Scanning Probe Microscopy

Nanotechnology II
Nanotechnology II

•  At the end of this module you will be able to;

–  Apply the fundamental principles that underpin nanotechnology
materials and devices
–  Explain the conventional and emerging synthesis techniques
available for nanomaterials
–  Apply different nanochemistry concepts in order to manipulate
nanoscale materials
–  Explain the role of Nanotechnology in society and the constraints
within which their engineering judgment will be exercised
–  Evaluate and analyze the mechanical, chemical and other
properties of bulk nanostructured metals, nanocomposite and
carbon nanotubes depending on their requirement
–  Maintain an open and questioning mind toward new ideas and
alternative points of view on Nanotechnology
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There is plenty of room at the bottom

“But I am not afraid to consider the final question as to

whether, ultimately – in the great future – we can arrange
the atoms the way we want; the very atoms, all the way
down! …
when we have some control of the arrangement of
things on the small scale we will get an enormously
greater range of possible properties that substances can
have, and of different things that we can do.

What would the properties of materials be if we

could really arrange the atoms the way we want them?”

Richard P. Feynman (1964)

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Size scales from human to atom

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Imaging ranges for different microscopy techniques

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Concept: Eye and Finger

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Advanced microscopy

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Scanning Probe Microscopy

•  The principle of scanning probe microscopes is

to move a sharp tip close to a surface in order
to measure various properties with a spatial
resolution on the nanometer or even atomic
scale.

•  The first kind of scanning probe microscope, the

scanning tunneling microscope, (STM) was
invented in 1981/1982 by Binnig and Rohrer who
received the Nobel prize in physics 1986 for this
invention.
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History of SPM
•  1972 Development of the Topografiner (precursor of the STM).
•  1981 Construction of the first STM by Binnig, Rohrer, Weibel
and Gerber.
•  1982 First image of the atomic structure of the Si (111)-(7×7)
surface by Binnig, Rohrer, Weibel and Gerber.
•  1985 Invention of the atomic force microscope (AFM) by
Binnig, Quate and Gerber.
•  1986 Nobel prize in physics for the invention of the STM
awarded to Binnig and Rohrer.
•  1987 Element-sensitive imaging of GaAs by Feenstra.
•  1990 Optical beam deflection method introduced by Meyer
and Amer.
•  1990 First positioning of single atoms on a surface with a low
temperature STM by Eigler.
•  1993 Tapping mode introduced by Zhong, Inniss, Kjoller, and
Elings.
•  1995 First atomic resolution with an AFM by Giessibl. • 1998
First vibrational spectroscopy with the STM by Stipe and Ho.

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1. Scanning tunneling Microscopy
STM

•  The STM works by scanning a very sharp metal

wire tip over a surface. By bringing the tip very
close to the surface, and by applying an
electrical voltage to the tip or sample, we can
image the surface at an extremely small scale –
down to resolving individual atoms.

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Operational principle - STM

•  A voltage is applied between the tip and the

(conducting) sample.

•  The tip is approached toward the sample surface until a

current flows. A current (the tunneling current) can be
detected shortly before tip and sample come into direct
contact.

•  This happens at distances between tip and sample of

the order of 0.5–1 nm.

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Operational principle - STM

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Principle of STM

The tunneling current increases with

decreasing tip-sample distance. Thus a
certain measured tunneling current
corresponds to a specific tip-sample
distance.
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Operational principle - STM
•  While the tip is scanned along the surface in x and y
directions, a feedback mechanism constantly adjusts the
tip height by approaching or retracting the tip to a tip-
sample distance at which the tunneling current
remains constant.
•  If there is an atomic step at the surface, and the tip
approaches this step edge, the tunneling current will rise
due to the smaller distance between tip and sample.
•  As a reaction to this the feedback circuit will retract the
tip in order to maintain a constant tunneling current, i.e. a
constant tip sample distance.
•  Recording the feedback signal (tip height) as a function
of the lateral position results in a map (or image) of the
tip height, which often corresponds to the surface
topography of the sample surface. 15
Operational principle - STM

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17
Modes of Operation - STM

•  Constant current mode

–  By using a feedback loop, the tip is vertically adjusted
in such a way that the current always stays constant.
A kind of a topographic image of the surface is
generated by recording the vertical position of the tip.
•  Constant height mode
–  In this mode the vertical position of the tip is not
changed. This mode is only appropriate for atomically
flat surfaces as otherwise a tip crash would be
inevitable. One of its advantages is that it can be used
at high scanning frequencies (up to 10 kHz).

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Technical challengers

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Positioning

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Piezoelectric materials

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Poling/polarization

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Polarization

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Piezoelectric phenomenon

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Piezoelectric materials

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Piezoelectric tube actuator

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Piezoelectric motors

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Coarse positioners

•  Mechanical Positioner
The tip approaches the sample with the help of springs.

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Vibration Isolation

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Vibration Isolation

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Vibration Isolation

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Vibration Isolation

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Vibration Isolation materials

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Transmissibility

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Isolation Insertion loss

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Atomic Force Microscopy

(AFM)
Atomic Force Microscope (AFM)

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The First AFM

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AFM

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Cantilever

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AFM tips

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The physics of AFM

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STM vs. AFM
STM
Not true topographic imaging because it
measures electron density of states, not
nuclear positions
High lateral and vertical resolution
Probe electronic properties
Sensitive to noise
Image quality depends on tip conditions
No direct chemical identification
Only for conductive materials
AFM
Real topographic imaging
High lateral and vertical resolution
Probe various physical properties
including magnetic, electrostatic, friction
and elastic modulus.
Can manipulate molecules and fabricate
nanostructures
Image quality depends on tip conditions
No direct chemical identification
Contact mode can damage the sample
Apply to both conducting and non-
conducting materials
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Introduction

Instead of the tunneling current, which is

the measured quantity in STM, in an
atomic force microscope
- the force between the tip and sample is
measured

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Force-distance curve
•  Three different regimes can
be distinguished.
–  (a) If the tip is far away from
the surface the force between
tip and sample is negligible.
–  (b) For closer distances an
attractive (negative) force
between tip and sample
occurs.
–  (c) For very small distances a
strong repulsive force
between tip and sample
occurs.
One problem with this behavior is that the tip-sample force depends non-
monotonously on the tip-sample distance, i.e. for one value of the measured
force in the attractive regime there are two tip-sample distances, point 1 and
point 2 on the force distance curve
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Atomic force

•  How can you measure the force between

tip and the sample?

The force between tip and sample can be measured in

a static mode using the deflection of the cantilever on
which a tip is mounted.

The cantilever acts as a spring and its deflection is

proportional to the tip-sample force.

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How to measure the force?

•  If the stiffness of the cantilever spring k (spring constant)

is known, the force between tip and sample can be
determined by measuring the bending of the cantilever.

•  Hooke’s law gives F = −kz, where F is the force and z is

the distance the cantilever spring is bent relative to its
equilibrium position without the sample present

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Deflection of the cantilever

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Deflection of the cantilever

•  How to measure the deflection of

cantilever?

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Operational principle

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Principles of AFM

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Principles of AFM

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AFM image acquisition at constant force

•  Mironov: Fundamentals of scanning probe microscopy, 2004

Modes of Operation
Contact mode

Non-contact mode

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Contact mode

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Contact mode

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Non-contact mode

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Non-contact mode

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Topography

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AFM on butterfly wing surface

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AFM Phase imaging
Phase Imaging refers to the monitoring of the phase lag between the
signal that drives the cantilever oscillation and its output signal as shown
in Figure 1. Changes in the phase lag reflect changes in the mechanical
properties of the sample surface.

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Phase image of block copolymer

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Polyurethanes with peptides

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AFM phase image
Polystyrene-polybutadiene blend on silicon substrate

Topography image Phase image

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What can you measure with AFM?

•  Topography
–  True measurement of z (height) enables
roughness analysis
•  Morphology based on mechanical or
material contrast
–  Phase imaging
•  Mechanical properties
–  Stiffness (modulus) and adhesion

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