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L-17 Characterization II

It's about nanotechnology

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0% found this document useful (0 votes)
18 views25 pages

L-17 Characterization II

It's about nanotechnology

Uploaded by

gitu0853
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
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AFM

Introduction

• High-resolution type of
scanning probe
microscopy, with
demonstrated resolution
of fractions of a nanometer,
more than 1000 times
better than the optical
diffraction limit
How It Works
• Invented in 1986
• Cantilever
• Tip
• Surface
• Laser
• Multi-segment photodetector

Figure 4. Three common types of AFM tip. (a) normal tip (3 µm tall); (b)
supertip; (c) Ultralever (also 3 µm tall). Electron micrographs by Jean-
Paul Revel, Caltech. Tips from Park Scientific Instruments; supertip
made by Jean-Paul Revel.

http://www.molec.com/what_is_afm.html
http://stm2.nrl.navy.mil/how-afm/how-afm.html#imaging%20modes
Atomic Force Microscope (AFM)
Introduction
The atomic force microscope (AFM) was invented
in1986 by Binnig, Quate and Gerber.

The AFM raster scans a sharp probe over the surface


of a sample and measures the changes in force
between the probe tip and the sample.

4
Working Concept

The physical parameter probed is a force resulting from different


interactions.
Thus, an AFM image is generated by recording the force changes as
the probe (or sample) is scanned in the x and y directions.
The sample is mounted on a piezoelectric scanner, which ensures
three-dimensional positioning with high resolution.
The force is monitored by attaching the probe to a pliable cantilever,
which acts as a spring, and measuring the bending or "deflection" of
the cantilever.

5
Principle
• Consists of a cantilever with a sharp tip (probe) at its end that is used to scan
the specimen surface

• Cantilever is typically silicon or silicon nitride with a tip radius of curvature on


the order of nanometers

• When the tip is brought into proximity of a sample surface, forces between the
tip and the sample lead to a deflection of the cantilever according to Hooke's
law

• Depending on the situation, forces that are measured in AFM include


mechanical contact force, van der Waals forces, capillary forces, chemical
bonding, electrostatic forces, magnetic forces (see magnetic force microscope,
MFM), Casimir forces, solvation forces, etc

• As well as force, additional quantities may simultaneously be measured


through the use of specialised types of probe (see scanning thermal
microscopy, photothermal microspectroscopy, etc.).
Working concept of AFM

7
Basic set-up of an AFM

The ability of an AFM to achieve near atomic scale


resolution depends on the three essential
components:
(1) a cantilever with a sharp tip,
(2) a scanner that controls the x-y-z position, and
(3) the feedback control and loop.

8
• Cantiliever with a sharp tip. The stiffness of the cantilever
needs to be less the effective spring constant holding atoms
together, which is on the order of 1 - 10 nm.

• The tip should have a radius of curvature less than 20-50 nm


(smaller is better) a cone angle between 10-20 degrees.

• 2. Scanner. The movement of the tip in the sample in the x, y,


and z-directions is controlled by a piezo-electric tube scanner.

• For typical AFM scanners, the maximum ranges for are 80 mm


x 80 mm in the x-y plane and 5 mm for the z-direction.

9
3. Feedback control. The forces that are exerted
between the tip and the sample are measured by the
amount of bending (or deflection) of the cantilever.
By calculating the difference signal in the photodiode
quadrants, the amount of deflection can be
correlated with a height .
Because the cantilever obeys Hooke's Law for small
displacements, the interaction force between the tip
and the sample can be determined.

10
Imaging Modes

• Contact Mode

• Tapping Mode

• Non contact Mode

11
Topography
• Contact Mode
– High resolution
– Damage to sample
– Can measure
frictional forces
• Non-Contact Mode
– Lower resolution
– No damage to
sample
• Tapping Mode
– Better resolution 2.5 x 2.5 nm simultaneous topographic and friction image of highly
oriented pyrolytic graphic (HOPG). The bumps represent the

– Minimal damage to topographic atomic corrugation, while the coloring reflects the lateral
forces on the tip. The scan direction was right to left
sample http://stm2.nrl.navy.mil/how-afm/how-afm.html#imaging%20modes
Contact mode
• The tip is "dragged" across the surface of the sample and the contours
of the surface are measured either using the deflection of the cantilever
directly or, more commonly, using the feedback signal required to keep
the cantilever at a constant position.

• Because the measurement of a static signal is prone to noise and drift,


low stiffness cantilevers are used to achieve a large enough deflection
signal while keeping the interaction force low.

• Thus, contact mode AFM is almost always done at a depth where the
overall force is repulsive, that is, in firm "contact" with the solid
surface.

13
Contact Mode AFM

Laser

Detector Z

Tip Cantilever
Simple
X,Y
Not too affected by humidity

Operation in liquid
Feedback: Deflection of cantilever
Damage to soft samples

Slide courtesy of Duncan Sutherland


Contact mode - short-range interactions (Å) -
interatomic forces

Tip: 5-20 nm radius, 10-25 μm high, on


50-400 μm cantilever beam

Cantilever: low stiffness - can't deform


surface

Tip contacts surface

Tip scans surface: either tip or specimen


moved by piezoelectric positioning
system over x and y
Detector system can measure deflections in
nm range
Contact mode - short-range
interactions (Å) - interatomic forces

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
Tapping mode
• The cantilever is driven to oscillate up and down at or near its
resonance frequency.
• The amplitude of this oscillation usually varies from several nm to
200 nm.
• The interaction of forces acting on the cantilever when the tip comes
close to the surface, Van der Waals forces, dipole-dipole
interactions, electrostatic forces, etc.
• This causes the amplitude of the cantilever's oscillation to change
(usually decrease) as the tip gets closer to the sample.
• This amplitude is used as the parameter that goes into the electronic
servo that controls the height of the cantilever above the sample.
• A tapping AFM image is therefore produced by imaging the force of the
intermittent contacts of the tip with the sample surface.

17
Tapping mode - long-range forces - van der Waals,
electrostatic, magnetic

Tip vibrates (105 Hz) close to


specimen surface (50-150 Å)
with amplitude 10-100 nm

May at times lightly contact


surface

Suitable for soft materials


Non contact method
• In non-contact mode, the tip of the cantilever does not contact the sample
surface.
• The cantilever is instead oscillated at either its resonant frequency or just
above (amplitude modulation) where the amplitude of oscillation is
typically a few nanometers (<10 nm) down to a few picometers.
• The van der Waals forces, which are strongest from 1 nm to 10 nm above
the surface acts to decrease the resonance frequency of the cantilever.
• Measuring the tip-to-sample distance at each (x,y) data point allows the
scanning software to construct a topographic image of the sample surface.
• Non-contact mode AFM does not suffer from tip or sample degradation
effects that are sometimes observed after taking numerous scans with
contact AFM. This makes non-contact AFM preferable to contact AFM for
measuring soft samples, e.g. biological samples and organic thin film.

19
Applications
The AFM is useful for obtaining three-dimensional topographic
information of insulating and conducting structures with lateral
resolution down to 1.5 nm and vertical resolution down to 0.05 nm.
These samples include clusters of atoms and molecules, individual
macromolecules, and biologic al species (cells, DNA, proteins).
Minimal sample preparation involved for AFM imaging.
The AFM can operate in gas, ambient, and fluid environments and
can measure physical properties including elasticity, adhesion,
hardness, friction and chemical functionality.

20
Applications

• 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
• Study Surface Frictional Forces
• Ion Channel Localization
Advantages
The AFM has several advantages over the scanning electron
microscope (SEM).
Unlike the electron microscope which provides a two-
dimensional projection or a two-dimensional image of a
sample, the AFM provides a true three-dimensional surface
profile.
Additionally, samples viewed by AFM do not require any
special treatments (such as metal/carbon coatings) that would
irreversibly change or damage the sample.

22
While an electron microscope needs an expensive
vacuum environment for proper operation, most AFM
modes can work perfectly well in ambient air or even a
liquid environment.
This makes it possible to study biological macromolecules
and even living organisms.
In principle, AFM can provide higher resolution than SEM.

23
Disadvantages
A disadvantage of AFM compared with the scanning electron
microscope (SEM) is the image size.
The SEM can image an area on the order of millimetres by millimetres
with a depth of field on the order of millimetres.
The AFM can only image a maximum height on the order of
micrometres and a maximum scanning area of around 150 by 150
micrometres.
Another inconvenience is that at high resolution, the quality of an
image is limited by the radius of curvature of the probe tip, and an
incorrect choice of tip for the required resolution can lead to image
artifacts.

24
STM vs AFM

STM collects the tunnelling current between the tip apex and the sample when
a bias voltage is applied. b | AFM detects local forces and corresponding
mechanical parameters through a spring-like cantilever

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