Advanced Characterization Techniques

Assignment# 01

Arslan Maqbool
CM2351
Advanced Characterization Techniques

ATOMIC FORCE MICROSCOPY

INTRODUCTION TO AFM
The Atomic force microscope (AFM) was developed to overcome a basic drawback with STM (it
can only image conducting or semiconducting surfaces). The AFM has the advantage of imaging
almost any type of surface, including polymers, ceramics, composites, glass, and biological
samples. It is used for surface characterization.

The AFM was invented in 1985. The original AFM consisted of a diamond tip attached to a strip
of gold foil. The diamond tip contacted the surface directly, with the interatomic van der Waals
forces providing the interaction mechanism. Probes are typically made from Si 3N4, or Si. Due to
different cantilever length and materials, spring constants and resonant frequencies can vary.

Atomic force microscopy is a powerful source of topography measurement technique of a

surface, which can be used in air, liquid or vacuum to generate images with atomic resolution.
Unlike Scanning Electron Microscopy (SEM) atomic force microscopy can generated 3D images.
Furthermore, it can provide information on nanoscale chemical, material (modulus, frictional),
electrical and magnetic properties.

WORKING PRINCIPLE
AFM is a type of Scanning Probe Microscopy (like Scanning Tunnelling Microscope (STM)) where
it uses raster scans to probe the local properties (such as topography, stiffness, friction, etc.) by
measurements of the 3D displacement of the probe tip as obtained by the piezoelectric
ceramic. The displacement of the probe is based on the measured force between the probe tip
and sample.

It is one of the most important tools for imaging on the nanometer scale, Atomic Force
Microscopy uses a cantilever with a sharp probe (<10 nm) that scans the surface of the
specimen at very short distance (0.2-10 nm probe-sample separation). The probe is placed on
the end of a cantilever (which one can think as a spring), when the tip of the probe travels near
to a surface, the forces between the tip and sample deflect the cantilever according to Hooke’s
law.

F=-k·x

F=Force

k = spring constant

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x = cantilever deflection

If the spring constant of cantilever (typically ~ 0.1-1 N/m) is less than surface, then the
cantilever bends and deflection is observed. A laser beam is used to detect cantilever
deflections towards or away from the surface. A position-sensitive photo diode (PSPD) is used
to track these changes. Thus an AFM images the topography of a sample surface by scanning
the cantilever over a region of interest. By using a feedback loop to control the height of the tip
above the surface the AFM can generate an accurate topographic image of the surface.

INSTRUMENTATION AND COMPONENTS

The atomic force between a sample and tip are measured using a laser and a detector to
monitor the cantilever motion. The sample holder moves the sample up and down via a
piezoelectric scanning tube to maintain the interaction force to a preselected level.

A three-dimensional image can finally be constructed by recording the cantilever. The piezo
stage has active feedback control with sensors for distance control. A magnetic sample holder is
attached to the stage. This assembly is fixed to the three-channel piezo stage. The set-up is
placed in a closed chamber to reduce the thermal drift. The He-Ne laser connected to the AFM
head reduces non-thermal noise which affects the stability of the laser diode. The noise power
spectra are obtained with a Fourier analyzer. The spectra are on-line fitted with resonance
curves. The cantilever chip is glued to the mount which is held by the magnets in the AFM head.

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Modes of Operation
There are multiple methods of imaging a surface using an atomic force microscope; these
imagining modes uniquely utilize the probe and its interaction with the surface to obtain data.
Hence there are 3 primary imaging modes in AFM depending whether the cantilever vibrates
during the vibration:

(1) Contact AFM (< 0.5 nm probe-surface separation)

(2) Intermittent contact (tapping mode AFM) (0.5-2 nm probe-surface separation)

(3) Non-contact AFM (0.1-10 nm probe-surface separation)

1. Contact Mode AFM:

In this mode the tip is dragged across the surface. When the spring constant of cantilever is less
than surface, the cantilever bends. The force on the tip is repulsive so by maintaining a constant
cantilever deflection the force between the probe and the sample remains constant and an
image of the surface is obtained.

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 Advantages: fast scanning, good for rough samples, used in friction analysis
 Disadvantages: at times forces can damage/deform soft samples, contamination of the
surface

2. Intermittent Mode (Tapping):

The imaging is similar to contact. However, in this mode the cantilever is oscillates at its
resonant frequency, but the oscillation amplitude is (20-200) nm. The probe lightly “taps” on
the sample surface during scanning. The tip-sample interaction alters the amplitude, resonance
frequency and phase angle of the oscillating lever. By maintaining constant oscillation
amplitude, a constant tip-sample interaction is maintained, and an image of the surface is
obtained. It is mostly suitable for imaging soft samples.

 Advantages: allows high resolution of samples , Good for biological samples

 Disadvantages: more challenging to image in liquids, slower scan speeds

3. Non-contact Mode:

In non-contact mode, the tip vibrates slightly above its resonance frequency and does not
contact the surface of the sample. The resonance frequency and amplitude of oscillating
cantilever changes as it approaches the surface due to the interactions with weak long-range
forces thus essentially imaging the surface. Using a feedback loop to monitor changes in the
amplitude due to attractive Vaander Waals forces the surface topography can be measured.
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 Advantages: Very low force exerted on the sample (10 N), so probe lifetime is
increased.
 Disadvantages: Generally lower resolution, usually need ultra-high vacuum (UHV) for
best imaging.

RESULTS INTERPRETATION
Interpreting AFM results involves understanding the topographical features, surface roughness,
mechanical properties, and other characteristics of the sample being analyzed. Here are some
key aspects to consider when interpreting AFM results:

Topography: AFM provides detailed topographical maps of surfaces, showing height variations
at the nanoscale. Analyzing these maps helps understand surface features, such as peaks,
valleys, grains, and defects.

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Surface Roughness: Quantifying surface roughness involves measuring features like average
roughness (Ra), root mean square roughness (Rq), or maximum height (Rmax). These metrics
provide insights into the surface texture and can be crucial in various applications, such as in
material science or engineering.

Material Properties: AFM can measure material properties like elasticity, adhesion, stiffness,
and friction at the nanoscale by using techniques such as force spectroscopy or
nanoindentation. These measurements aid in understanding the mechanical behavior of
materials.

Phase Imaging: Some AFM modes can capture phase contrast images that reveal differences in
material composition or properties. This can be particularly useful in distinguishing materials
with similar topography but different chemical or physical characteristics.

Sample Preparation: Proper sample preparation is critical for accurate AFM results. Variations
in sample preparation methods can significantly affect the obtained images and measurements.

Data Analysis: Advanced data analysis techniques are often used to process AFM data,
including software-based tools for extracting quantitative information and statistical analysis of
surface features.

Comparison and Correlation: Comparing AFM results with other imaging techniques or
experimental data can provide a comprehensive understanding of the sample's characteristics.

AFM Advantages (STRENGTH)

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 three-dimensional surface profile.

In addition, samples viewed by AFM do not require any special treatments (such as
metal/carbon coatings) that would irreversibly change or damage the sample, and does not
typically suffer from charging artifacts in the final image.

While an electron microscope needs a Piezoelectric scanners 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.

1. It does not require either a vacuum or the sample to undergo treatment that might
damage it.
2. The AFM can be used to study a wide variety of samples i.e. plastic, metals, glasses,
semiconductors, and biological samples such as the walls of cells and bacteria.

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3. It does not require a conductive sample.

4. It produces high resolution images in the range of nanometers.
5. There is no radiation damage of the sample.

AFM Disadvantages (LIMITATIONS)

1. The atomic force microscope is invaluable if you want to measure incredibly small
samples with a great degree of accuracy.
2. Another disadvantage is the relatively slow scan time, which can lead to thermal drift on
the sample.
3. The physical probe used in AFM imaging is not ideally sharp. As a consequence, an AFM
image does not reflect the true sample topography, but rather represents the
interaction of the probe with the sample surface. This is called tip convolution.

4. The tip health is a very crucial part in the measurement techniques. Multi peaks in the
probe due to attachment of contaminants can produce ghost image.
5. Contact and tapping mode can be regarded as destructive mode for soft samples. In
these methods the tips can also blunt very frequently.
6. External periodic vibrations such as regular power supply (50 Hz), walking, clapping,
thermal drift and capillary effect can greatly vary the observation.
7. It is quite complex and very vulnerable to outside contaminations.
8. It may damage soft samples during imaging.

APPLICATIONS OF AFM:
The AFM has been applied to problems in a wide range of disciplines of the natural sciences,
including solid-state physics, semiconductor science and technology, molecular engineering,
polymer chemistry and physics, surface chemistry, molecular biology, cell biology, and
medicine.
1. Applications in the field of solid state physics include (a) the identification of atoms at a
surface, (b) the evaluation of interactions between a specific atom and its neighboring
atoms, and (c) the study of changes in physical properties arising from changes in an
atomic arrangement through atomic manipulation.
2. Nanoindentation is a useful tool that allows the direct measurement of mechanical
properties of thin films, including polymer films AFM nanoindentation can be used for
studying the mechanical properties of ultra-thin polymer films.
3. AFM can image non-conducting surfaces. So, it was immediately extended to the
biological systems, such as analyzing the crystals of amino acids and organic polymers it
can also be used for the analysis of DNA and RNA.

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4. Elastic properties can be evaluated by using force mode of atomic force microscopy. It
gives information on the properties of various regions on the sample surface.
5. AFM can be used for evaluating the aging of polymer surfaces by mapping the
distribution of adhesion surfaces. It can be done by modifying the tip of AFM.
6. It can also be used for nanoscale mapping of mechanical properties of polymer surfaces
by means of AFM noise analysis.

FUTURE TRENDS AND INNOVATION

Traditional AFM can be relatively slow in acquiring images. Future advancements may focus on
improving the speed of data acquisition, enabling researchers to study dynamic processes at
the nanoscale in real-time. Integrating AFM with other imaging techniques, such as scanning
electron microscopy (SEM) or fluorescence microscopy, can provide complementary
information. Multimodal AFM setups may become more common, allowing researchers to
obtain a more comprehensive understanding of samples.

Enhancements in AFM probe technology and instrumentation may lead to improvements in

spatial resolution, allowing researchers to investigate structures at an even smaller scale.
Advanced techniques for quantitative mapping of mechanical properties, such as stiffness and
adhesion, are likely to be developed. This can provide deeper insights into the nanomechanical
behavior of materials and biological samples.

The capability to perform AFM measurements in situ (within a controlled environment) or in

operando (under working conditions) can expand the range of applications, especially in fields
like catalysis, electrochemistry, and biological studies. Integration of machine learning
algorithms for data analysis and interpretation can enhance the efficiency and accuracy of AFM
measurements. This may include automated image recognition, artifact correction, and real-
time analysis.

Advancements in environmental AFM techniques will likely enable researchers to study

samples in a wider range of conditions, including varying temperatures, humidity levels, and gas
atmospheres. While AFM traditionally provides 2D images, future developments may focus on
improving the ability to obtain 3D structural information at the nanoscale, providing a more
complete representation of complex samples.

AFM instrument manufacturers may continue to refine and develop user-friendly, integrated
systems, making AFM more accessible to a broader range of researchers and industries. The
development of specialized probes and sensors for specific applications, such as biological
studies or semiconductor characterization, may become more prevalent.

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CONCLUSION
AFM serves as a very powerful tool for the measurement of surface topography. Even though a
Profilometer can do the same, the lateral resolution in AFM is much better since the lateral
resolution of the Profilometer is limited by the Rayleigh criterion. Furthermore, AFM can be
used in myriad of other purposes such as determining the magnetic domains, determination of
surface friction, sample modulus, etc. AFM provides exceptional resolution, enabling
researchers to explore nanoscale structures and surfaces with unprecedented detail. Its
adaptability across diverse fields—ranging from materials science and biology to semiconductor
industry and beyond—showcases its broad utility. Integration with other microscopy
techniques and complementary methods enhances AFM's analytical power, enabling
comprehensive sample characterization. AFM allows for precise quantitative measurements of
mechanical, electrical, and chemical properties, offering insights into material behavior at the
nanoscale. The ability to perform measurements in various environments and real-time
conditions opens doors for studying dynamic processes and functional materials. As research
progresses, future developments in AFM are poised to further enhance its speed, resolution,
versatility, and applicability. These advancements will continue to expand its horizons, making
AFM an indispensable tool for scientific discovery and technological innovation in the nano
world.