Wa0011.

Unit -3 (Characterization techniques for Nanomaterials)
(I) Optical Microscopy
The optical microscope often referred to as the light microscope, is a type of microscope that
uses visible light (wavelength) and a system of lenses to magnify images of small subjects.
Modern developments in CMOS and charge-coupled device (CCD) cameras allow the
capture of digital images. Purely digital microscopes are now available which use CCD
camera to examine a sample, showing the resulting image directly on a computer screen
without the need for eyepieces.
There are two basic types of optical microscopes: Simple microscopes & Compound
microscopes. A simple microscope is one that uses a single lens for magnification, such as a
magnifying glass while a compound microscope uses several lenses to enhance the
magnification of an object. For viewing and analysing morphologies of materials (nano or
micro materials) generally compound microscopes are being used.
The Principle: An optical microscope creates a magnified image of an object specimen with
an objective lens and magnifies the image further more with an eyepiece to allow the user to
observe it by the naked eye or captured through sophisticated cameras.
The working:
The Basic components:
Applications:
(2) Scanning Electron Microscopy (SEM)
Principle:
Instrumentation and Working
Instrumentation:
Working:
Comparison between SEM and TEM
(3) Transmission Electron Microscopy (TEM)
A Transmission Electron Microscope (TEM) utilizes energetic electrons to provide

morphologic, compositional and crystallographic information on samples.
At a maximum potential magnification of 1 nanometer, TEMs are the most powerful
microscopes. TEMs produce high-resolution, two-dimensional images, allowing for a wide
range of educational, science and industry applications.
Principle:
Working:
Diagram to represent TEM’s working

Specimen/Sample Preparation
A TEM specimen must be thin enough to transmit sufficient electrons to form an image with
minimum energy loss. Therefore specimen preparation is an important aspect of the TEM
analysis. For most electronic materials, a common sequence of preparation techniques is
ultrasonic disk cutting, dimpling, and ion-milling. Dimpling is a preparation technique that
produces a specimen with a thinned central area and an outer rim of sufficient thickness to
permit ease of handling. Ion milling is traditionally the final form of specimen preparation. In
this process, charged argon ions are accelerated to the specimen surface by the application of
high voltage. The ion impingement upon the specimen surface removes material as a result of
momentum transfer.
Applications
TEM gives information about: topography (the surface features of a sample), morphology
(the shape and size of the particles), composition (the elements and compounds that present
in the given sample) and crystallographic information (how the atoms are arranged in the
sample).
Industrial Purpose
Educational/Academic Purpose
Advantages and Disadvantages

Difference between Optical Microscope and Electron Microscope
(4) Atomic Force Microscopy (AFM)
The atomic force microscope (AFM) is one kind of scanning probe microscopes (SPM),
invented by G. Binning and H. Rohrer in 19881. AFM has been becoming a more and more
important instrument in nano science and technology.
AFM Working Principle
The AFM principle is based on the cantilever/tip assembly (commonly referred to as the
probe) that interacts with the sample. The AFM probe interacts with the substrate through a
raster scanning motion. The up/down and side to side motion of the AFM tip as it scans along
the surface is monitored through a laser beam reflected off the cantilever. This reflected laser
beam is tracked by a position sensitive photo-detector (PSPD) that picks up the vertical and
lateral motion of the probe. The deflection sensitivity of these detectors has to be calibrated in
terms of how many nanometers of motion correspond to a unit of voltage measured on the
detector.
Schematics of AFM working

Advantages Disadvantages/Limitations
 No lenses and light sources are  It can only image a maximum height
needed in the order of 10-20 μm and
 Both conducting and nonconducting maximum scaning area of about 150
samples can be analysed x150 μm2
 3 Dimensional images are obtained  The scanning speed is limitted
 No need of vacuum: samples can be  Highly dependent on AFM probes
analysed in open air (data not independent of tip)
 Easy sample preparation  Tip or sample can be damaged
 Along with sample morphology and
topography, the rms roughness of the
sample can be measured
 Living system (bacteria,DNA, RNA,
tissues, etc) can be studied
Applications: Applications of atomic force microscopy (AFM) include biochemistry
applications (imaging the structure of biological molecules, cellular components, cells or
tissues), chemistry, materials science and nanotechnology applications (imaging of polymers,
nanostructures or other materials) and physics and biophysics applications (measuring forces
between the AFM tip and the sample surface).
Comparision between AFM, SEM and TEM

(5) Scanning Tunneling Microscopy (STM)
The development of the family of scanning probe microscopes started with the original
invention of the STM in 1981. Gerd Binnig and Heinrich Rohrer developed the first working
STM while working at IBM Zurich Research Laboratories in Switzerland. This instrument
would later win Binnig and Rohrer the Nobel prize in physics in 1986.
How an STM Works
The scanning tunneling microscope (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.
Principles and working: The STM is based on several principles. One is the quantum
mechanical effect of tunneling. It is this effect that allows us to “see” the surface. Another
principle is the piezoelectric effect. It is this effect that allows us to precisely scan the tip with
angstrom-level control. Lastly, a feedback loop is required, which monitors the tunneling
current and coordinates the current and the positioning of the tip. This is shown schematically
below where the tunneling is from tip to surface with the tip rastering with piezoelectric
positioning, with the feedback loop maintaining a current setpoint to generate a 3D image of
the electronic topography:
Working of STM
Applications/Uses
(6) X-Ray Diffraction (XRD)
Diffraction techniques using X-rays produce information about crystal structure, and are used
to understand structure (Bravais lattice) of bulk materials and can be extended to investigate
nanomaterials. However the usual diffraction analysis relies on the long range periodic
arrangement of atoms/molecules.
What are X-rays?
X-ray diffraction and working

The XRD pattern of Nanomaterials
Prepared by Dr A B Panda for 6th Sem students Physics Hons

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Unit -3 (Characterization techniques for Nanomaterials)

(I) Optical Microscopy

Instrumentation and Working

A Transmission Electron Microscope (TEM) utilizes energetic electrons to provide

Diagram to represent TEM’s working

Advantages and Disadvantages

(4) Atomic Force Microscopy (AFM)

AFM Working Principle

Schematics of AFM working

Comparision between AFM, SEM and TEM

How an STM Works

(6) X-Ray Diffraction (XRD)

X-ray diffraction and working

Prepared by Dr A B Panda for 6th Sem students Physics Hons

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