry, it is immediately
ready for powder deposition
diluted dispersant suspensions of carbon nanotubes
are spin coated on a silicon wafer

Absorption on a polycationic treated surface or on an


agarose coating then fixing agent is added.

Bio-particles in buffer

Soft and bio-materials


Hard materials

A microtone is typically used to produce 0.5 micron or


thinner slices Thin films can be spin coated on silicon
or a glass substrate
etching technique

AFM FOR NANOMATERIAL


CHARACTERIZATION
(cellulose nano crystals)
SAMPLE PREPARATION
TRAVERSE ELASTIC MODULUS
STIFFNESS MEASUREMENT
TOPOGRAPY
TIP SURFACE ADHESION
BENDING RIGIDITY

Atomic Force Microscopy Characterization of Cellulose Nanocrystals :Roya R. Lahiji,Xin Xu,Ronald


Reifenberger, Arvind Raman,Alan Rudie, and Robert J. Moon*,: 2010 American Chemical Society

SAMPLE PREPARATION
DEPOSITION ON FRESHLY
PREPARED MICA SHEET

2% Wt CNC
conc.

Washing with deionized water

Force displacement in AFM

I slope:
Cantilever- CNC stiffness
Modulus of CNC
Elastic response

Pull off forces:


Tip-surface interaction
Adhesion
Sufcace chemistry of CNC

Indentation

Approach
Withdraw

At any applied force value, the corresponding


difference in z-distance between the F(z) curves
provides a measure of the CNC indentation at
that force value
d = cantilever bending +nano
crystal

Indentation
length

TRAVERSE ELASTIC MODULUS


Theoretical value

Three-dimensional quartersymmetry model of the CNC-AFM


indentation

Experimental value

Continued.
The resulting F() curve can be fitted to physics-based
models that predict the AFM tip-substrate contact
mechanics, and the elastic modulus can be estimated by
tuning the theoretical elastic modulus value to match the
theoretical prediction with observed data.

Traverse elastic modulus:


E= 18-50 mPa
Mean = 35 mPa

STIFFNESS MEASUREMENT
Keff (effective stiffness) = Kc(cantilever stiffness) +Ksample (stifness b/w tip and sample)
The slope of the F(z) = dF/dz
dF/dz

The effective stiffness contrast between mica and


CNC can come due to
meniscus effects caused by moisture
condensing
contact geometry effects,
material property effects

TOPOGRAPY

Observation: variable height


(2-8nm)
Length (100nm-300nm)
RH influence:
Not remarkable

Tip surface adhesion


Observation:
Measured in jumping mode
No CNC height effect
Edge effect
Almost uniform along the length
Affecting parameters:
Rh in adhesion due to
meniscus effect of water
Contact geometry also affects

Bending rigidity
Measured in contact-mode AFM by pushing an AFM tip
against a CNC
By increasing the normal force into the 8-10 nN range, it
was observed empirically that crystals A and B( 3-5 nN were
insufficient to cause the relative motion )
The small radius of the bending curvature (i.e., large
amount of bending over an 100 nm crystal length
stiffening contribution of interhydrogen bonding between
neighboring cellulose chains within the crystalline cellulose
will resist local cellulose chain deformation resulting from an
applied load.

dynamic-mode AFM
topography images of two
CNCs prior to and after
manipulation (crystals A
and B)

Indicating direction of force

APPLICATIONS
Nanostructures
Bucky balls and nanotubes.
Surface of polymers
Diffraction grating
Integrated circuits.
pharmaceutical research, including drug
polymorphic discrimination ,
determination of intrinsic dissolution rate of
crystal planes,
quantitation of adhesion between powders and
particles and gelatine surfaces ,
For characterisation of nanoparticles

ADVANTAGES OF AFM
Does not require vacuum to operate.
Gives a 3D topographical representation of the
surface of the sample.
Can give additional information about the physical
characteristics of the material like co-efficients of
friction.
Nanomanipulation.

Limitations:

Nonlinear behaviors in TM complicate the analysis of the data in terms of


quantitative surface mechanical properties
Indirect force modulation, generally realized by modulating either the height of
the sample or that of the cantilever holder, induces shear stress of the contact due
to the AFM configuration. Friction properties are thus mixed in the data leading
to possible artifacts and make it difficult to realize true elastic imaging of surface
Shear deformation or tip sliding may interfere in the measurements .

THANK
YOU