Chemistry (18BSCH03) Jan-June 2020

Module 4
Nanomaterials and their spectroscopic characterization
S.No Questions Marks
1 Discuss the optical properties of nano materials. 4
 Nanomaterials exhibit a different optical property from their bulk
material,
 It depends on their size, shape and diameter which causes
difference in extinction of light.
 EXTINCTION - the reduction of the intensity of transmitted
light as a result of absorption and scattering.
 When light is incident on nanoparticle we observe extinction.
 At diameter less than 20nm, extinction involves only absorption.
 At diameter between 20-100nm, extinction involves both
absorption and scattering.
 And the size above 200nm extinction is mainly due to scattering.
 These changes causes difference in the colour between Bulk and
nanoparticle.
Eg., Gold spheres of 2-5nm exhibit yellow color.
Gold spheres of 10-20nm exhibit red color.
Gold spheres of >20nm exhibit purple color
2 Describe the electrical properties of nano materials 4
 This property depends on surface scattering of electrons and
change In crystal structure,
 The property may vary depending on the following conditions:
 Conducting nanoparticles: Reduction in size will increase in
crystal defects like frenkel defect and schotky defect, which
 creates a hole in the crystal. Also conduction can be improved by
adding impurity to it.
 Insulating nanoparticles: Reduction in size results in reduction of
structure leading to widening of band gap.
 Because of these variations some material undergo transition
from insulator to semiconductor, conductor to semiconductor,
insulator to conductor etc.,
3 Explain the magnetic properties of nano materials 4

 It depends on the size and structure of the material.

 Size ranging from 1-100nm show supermagnetism.
 These acts as single magnets.
 this makes us to control the tiny magnets by removing or
applying the field
4 Discuss the principle and instrumentation of UV-VIS Spectrophotometer 8
Principle:

 Spectrophotometry is a technique that uses the absorbance of light

by an analyte at a certain wavelength to determine the analyte
concentration. UV-Vis spectrophotometry uses liquid in UV
(190-400nm) and Visible (400-765nm) part of the
electromagnetic spectrum.
 UV−Vis spectrophotometer measures absorbance or transmittance
 from the UV range based on the principle of Lambert−Beer rule.

In this instance the value I/Io is called transmittance (T) and the
value I/Io*100 is called transmission rate (T%). The value log (1/T) =
log (Io/I) is called absorbance (Abs).

T = I/Io = 10−kcl

Abs = log (1/T) = log(Io/I) = − ɛcl

Here ɛ is proportionality constant and & l = length of light path through

the cuvette in cm.
Instrumentation:

• H2-D2 lamp with tungsten filament is used as source,

• The light passes through a monochromator containing a lens,
prism and slit to get the required wavelength
• the light is split into two equal intensity beams by a beam
splitter.
• One beam passes through a small transparent container (cuvette)
containing a solution of the compound being studied in a
transparent solvent.
• The other beam, the reference, passes through an identical
cuvette containing only the solvent.
• Quartz or fused silica cuvettes used.
• The light sensitive detector follows the sample chamber and
measures the intensity of light transmitted from the cuvettes and
passes the information to a meter that records and displays the
value to the operator on a screen.
5 Discuss the instrumentation and principle of Infrared Spectrometer. 8

 It deals with the absorption of radiation in the infrared region of

the electromagnetic spectrum (4000-1300 cm-1, 1300-400cm-1).
 IR spectrum gives sufficient information about the structure
(identification of functional groups) of a compound and can also
be used as analytical tool to assess the purity of a compound.
 The absorption of infrared radiation by a molecule causes
changes in their vibrational and rotational energy levels.


 When the energy in the form IR then if the applied frequency is
equal to vibrational frequency a peak is observed,
 These peaks are characteristic functional groups and the bonds
present in the molecule, thus IR spectrum of a compound is
considered is as the fingerprint for the chemical compound.
 Instrumentation:

 Light source is either tungsten filament,

 Beam splitter splits the light into 2 paths, one towards fixed
mirror, other towards moving mirror,
 Moving mirror when in position A gives constructive
interference and in position B gives destructive interference,
 The sample is crushed & made paste using KBr, mull oil and
pressurised to get pellets.
 Detectors are devices that convert the radiant energy into an
electrical signal

6 Explain the process of nano materials production by Sol-gel/bottom 8

up process.
Bottom-up approach: The building of nanostructures starting with
small components such as atoms or molecules is called bottom-up
approach
 • Starting material is M-OR, M is metal, R is Alkyl group
• On hydrolysis it gives M-OR it gives Sol (liquid state of
colloids)
MOR + HOH MOH + ROH
• MOH on condensation gives gel (semi solid state of colloids)
MOH + MOR MOM + ROH
The obtained sol and gel can be subjected to following processes.
• Evaporation: removal of 90% of moisture gives Xerogel
• Aeration: Replacing the moisture with dry CO2 gives Aerogel.
• Calcination: heating the compound in inert chamber at 400-
6000C for 4-5 hrs.

7 Explain the process of nano materials preparation by Mechanical 8

grinding (Ball milling)/top down process.

.Top-down approach: The process of making nanostructures starting

with larger structures and breaking away to nano size is called top-down
approach.
 This process is used in producing metallic and ceramic
nanomaterials.
 Ball mills rotate around a horizontal axis , partially filled with
the material to be ground plus the grinding medium.
 the ball milling method consists of balls many small iron,
hardened steel, silicon carbide, balls are made to rotate inside a
mill (drum).
 The material is taken inside the steel container. This material will
be made into nanosize using the ball milling technique.
 A magnet is placed outside the container to provide the pulling
force to the material and this magnetic force increases the milling
energy when milling container or chamber rotates the metal
balls.
 The ball to material mass ratio is normally maintained at 2 : 1
 After preparing the powders, annealing is done at a suitable
temperature for the certain period of time so as to get nanotubes.
Ball milling is a mechanical process and thus all the structural and
chemical changes are produced by mechanical energy.