Atomic Force Microscopy

Presented by Psylla Christina

MSc Applied and Engineering Physics
Department of Physics
TU München
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 Outline
 Introduction
 Advantages of AFM
 Disadvantages of AFM
 How does AFM work?
- How are the forces measured?
 Experimental setup of AFM
- On which experimental parameters do the spatial resolutions depend?
- How should a successful atomic force microsope be designed and constructed?
- AFM tip
- AFM cantilever
 Imaging methods
-What types of forces are measured?
-Modes of operation: Contact Mode, Non-Contact Mode,
Tapping Mode
-What are force curves?
 Examples of AFM images
-Topography scanning
-Elimination of extreme point
-A better view
- Thickness of a Thin Layer
of Pd on Si Wafer
-Surface roughness
 References 2
 Introduction

 Atomic force microscopy is a high resolution type of scanning probe

microscopy that allows us to see and measure surface structure in length
scale 10nm-100μm with unprecedented resolution and accuracy
(lateral resolution~30 nm, vertical resolution~0.1 nm)

 Unlike an imaging traditional microscope, AFM provides height information

of the sample

 Almost any sample can be imaged, be it very hard (ceramic material) or

very soft (human cells, individual molecules of DNA)

 We can generate images which look at the sample from any conceivable
angle with simple analysis software

 Currently AFM is the most common form of scanning probe microscopy and
is used in all fields of science as chemistry, biology, physics, materials
science, nanotechnology, astronomy, medicine and more

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 Advantages of AFM

 minimal sample preparation

 it does not require a conductive sample

 provides a three-dimensional surface profile (ability to magnify in the X,Y,Z

axes)

 works perfectly well in ambient air or even a liquid environment

 possible to study biological macromolecules and even living organisms

 it does not require expensive equipment

 due to its small size, it can also be combined with other microscopes or
intruments

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 Disadvantages of AFM

 not practical to make measurements on areas greater than 100μm

 limited scanning speed, requiring several minutes for a typical scan

 images can be affected by nonlinearity, hysterisis and creep of the

piezoelectric material

 possibility of image artifacts

 an AFM image does not reflect the true sample topography, but rather
represents the interaction of the probe with the sample surface

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 How does AFM work?
 AFM provides a 3D profile of the
surface on a nanoscale, by
measuring forces (Van der Waals
forces, dipole-dipole interactions,
electrostatic forces) between a
sharp probe (<10 nm) and surface at
very short distance (0.2-10 nm
probe-sample separation)

 the probe is supported on a flexible

cantilever

 the AFM tip “gently” touches the

surface and records the small force
between the probe and the surface

 forces between the tip and the

sample lead to a deflection of the
cantilever according to Hooke´s law

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 How are the forces measured?

 the probe is placed on the end of

a cantilever (which one can think
of as a spring)

 the amount of force between the

probe and sample is dependent
on the spring constant (stiffness of
the cantilever) and the distance
between the probe and the
sample

 this force can be described using

Hooke’s Law:
F=-k·x

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Experimental setup of AFM

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 The cantilever is a bendable
structure used to hold the tip. It is
basically a spring with stiffness k
 The piezoelectric materials are
used for controlling the motion of
the probe as it is scanned across
the sample surface
 A laser beam is reflected by the
back side of a reflective cantilever
onto the photodetector
 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
 The feedback loop includes all of
the structural elements that are
required to hold the probe at a
fixed distance from the sample.

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On which experimental parameters do the spatial
resolutions depend?

 Τhe vertical resolution (~ Å)  The lateral resolution

depends on: (~ Å to few tens of nm)
depends on:
• Laser intensity noise
• Positionning noise of piezo-
• Photodiodes’noise ceramics X,Y

• Thermal noise of cantilever • Tip sharpness

• Positionning noise of • Long or short range interaction

piezo-ceramic Z

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How should a successful atomic force microsope be
designed and constructed?

 A very sharp probe must be constructed for measurement of high-resolution

images

 A feedback controller that permits rapid control so that the probe can follow
the topography on the surface must be created

 An X-Y-Z piezoelectric scanner that has linear and calibrated motion must
be created

 A stucture that is very rigid must be constructed, so that the probe does not
vibrate relative to the surface

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 AFM TIP
The tip of the AFM is used:

 for imaging
 for measuring forces (and mechanical properties) at the nanoscale
 as a nanoscale tool, i.e. for bending, cutting and extracting soft materials
 high-resolution image control

In AFM all what is «seen», is seen by the tip, so everything depends on its
shape

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 AFM TIP

 AFM tips with a polygon based

pyramid shape positioned close to
the free end of the AFM cantilever

 Macroscopic half-cone angle 20°

to 25° viewed along the cantilever
axis, 25° to 30° viewed from the
side

 Half-cone angle smaller than 10°

at the apex

 AFM tip height ~10-17 µm

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 AFM TIP

Conical tips are more preferable than pyramidal tips

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AFM artifact arising from a tip with a high radius of curvature with respect to
the feature which is to be visualized

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 AFM CANTILEVER

 cantilevers are commonly fabricated from silicon, silicon nitride, or polymers

 the fabrication process typically involves undercutting the cantilever

structure often with an anisotropic wet or dry etching technique

 without cantilever transducers, AFM would not be possible

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 Two equations are key to understanding the behavior of the cantilever:

The first is Stoney's formula, which relates cantilever end deflection δ to applied
stress σ:

where ν is Poisson’s ratio, E is Young’s modulus, L is the beam length and t is

the cantilever’s thickness.

The second is the formula relating the cantilever spring constant to the cantilever
dimensions and material
constants:

where F is force and w is the cantilever width.

The spring constant ω0 is related to the cantilever resonance frequency by the

usual harmonic oscillator formula:

A change in the force applied to a cantilever can shift the resonance frequency.
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Imaging methods
 Contact mode
• tip is in contact with the substrate
• high resolution
• can damage fragile surfaces

 Non-contact mode (NCM)

• tip is oscillating and not touching the
sample

 Tapping mode
• tip is oscillating and taps the surface

 Lateral force microscopy (LFM)

• tip is scanned sideways
• used to measure friction forces on the
nanoscale

 Force Modulation Microscopy

• rapidly moving the tip up and down
while pressing it into the sample.
• possible to measure the hardness of
the surface and characterize it
mechanically
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Imaging methods
 Electrical force microscopy
• If there are varying amount of charges
present on the surface, the cantilever
will deflect as it is attracted and
repelled

 Kelvin probe microscopy

• By applying an oscillating voltage to an
oscillating cantilever in non-contact
mode and measuring the charge
induced oscillations, a map can be
made of the surface charge
distribution

 Magnetic Force Microscopy

• If the cantilever has been magnetized
it will deflect depending on the
magnetization of the sample.

 Liquid sample AFM

• Immersing the cantilever in a liquid
• Image wet samples

 Electrochemical AFM
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 What types of forces are measured?

 The dominant interactions at short

probe-sample distances in the
AFM are Van der Waals (VdW)
interactions

 During contact with the sample,

the probe predominately
experiences repulsive Van der
Waals forces (contact mode)

 As the tip moves further away

from the surface attractive Van der
Waals forces are dominant (non-
contact mode)

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 Modes of operation

There are 3 primary imaging

modes in AFM:

 Contact AFM (< 0.5 nm probe-

surface separation)

 Intermittent contact (tapping mode

AFM) (0.5-2 nm probe-surface
separation)

 Non-contact AFM (0.1-10 nm

probe-surface separation)

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 Contact mode (repulsive VdW)

 When the spring constant of cantilever is less than surface, the cantilever
bends

 The force on the tip is repulsive

 By maintaining a constant cantilever deflection (using the feedback loops)

the force between the probe and the sample remains constant and an
image of the surface is obtained.

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 Contact mode

Advantages Disadvantages

 High resolution  High contact pressure (GPa)

 Fastest of all the topographic  Lateral forces are experienced by

modes both probe and sample

 No problem with surface pollution  Tip sharpness is limited and so

(Imaging in air and liquid is does lateral resolution
possible)
 It can modify/destroy the observed
 Measurement of physical surfaces, so no soft materials can
parameters like electrical and be used
thermal properties

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 Non-Contact mode (attractive VdW)

 The probe does not contact the sample surface

 The cantilever is oscillated near its resonant frequency (about 100 to 400 kHz)
with an amplitude of a few nanometers (<10 nm)

 As the tip comes near the sample surface, the system detects variations in the
resonant frequency or vibration amplitude

 The frequency deviation is used to make an image of the sample

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A virus coated on a multilayered polymer surface
was imaged. The delicate surface of the virus
can be clearly seen from the phase information
acquired by Non-Contact mode. 26
 Non-contact mode

Advantages Disadvantages

 soft materials (very low force  low lateral resolution because

exerted on the sample(10-12 N) of the long range forces

 no limitation in tip’s sharpness  surface pollution

 extended probe lifetime  usually needs ultra high

vacuum (UHV) for better
imaging

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 Tapping mode

 The imaging is similar to contact

 The cantilever is driven to oscillate

up and down at near its resonance
frequency by a small piezoelectric
element mounted in the AFM tip
holder

 The probe lightly “taps” on the

sample surface during scanning,
contacting the surface at the
bottom of its swing

 The amplitude is used for the

feedback and the vertical
adjustments of the piezoscanner
are recorded as a height image
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 a: the oscillation amplitude of the
cantilever is constant,
representing the “free space”
situation where there is no
interaction between the tip and the
surface
 b: the amplitude decreases when
the tip approaches close enough
to the sample surface so that it
“feels” attractive and/or repulsive
forces
 c: The cantilever stops oscillating
when the tip is brought in to
mechanically contact the surface

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 Tapping mode

Advantages Disadvantages

 improved lateral resolution (~ 5 nm)  5 to 10 times slower than contact

compared to contact mode and non- mode (We need 5-20 minutes to
contact mode (short range repulsive obtain an image)
forces dominate)
 tip is damaged after several scans
 reduced forces applied on surface
compared to contact mode (so we
can observe soft materials)
 no friction forces, so sharper tips can
be used
 pollution layer is not a problem
(works in air, liquids)

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Epitaxial Silicon (1x1μm2)

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 What are force curves?

 Force curve analyses can be used to determine chemical and mechanical

properties such as adhesion, elasticity, hardness and rupture bond lengths

 Force curves measure the amount of force felt by the cantilever as the
probe tip is brought close to - and even indented into - a sample surface
and then pulled away

 In a force curve analysis the probe is repeatedly brought towards the

surface and then retracted

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 The slope of the deflection (C)
provides information on the
hardness of a sample

 The adhesion (D) provides

information on the interaction
between the probe and sample
surface as the probe is trying to
break free

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Examples of AFM images

Topography Scanning

Example of generated image upon

scanning Pd thermally evaporated
on Si

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Elimination of Extreme Points

This targets the highest points of

the sample and eliminates them
It then manipulates the image to
create a smaller dynamic depth

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 A better view

Now:

 Removed extreme points

 Digitally decreased the height of

analysis

 Less than 1/3 as high

as initial scan

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Thickness of a Thin Layer
of Pd on Si Wafer

Systematic error

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Surface roughness

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 References

 “Atomic Force Microscopy” by Peter Eaton and Paul West

 “Atomic Force Microscopy & CT-AFM” by K.Bouzehouane

 Automatic drift elimination in probe microscope images based on

techniques of counter-scanning and topography feature
recognition”Yurov, A. N. Klimov (1994)

 “Scanning tunneling microscope calibratiion and reconstruction of real

image: Drift and slope elimination” G. Schitter, M. J. Rost (2008)

 Introduction to Scanning Probe Microscopy (SPM) Basic Theory Atomic

Force Microscopy (AFM) Robert A. Wilson and Heather A. Bullen,*
Department of Chemistry, Northern Kentucky University, Highland
Heights, KY 41099.

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