PHOTOCATALYTIC PERFORMANCE OF MGO FOR PHOTOCATALYTIC

DEGRADATION OF MALACHITE GREEN DYE UNDER VISIBLE LIGHT

Submitted to
GOBI ARTS & SCIENCE COLLEGE (Autonomous)
GOBICHETTIPALAYAM
Affiliated to BHARATHIAR UNIVERSITY, COIMBATORE
In partial fulfilment for the award of the degree of
MASTER OF SCIENCE IN PHYSICS
Submitted by

THIYAGARAGAN K
[21-08-139]

Under the guidance of

Mrs. S. KAVITHA M.Sc., M.Phil.,
Assistant professor of physics

Department of physics
GOBI ARTS &SCIENCE COLLEGE (Autonomous)
(An Autonomous institution affiliated to Bharathiar University, Coimbatore and
Reaccredited by NAAC with “A” Grade)
Gobichettipalayam – 638453
APRIL-2023
 CERTIFICATE

This is to certify that the dissertation entitled “PHOTOCATALYTIC

PERFORMANCE OF MgO FOR PHOTOCATALYTIC DEGRADATION
OF MALACHITE GREEN DYE UNDER VISIBLE LIGHT ” submitted to
GOBI ARTS & SCIENCE COLLEGE (Autonomous), Gobichettipalayam in
partial fulfillment for the requirement of award of the degree of Master of
Science in Physics is a record of original project work done by
THIYAGARAGAN K (21-08-139) during the period 2022-2023 of her study in
this college under my guidance and this project work has not formed the basis
for the award of any degree / diploma/ Associate-ship / Fellowship / other similar
title to any candidate in any university.

Date: Signature of the Guide:

Place: Name : S. KAVITHA

Counter Signed

Head of the Department Principal

Internal Examiner External Examiner

 DECLARATION

This is to declare that the dissertation entitled “PHOTOCATALYTIC

PERFORMANCE OF MgO NANOPARTICLES FOR
PHOTOCATALYTIC DEHYDRATION OF MALACHITE GREEN DYE
UNDER VISIBLE LIGHT” submitted to GOBI ARTS & SCIENCE
COLLEGE (Autonomous), Gobichettipalayam in partial fulfillment for the
requirement of award of the degree of Master of Science in Physics is a record
of original project work done by me under the guidance of Mrs. S. KAVITHA
M.Sc., M.Phil., Assistant professor, Department of Physics, Gobi Arts &
Science College (Autonomous), Gobichettipalayam and this project work has not
formed the basis for the award of any degree / diploma/ Associate-ship /
fellowship / other similar title to any candidate in any university.

Date: Signature

Place: THIYAGARAGAN K.
 ACKNOWLEDGEMENT

The project work cannot be a one-man show. Although it is impossible to

give individual thanks to all helpful faculty members and to those in connections.
I take this opportunity to express my gratitude for them.

I would like to thank Dr. V. THIAGARASU M.Sc., M.Phil., B.Ed.,

Ph.D., Principal, Gobi Arts & Science College, Gobichettipalayam for providing
me an opportunity to do this project.

I would like to thank specially Mrs. R. BANUPRIYA M.Sc., M.Phil.,

PGDCA., Ph.D., Associative Professor in Physics, Gobi Arts & Science
College, Gobichettipalayam who extended helping hands and encouragement for
the successful completion.

I wish to place my hearty and sincere thanks to my respectable Guide

Mrs. S. KAVITHA., M.Sc., M.Phil., Department of Physics, Gobi Arts &
Science College, Gobichettipalayam for her constant encouragement, wealthy
advice and administrative support given in all aspect during the project.

And I would like to thank the faculty members of the Department of Physics for
their valuable advice and encouragement during the entire period of study.
I cherish to acknowledge the benevolence to my parents, Sisters and
Friends for their constant love, encouragement, enthusiasm, blessing, co-
operation and support during the entire course of study

.
THIYAGARAJAN K
contents
CHAPTER TITLE PAGE NO.

INTRODUCTION
1.1 NANOTECHNOLOGY
1.2 ORIGIN OF NANOTECHNOLOGY
1.3 NANOPARTICLES
I 1.4 NANOMATERIALS
1.5 NANOSCALES
1.6 SYNTHESIS OF NANOMATERIALS
1.7 APPLICATION OF NANOMATERIALS
1.8 ADVANTAGES OF NANOTECHNOLOGY
1.9 DISADVANTAGES OF NANOTECHNOLOGY

II LITERATURE SURVEY

III MATERIALS AND METHODS

CHARACTERIZATION TECHNIQUES
4.1 X-RAY DIFFRACTION METHOD
IV 4.2 UV-VISIBLE SPECTROSCOPY
4.3 FTIR SPECTROSCOPY

V EXPERIMENTAL METHODS
5.1 SYNTHESIS OF MGO NANOPARTICLES
VI RESULT &DISCUSSION
6.1 X-RAY DIFFRACTION STUDY
6.2 FTIR ANALYSIS
6.3 UV ANALYSIS
6.4 PHOTOCATALYTIC ANALYSIS

VII CONCLUSION
VIII REFERENCE

CONTENTS
 CHAPTER-I
INTRODUCTION

1.1 NANOTECHNOLOGY

Nanotechnology refers to the branch of science and engineering to

designing, producing and using structure, device and system by manipulating
atoms and molecules at nano scale. The other name of nanotechnology is
molecular manufacturing. The word nano is believed to have originate from the
Greek word "NANNOS" which means dwarf or something very small. Nano
science is also commonly known as the scientific study of molecular structure
at the atomic or molecular scale with at least one of their dimensions measuring
between 1 to 100 nanometers. Nanotechnology invented to increase the surface
area of the material. Nanotechnology is not a microscopy. Principle of
nanotechnology is self-contained and unified in presentation.

 Nanotechnology is the ability to build and shape matter one atom at a

time.
 Science of material with at-least one spatial dimension in the range of
1-100 nm.
 A technology that is concerned are based on single or integrated
nanoscale components.
 This technology enabled material have novel physical-chemical
properties that are unique from the bulk specimen due to their
reduced size.

 This field has exhibited an excellent potential to consume small

quantity of resource in developing novel material and devices.

 Nanotechnology is still in its early stage, with an almost erratic

growth that keeps steadily increasing.
 The four generations of nanotechnologies are:
 Passive nanostructure

 Active nanostructure

 System of nano system

 Molecular nano system

1.2 ORGIN OF NANOTECHNOLOGY

The ideas and concepts behind nanoscience and nanotechnology with
the top entitled "There's Plenty of Room at the Bottom" by physicist
RICHARD FEYNMAN at an American physical society meeting at the
California institute technology on December 29 1959, long before the term
nanotechnology was used.

 The term "NANOTECHNOLOGY" was introduced by NORIO

TANIGUCHI in 1974 during scientific conference, but the idea of
building “SMALL” things is usually attributed to Richard Feynman
based on the talk gave 1959. He predicted that machine built smaller
machines and other products with atom by control, a process which was
later molecular manufacturing.

 The first observation size measurement of nanoparticles was

performed at the start 20th century by RICHARD ZSIGMONDY,
winner of noble prize in 1925. He was the first to term
NANOMETRE explicitly for characterizing particle sizes.

 In the year 1932 the noble prize winner in chemistry, IRVING

LANGMUIR, introduce the concept of MONO LAYER, the layer of
 material one molecule thick.

 The further development of Nano technology was achieved in 1981 by

GERD BINNING and HAINRICH ROHRAR at IBM. The invention of
scanning tunnelling Microscope (STM), for which they were awarded
noble prize in physics in 1986.

 In 1999, CHAD MIRKIN at North Western University invented DIP-PEN

NANOLITHOGRAPHY, leading to the manufacture of reproducible
"Writing" of circuits as well as pattering of bio materials for cell biology
research, nano encryption other applications.

 In 2004 the European commission promoted the communication “To

words European strategy for nano technology” and in 2008 released the
“Code of conduct for responsible for nano science and nano technologies
research”.

NANOSCIENCE

Nanoscience is the study of the properties of matter at the nanoscale. It is

used to manufacture structure in coal, silicon, inorganic materials, metals and
semiconductor that do not work with humidity. Nano technology and
nanoscience have become of fundamental importance to industrial application
and medical devices such as diagnostic biosensors, drug delivery system and
imaging probes.

1.3 NANOPARTICS

Nanoparticles or ultrafine particles is defined as particle of matter that is

between 1 and 100 nanometers in diameter. Nanoparticle are formed through
 either the breaking down of layer particles or by controlled assembly process.
The principal parameters of nanoparticle are their shape, size, surface
characteristics and inner structure.

Properties of Nano meterials:

 The surface area to volume ratio of nanoparticles is extremely high.

 Nanoparticles are so small that they can enter biological tissue.

Nano particles and its type:

 Nanosphere nanoparticle (matrix like structure)

 Nano capsule nanoparticle (core shell morphology)

Nanosphere:

Nanosphere polymeric nanoparticle the active compounds and the polymers

are uniformly dispersed. Nano sphere is a spherical particle whose diameter is
measured in nanometers. They are formed through either the breaking down of
larger particles or by controlled assembly processes.

Examples of nanosphere are,

 Liposomes

 Chitosan

 Neoplasm

 Polymer
Nano capsule:
Nano capsule nanoparticles the active compounds are confined and
surrounded by a polymer shell. The most commonly used nanoparticles are
titanium-di-oxide, carbon nanotubes, silica, copper, clay and aluminum oxide
are most widely used nanoparticles. A nano capsule is a nanoscale shell made
from a non-toxic polymer. It is made up of an oily or an aqueous core which
is surrounded by a thin polymer membrane.

1.4 NANOMETERIALS

A single unit is sized between 1 and 100 nm. Nano materials can also
be added to cement, cloth and other material to make them stronger and yet
lighter. Their size extremely useful in electronics and they can also be used in
environmental remediation.

Nano materials are categorized as,

 Zero dimensional (Ex: Nanoparticles)

 One dimensional (Ex: Nanotubes and Nanorods)

 Two dimensional (Ex: Graphene)

 Three dimensional (Ex: Nano prism and Nanoflowers)

Types of Nanomaterials
The most current nanomaterials could be organized into four types,

 Carbon based material

  Mental based material

 Dendrimers

 Composites

Carbon based Materials:

These nanomaterials are composed mostly of carbon atoms and it is

called as carbon-based nanomaterials. The form of a hollow spheres,
ellipsoid or tubes. Spherical and ellipsoidal carbon nanomaterials are referred
to as fullerene while cylindrical ones called nanotubes. These particles have
many potential applications including improved film and coating stronger
and lighter material and application in electronics.

Metal based materials:

These nanomaterials include quantum dots, nano gold, Nano silver and
metal oxides such as titanium-di-oxide. The quantum dot is a closely packed
semiconductor. Crystal comprised of hundreds or thousands of atoms and
whose size is on the order of a few nano meter to a few hundred nanometers.
Changing the size of quantum dot changes their optical properties.

Dendrimers:

These nanomaterials are nanosized polymers built from branched units.

The surface of a dendrimers has numerous chains ends which can be tailored to
 performed specific chemical function. The property could also be useful for
catalysis. Three dimensional dendrimers contain interior cavities into which
other molecules could be placed, they may be useful for drug delivery.

Composites:
Composites combine nanoparticles with other nanoparticles or with larger,
bulk type materials. Nanoparticles such as nanosized clays are already being
added to product ranging from auto parts to packing materials to enhance
mechanical, thermal, barriers and flame-retardant properties.

Properties of Nanometerials

 Nanomaterials are chemical substances or materials that are of size at-

least in one dimension in nanoscale 1-100 nm.

 Large surface of volume ratio leads better performance such as in

catalysis, solar veils, gas sensor.

 High percentage of atoms or molecules on the surface which leads to

unique properties.

 The physical and chemical properties are unique and change by size and

shape.

Carbon based nano materials

 Fullerene

 Carbon nanotubes
  Graphene

 Quantum dot

 Quantum well

 Quantum wires

 Nano shell

 Carbon nanobuds

Carbon nanofiber is a super material. It conducts heat and electricity

better than metals. So, carbon is used in nanotechnology. Carbon nanofiber is
strong, elastic and lighter when compared to steel carbon is most preferred
material for nanostructure because of large surface to volume ratio, high
conductivity and electron mobility at room temperature.

Fullerenes:

Fullerenes is an allotrope of carbon whose molecule consist of carbon

atoms connected by single and double bond so as to form a closed or partially
closed mesh with fused rings of five to seven atoms. The molecule may be
hollow sphere, ellipsoid, tube and other shapes and size. Fullerene structure is
similar to that of graphite and made up of a sheet of connected hexagonal rings.
Fullerene often referred to as bucky balls and bucky tubes depend on shape.
Cylindrical fullerene referred to as nanotubes.
Application of Fullerence:

 Behavior and structure depend on temperature.

 Structure can be change under different pressure.

 Ionization enthalpy is 7.61 electron volts.

 Electron affinity is 2.6 to 2.8 electron volts.

Chemical properties of fullerence:

 It is stable but not totally unreactive.

 It can act as electrophile.

 It is ferromagnetic.
Carbon Nanotubes (CNT)

Carbon nanotubes (CNT) is a derivative of both carbon fiber and fullerene

with molecules composed of 60 atoms of carbon arranged in particular muffled
tubes. It is a tube made of carbon with diameter typically measured in
Nanometers.

These are three types of nanotubes,

 Single walled nanotubes

 Double walled nanotubes

 Multi walled nanotubes

Single walled nanotubes:

 Single walled carbon nanotubes are an allotrope of sp2 hybridized carbon
similar to fullerenes. The structure can be through of as a cylindrical tube
comprised of 6 membered carbon rings as in graphite. The cylindrical tubes may
have one or both ends capped with a hemisphere of the bucky ball or fullerene
structure. Single walled nanotube is classified into three types,

 Armchair

 Zigzag

 Chirality

Double walled nanotube:

Double walled carbon nanotubes are coaxial nanostructure composed

of exactly two single walled carbon nanotubes one nested in another.
Multi walled nanotube:

It consists of a series of single wall tubes nested within one another. They
may be few as 6 or as many 25 such concentric wall. Multiple concentric rolled
layers of carbon atoms in multi walled carbon nanotubes.

Properties of carbon nanotube:

 Carbon nanotubes have high thermal conductivity and electrical

conductivity.
 Carbon nanotubes are very elastic.
 Carbon nanotubes have a low thermal expansion coefficient.

Graphene:

It is allotrope of carbon consist of a single layer of atoms arranged in a

hexagonal lattice nanostructure. The name in derived from "graphite". The
suffix "ene" reflecting the fact that the graphite allotrope of carbon contains
numerous double bonds. Allotrope of carbon has different dimensions such as
1 dimension (carbon nanotube) and 2 Dimension (graphene). Graphene is 2D
structure with sp2 hybridization. Semiconductor nanoparticles composites
could provide new way to design graphene-based composites of catalytic and
photocatalytic reaction.

Application of grapheme:

Graphene is used in transport, medicine, electronics, energy, defense,

 desalination. Graphene has been used in different products. The potential of
graphene is limited only by our imagination. Graphene is used in the
manufacturing of microchips, transistor, development of conductive inks that
allow the circuit printings. Graphene is used in batteries to increase the
autonomy and reduce the charging time; this can improve the performance of
electric cars.

 High thermal conductivity.

 High electrical conductivity.

 High elasticity and flexibility.

 High hardness.

 Ionizing radiation is not affected.

 Transparent material.

 Antibacterial effect. Bacteria are not able to grow in it.

 Low joule effect, heating when conducting electrons.

 Low electricity consumption compared to other compounds.

Quantum well:

Quantum well is a nanometer thin layer which can confine particles in the
dimension perpendicular to the layer surface whereas the movement in the
other dimension is not restricted. Quantum well is widely used in diode laser,
including red laser for DVD and laser pointer, infrared laser in fiber optic
 transmitter or in blue lasers advantages of quantum well is low threshold
current density excellent temperature features high modulation rate and
wavelength adjustability. A quantum well is a potential well with only discrete
energy values. Quantum well is formed when the thin layer of narrow gap
semiconductor material lies between a thicker layers of wider gap materials.

Quantum wired or nanowires

Nanowires are also called as quantum wires. Nanowires are one

dimensional. Quantum wires are extremely narrow structure where electron
transport is possible only in transverse mode. Nanowire is a nanostructure in the
form of a wire with diameter of the order of a nanometer. Nanowires can be
defined as structure that have a thickness or diameter constrained length.
Nanowires are used for connectors for the transportation of electron. Cobalt,
copper, silicon and gold have been used to make nanowires. Chemical vapor
deposition is used for the production of nanowires. Quantum wire is an
electrically conducting wire in which quantum effects influence the transport
properties.

They appear in dimension of nanometers. So, they are also called as

nanowire. The diameter is 125- 425nm. Nanowires are found in deep in the
ocean or underground where there is no oxygen, geo barter bacteria "breathe"
by projecting tiny protein filament called nanowires into the soil to dispose of
excess electron. Low dimensional nanoscale materials such as nanowires,
nanotubes (1 dimensional structure). Nano wires generally have a thickness or
diameter of tens of nanometer or less and a variable length. Nanowires are
solid crystalline fibers rather than hallow tubes.
Quantum Dots:

Quantum dot are semiconductor nanocrystal that have a reactive core

which controls their optical properties. They are semiconductor nanoparticles
that glow a particular color after being illuminated by light glowing color
depends on the size of the nanoparticles. There are four types of quantum dot,

 Inorganic quantum dot

 Carbon based quantum dot

 Perovskite quantum dot

 Quantum dot kit

The electron in a quantum dot is confined to 2D within quantum well in
a thin layer of semiconductor. Quantum dot are created through injection of
reactant into a solvent solution. It is used for their unique optical properties
they emit light of specific wavelength if energy is applied to them. Quantum
dot is a human made nanoparticle that has semiconductor properties. The size
of quantum dot is from 2 to10 nanometers. Quantum dot are used in numerous
biomedical application such as drug delivery, live imaging and medical
diagnosis. Quantum dot are man-made nanoscale crystal that can transport
electron. The dots show quantum effects because they are so little so they are
called as quantum dot.

Quantum shell

Nano shell are spherical particles consisting of a dielectric core

surrounded by a thin metallic shell most commonly gold. Nano shell convert
light to heat energy. The transferred heat is strong enough to destroy the cancer
cell. Healthy cells then consume the dead cancer cells through phagocytosis.
Nano shell made of a core of silica and a metallic outer layer. Nano shell are
injected into the blood stream and as they circulate through blood, they can
uptake naturally at a tumor site.
Carbon nanobuds

A carbon nanobuds is a material that combines carbon nanotubes and

spheroidal fullerenes both allotropes of carbon forming "buds" attached to the
tubes. Nanotubes exhibits properties of carbon nanotubes and fullerenes.
Carbon nanobuds have a much higher chemical activity than single walled
carbon nanotubes. Carbon nanotubes such as 1D electrical conductivity,
flexibility and manufacturing adaptability, and some of the chemical properties
of fullerenes. The chemical bonds between the nanotube wall and the fullerenes
on the surface can lead to change transfer between the surfaces. The presence of
fullerenes in carbon nanobuds leads to smaller bundle formation and higher
chemical reactivity. Carbon nanobuds can conduct electricity regardless of
whether the single walled carbon nanotubes are a metallic or semiconducting
base.

Bucky Balls

The fullerenes having a closed structure are called bucky balls. A bucky
balls containing 60 carbon atoms in its molecule is famously known as
buckminsterfullerene. Bulky ball may be used to store hydrogen, possibly as a
fuel tank for fuel cell powered cars. Bucky balls can reduce the growth of
bacteria in pipes and membrane in water system. A form of carbon composed
cluster of 60 carbon atoms bonded together in a polyhedral or many side
structure composed of pentagons and hexagons like the surface of a soccer ball.
Bucky balls are found in meteorites, earth rock and candle soot.

Light carbon nanotubes used in bike frames and tennis rackets. Bucky balls
are 5mm in diameter. Each full-size set includes 216 rare earth bucky balls
magnets.

Physical properties of Bucky balls:

 Buckminsterfullerene is stable at high temperature and pressure.

 Fullerene are covalent and soluble in organic solvent but in soluble in

water.
Fuel Cells:

Fuel cells is the electrochemical cell that converts the chemical energy of
a fuel and an oxidizing agent into electricity through redox reaction. Carbon
nanotubes have application in battery technology. Lithium which is a charge
carrier in some batteries can be stored inside nanotubes. It is estimated that one
lithium atom can be stored for every six carbons of the tube. Storing hydrogen
in nanotubes is another possible application one that is related to the
development of fuel cells as sources of electrical energy for future automobiles.
A fuel cell consists of two electrodes separated by a special electrolyte that
allows hydrogen ions but not electrons to pass through it. Hydrogen is sent to
the anode where it is ionized. Hydrogen fuel cell produce no harmful emission,
eliminating the cost associated with handling and storing toxic material like
battery acid or diesel fuel. The freed electrons travel through an external wire to
the cathode. The hydrogen ions diffuse through the electrolyte to the cathode
where electrons, hydrogen and oxygen combine to form water. Fuel cell used
for commercial, industrial and residential buildings and in remote are
inaccessible areas.

Application of Fuel cells:

 Hetero-polyacid nanoparticles for high temperature

operation of a direct methanol fuel cells.

 Preparation and characterization of new carbon for fuel cell

application.
 Pulse electrodeposition for preparing PEM fuel cell electrode.

Nanoscale and their Properties:

The region of 1-100 nm where properties of substance differ from those

at a larger scale. Nanotechnology makes use of these nanoscale properties to
develop new material and devices. Nano scale material in a range of cosmetics
provide function such as improved coverage, absorption or cleaning.
Nanoparticles give the surface of these textile fibers structure with an effect
similar to a lotus plant leaves making the fibers water and dirt repellent. Nano
scale material can have one, two or three dimensions in the nanoscales regime
 which adds to the variety of phenomenon that can be explored in nano science
and technology.

Chemical properties of nanoscale:

The large surface to volume ratio tends to improve the interfacial and
surface chemistry of the material for their efficient reaction. Example:
Nanocataylst tends to improve the rate of a reaction while compared to their
bulk counterparts.

Electronic properties of nanoscale:

The quantum confinement effects taking place in the nanomaterials could

be used to engineer their bandgap values that could further influence the density
of states and result with a superior conductivity in them. Additionally, they also
facilitate the phenomenon of electron tunnelling to take place.

Optical properties of nanoscale:

The absorption and fluorescence of nanocrystal are unique and they have
been used to realize optoelectronic application such as display light emitting
diodes, solar cells etc.

Magnetic properties of nanoscale:

The concept of giant magneto-resistance observed in nanoscale

heterostructure and variation in magnetic susceptibility values could be
hardness for application in memories, generators, sensors etc.

Thermal properties of nanoscale:

The increased thermoelectric performance of nanoscale material and

interfacial thermal resistance properties of the nanomaterial makes them an
eligible candidate for high temperature application such as automobile
alternators, power generator, motors, ultrasensitive analytical instruments and
also in medical diagnostics.

Mechanical properties of nanoscale

 The improved tensile strength and hardness in the light weight
nanocomposites, compression properties and nano mechanics of molecular
structure could be capitalized for a number of applications that included
automobile industries mainly.
Fluid properties of nanoscale

At nanoscale dimension the flow of liquid through the nanochannels

could be enhanced significantly. They also help in biological application to
handle even very small amount of sample at ease. Likewise, the nanoscale
absorbed film are also used in other nano fluid application.

Nano metals:

Used to establish conducting screens, sensors and energy material. They

are also preferred for antibacterial and catalysis function.

1.4 synthesis of nanomaterial

Nanotechnology is dependent on nano structures that require creation and

characterization. Two fundamentally different approaches for the controlled
generations of nano structures have evolved. The nanomaterials can be
synthesized using two prominent approaches. They are

 Top-down and
 Bottom-up approaches

Top-Down approach:

The top-down approach to management is when company decisions are

made solely by leadership at the top, while the bottom-up approach gives all
teams a voice in these types of decisions. Top-down approach starts from a bulk
material that incorporates critical nanoscales details. The top- down approach
involves molding or etching materials into smaller components. In top-down
approach, nano-objects constructed from large entities without atomic-level
control.

Bottom-Up approach:
 The bottom- up approach is based on the principle of molecular self-
assembly. This phenomenon is defined as a spontaneous organization of
molecules under near thermodynamics equilibrium condition to form stable
structures. The materials and devices are built from molecular components
which assemble themselves chemically by principles of molecular recognition.
The method of forming a periodic nanostructure from the bottom-up is called
self-assembly.

The bottom-up approach involves assembling structures atom-by-

atom or molecule-by-molecule, and may prove useful in manufacturing
devices used in medicine. Bottom-up techniques built or grow large structure
of atom by atom or molecules by molecules.

1.7 APPLICATION:

Medical application:

 In nanotechnology nanoparticles are used for site specific drug

delivery.

 Micelles obtained from block co-polymers are used for drug

encapsulation.

 They transport small drug molecules to the desired location.

 Nano electrochemical system are utilized for the active release of

drugs.

 Iron nanoparticles or gold shells are finding important application

in the cancer treatment.

 Surgery could also be done on tissue, genetic and cellular levels.

  Sulfur is an interesting element for tumor take because it plays an
important role in cellular metabolism.

 Sulfur is an essential part of many enzymes and antioxidant

molecules like “GLUTATHOINE” and “THIOREDOXIN”.

 Cancer is also known as a malignant tumor or malign ant neoplasm

is a group of diseases involving abnormal cell growth with the
potential to invade or spread to other part of the body.

 Growth is considered to be either benign or malignant.

 Each type of cancer is unique with its own causes, symptoms, and
methods of treatment.

 Not all tumors are cancerous; benign tumors do not spread to other
parts of the body.

Treatment of cancer:

1. Surgery
Surgery can be used to diagnose, treat or even help prevent
cancer in some cases. Most people with cancer will have some type
surgery.
2. Chemotherapy

Chemotherapy (chemo) is the use of medicines of drugs to treat cancer.

3. Radiation therapy

Radiation therapy uses high energy particles or waves to destroy

or damage cancer cells. It is one of the most common treatments for
cancer, either by itself or along with other forms of treatment.
 4. Immunotherapy

Immunotherapy is treatment that uses your body’s own immune

system to help fight cancer.

5. Targeted therapy

Targeted therapy is a newer type of cancer treatment that uses

drugs or other substances to more precisely identify and attack cancer
cells, usually while doing little damage to normal cells.

6. Stem cell transplant

(Peripheral blood, bone marrow, and cord blood transplant) use

treat cancer.

7. Hyperthermia
The idea of using heat to treat cancer has been around for some
time, but early attempts had mixed results. Today, newer tools allow
more precise delivery of heat, and hyperthermia is being studied for use
against many typed of cancer.

NANOPORES:
Nanopores are tiny holes that allow DNA to pass through one strand
at a time will make DNA sequencing more efficient.

Agriculture Application:

To improve agriculture productivity via nano fertilizers, use of

efficient herbicides and pesticide, soil features regulation, waste water
management, and pathogen detector.

Nano medicine:
 Nanotechnology has found numerous applications in medical field.
Nano medicine is a branch of medicine that applies the knowledge and tools of
nanotechnology to the prevention and treatment of diseases. It can be used
designed to help immune cells engage and subsequently eliminated cancer
cells. Improved diagnosis, treatment, and monitoring of many serious illnesses,
including cancer, cardiovascular and neurological disorders, HIV/AIDS, and
diabetes.

Batteries:

Increasing the available power from a battery and decreasing power

from a battery and decreasing the time required a battery. These benefits are
achieved by coating the surface of an electrode with nanoparticles. Carbon
black nanomaterial is used in lithium batteries. It is used in the electrode it
does not store electrical energy and act as a “passive” conductivity to improve
power capability. The advantages of nanobatteries are higher power density,
shorter charging time, and longer shelf life.

Cosmetics:

Cosmetics is a good field. TiO 2 nanoparticles compared to UV

production property is bulk material. Cosmetics are nano-sized because to
improve UV protection, skin penetration, color, the release of fragrance, finish
quality, anti-aging effect and a variety of other properties. Dendrimers,
Cabooses, Nano emulsions are good examples of nanoform particles employed
in Cosmetics in application of nanotechnology. Topical skincare in
nanotechnology is defined as a particle that acts as a vehicle to assist the
ingredient in product formulation with increased penetration and leading to
greater efficiency of the product. When mixed into sunscreen, nanoparticles of
TiO2 and ZnO not only retain their highly effective UV light absorbing
capacity, but also absorbed and scattered visible light, rendering them
 transparent on skin.

Food technology:

 Nanomaterials are used as ingredients and additives (E.g.: vitamins,

antimicrobials, antioxidants) in nutrients and health supplement for
enhanced absorption and bio-availability.
 The antimicrobial properties of nanomaterials enable them to
preserve food during storage and transport.
 They are used as sensors in food production and at packaging plants.

Solar cells:

Nanocrystal solar cells are solar cells based on the substrate with a
coating of Nanocrystal. It is based on silicon, CdTe, CiGS are generally silicon
or various organic conductors. Nanoscales are involves using liquid process to
put billion of nano-sized holes in each square inch of a solar cells surface. The
efficiency cells are 31%. Solar cells are also called as photovoltaic cell. It is
electric devices convert into solar energy light directly by the photovoltaic
effect.

1.8 ADVANTAGE OF NANOTECHNOLOGY

 Great change in electronic commodities.

 Blessing for the medical field.

 Manufacturing advantages
Generates energy at low speed.

 Energy generation.

 Treatment is possible to a great extent.

 Can be used in cosmetics as it absorbed much deeper into skin.

1.10 DISADVANTAGE OF NANOTECHNOLOGY

 Negative impact on environment.

 Unemployment may pre-vil.

 Economical imbalance.

 Hazardous weapons accessible.

 Negative impact on people’s health.

 Breathing in tiny particles could have a negative effect on our

lungs.
 CHAPTER-II
LITERATUR REVIEW

 Jaroslav Hornok et al [1] reported the uses of Nano scale filters in a variety of
application in which magnesium oxide having unique properties and used in
wide range of application in industry, agriculture, and medicines. MgO can be
prepared through different chemical (Bottom-up approach) or physical routes. In
additional to its unique material properties. Finally, potential application and
environmental friendliness.

 Zhen-Xing Tang et al [2] reported the new way of development in the area of
inorganic antibacterial agent. Nano-inorganic metal oxide has a potential to
reduce the bacterial contamination. It is used in many fields. It was prepared by
various synthesis method. The antibacterial activity and antibacterial
mechanisms of MgO Nano-particle were reviewed.

 Rahman TR et al [3] reported the MgO material with high surface area was
prepared via neem leaves extract & characterization of MgO with its antioxidant
and photo catalystic effect, the sample were characterized by X-ray powder
diffraction techniques, FE-SEM and UV-Visible spectroscopy.

 Rand Ali et al [4] reported the Physical properties of MgO nanoparticles and
their Antibacterial activities. In this study, an ultrasound device was used to
reduce the particle size, with the impact on the energy gap was set at the
beginning at5.39 eV and then turn to 4.10 eV. The morphological analysis by
atomic force microscopy showed that grain size MgO Nanoparticles was 67.70
nm which become 42.33 nm after the use of ultrasound and the sample were
characterized by FE-SEM, XRD, UV-Visible spectrum and EDAX.

 K. Ganapathi Rao et al [5] reported the structural properties of MgO Nano

particles by Co-precipitation techniques. And its application in the field of
environment. The synthesized metal oxide Nanoparticle have been Characterized
by X-ray diffraction (XRD), Particle Size Analyzer, SEM, Thermo Gravimetric
and Differential Thermal Analyzer (TG-DAT) for average size, Average particle
size, Morphology and stability respectively.

 Khansao. D. Salman et al [6] reported the metal oxide Nano particle material
were synthesis by Microwave and Sol-Gel method. The specific surface area of
the MgO Nanoparticles used Sol-Gel route was more than Microwave route. The
 sample were characterized by FE-SEM, X-ray diffraction (XRD), FTIR and BET
techniques.

 G. Sharma et al [7] reported the phytoassisted synthesis of MgO NPs with an

aqueous extract of sweritia chirayaita. The method is cost effective and eco-
friendly. The crystalline structure of MgO NPs was face-centered cubic
geometry. The sample were tested against gram-positive and gram-negative
bacteria by agar-well diffusion method it is to effective against both gram-
positive and gram-negative bacteria. MgO Nanoparticles were characterized by
UV-Visible spectroscopy, SEM, TEM and XRD techniques.

 Sutapa et al [8] reported the synthesis and structural profile analysis of the MgO
nanoparticle produced through the sol-gel method followed by annealing
process. The sample were characterized by, Fourier Transform Infrared
spectroscopy, Crystal profile analysis using (XRD) X-ray diffraction and
Morphology using Scanning Electron Microscopy (SEM).

 S. Rizwan Ali et al [9] reported the Magnesium oxide (MgO) nanoparticle

application in electron tunneling. Magnesium oxide (MgO) nanoparticles are
synthesized by a simple co-precipitation method. (SEM) Scanning electron
microscopy Studies reveal that picture of the sample are spherically shaped. The
sample were characterized by X-ray diffraction (XRD), SEM and TEM
techniques.

 Amisha kushwaha et al [10] reported the Magnesium Oxide Nanoparticles was

capping and enhanced free radical effect on the bacteria and its cell morphology.
The sample were prepared by Co-precipitation method. The sample were
analyzed by X-ray diffraction (XRD), Scanning Electron Microscopy (SEM),
TEM and FTIR techniques.

 Agrawal R.M et al [11] reported the structural and characterization of MgO

nanoparticle by using liquid phase method with large surface area in short
reaction time at room temperature and this method is the simplest, eco-friendly
method. In V/I characteristics techniques the activation energy of the MgO NPs
is 0.49eV or 48.196 KJ/mole so this sample shows the predominance of
electronic conductivity. The sample were characterized by X-ray diffraction
(XRD) and V/I characteristics techniques.

 Jayakaran Pachiyappan et al [12] reported the characterization of MgO NPs

and its application for photo catalytic removal of RhB and MB dyes. Material
has been prepared by a single-step co-precipitation method. MgO NPs exhibit
 cubic crystal structure. The sample were characterized by X-ray diffraction
(XRD), FTIR, P-XRD, UV-DRS, SEM, EDAX and Photo catalysis techniques.

 K.G. Manjunatha et al [13] reported the synthesis of metal oxide nanoparticles

and their surfactant modified carbon paste electrode (CPE) sensing for
paracetamol (PA). Sample were prepared by co-precipitation method. It has an
excellent electro catalytic activity and sensitive. The sample were analyzed by
X-ray diffraction (XRD), Scanning electron microscope (SEM) and Energy-
dispersive spectroscopy analysis (EDS).

 V. Sabari et al [14] reported the characterization of metal oxide and the sample
was prepared by sol-gel method. The result of cubic structure and the particle
size and lattice constant were analyzed by XRD, UV-Vis, Scanning Electron
Microscopy (SEM) and EDAX techniques. The MgO nanoparticles are used in
optical and sensor applications, telecommunication cables, conductor wires and
automotive switches.

 P. Vigneshwaran et al [15] reported the synthesis and characterization of MgO

nanoparticles by an orange fruit through green method. The sample were
prepared by Sol-gel method. The sample were analyzed by X-ray diffraction,
Scanning Electron Microscopy (SEM), UV-Vis and Transmission Electron
Microscopy (TEM) techniques.

 S. Lidvin daisy et al [16] reported the characterization of Magnesium oxide

Nanoparticles was prepared by Co-precipitation method. The sample were
characterized by X-ray diffraction, EDAX and Scanning electron Microscopy
(SEM).

 Rohit Kumar et al [17] reported the, varying morphology, structure and

composition metal oxide material shows different physical and chemical
properties. The photocatalytic performance of the material is strongly influenced
by morphology and structure as they are determined in turning its electronic
properties. Similarly, degradation of various pollutants and deactivation of some
organisms like Hela cancer cells and bacteria are also brought are also discussed
in report. Finally, potential applications and unanswered challenges about the
material are propounded for further research.

 Yingying Li et al [18] reported the photocatalysis, which harnesses light to

degrade pollutants, has been considered as the most green and low-cost approach
for environmental remediation. A novel wood photocatalyst was prepared by a
simple one-pot way. The prepared sample were characterized by X-ray
 diffraction, Scanning Electron Microscopy, Energy dispersive X-ray
spectroscopy, UV-Vis diffuse reflectance spectroscopy and X-ray photoelectron
spectra respectively. Results shows that the synthesized bismuth molybdate
Nano-eggshells were evenly growth on the surface of wood substrate. The study
offers exciting opportunities to achieve the industrialization of photocatalytic
wood products.

 Daimei Chen et al [19] reported the metal oxide material photocatalysts with the
different phase structures and morphologies were controllably synthesized via
reflexing method by adjusting the PH in the reaction system. The electron Spin
Resonance (ESR) and the photogenerated carriers trapping experiment suggested
that both have the same photocatalytic mechanism and the main oxidative
species for these samples are hydroxyl radical.

 Wenfeng Guo et al [20] reported the metal oxide material single-crystalline

were synthesized by a simple hydrothermal method in the presence of surfactant
sodium dodecyl sulphate (SDS), polyvinyl pyrrolidone (PVP), or
cetyltrimethylammonium bromine (CTAB). The sample were characterized by
X-ray diffraction (XRD), Transmission Electron Microscopy (TEM) and
Ultraviolet-Visible Diffuse Reflectance spectra (UV-Vis DRS) techniques.
 CHAPTER III
MATERIALS AND METHODS
DEFINATION OF MAGNESIUM OXIDE:

Magnesium oxide is also called as magnesia. Magnesia (the name derives probably
from Magnesia, a district of Thessaly in Greece). It is an alkaline earth metal oxide which is
usually obtained from the calcination of some naturally occurring minerals. Magnesium oxide
is solid material that physically chemically stable at high temperature. It is mostly used in re-
factory materials. It is an inorganic compound that occurs in nature as the mineral periclase.
In aqueous media combines quickly with water to form magnesium hydroxide. It is used as
antacid and mild laxative and has many non- medicinal uses. The important source of
magnesium oxide is in sea water, underground deposits, of brine and deep salt beds.

PROPERTIES OF MAGNESIUM OXIDE

Molecular formula MgO
Molar Mass 40.3044 g/mol
Appearance White hygroscopic solid
mineral
Density 3.58 g/cm3
Melting point 28520 C (5166 0F;31250 K)
Boiling point 36000C (6510 0F;3870 0K)
Solubility Soluble in acid (AMMONIA),
Insoluble in alcohol.

Electrical resistivity Dielectric

Band gap 5-7.6Ev
Refractive index 1.73463
Crystal structure Halite (cubic)

Flash point 2500 K (2200 C, 4000 F)

Nature of the material No

FUNDAMENTAL PROPERTIES OF MgO NANO PARTICLES:

Magnesium oxide nanoparticles are odorless and non-

toxic. Magnesium oxide is a semiconductor material
because magnesium and oxygen belong to 2nd and 6 th
group of the periodic table. They possess high hardness,
high purity and a high melting point. Magnesium oxide
 nanoparticles appear in a white powder form. Magnesium
oxide has a good corrosion resistance. It is a silvery white
metal that ignites easily in air and burns with a bright light.
Magnesium oxide is one-third less dense than aluminum. It
improves the mechanical, fabrication and welding
characteristics of aluminum when used as an alloying agent.
These alloys are used in aero-plane and car construction.

CHEMICAL PROPERTIES OF MAGNESIUM

OXIDE:

Magnesium is a fairly. Chemical formula of magnesium

oxide is MgO. It reacts slowly with cold water and more
rapidly with hot water. It combines with oxygen at oxygen
at room temperature to form a thin skin of magnesium
oxide. It burns with a blinding white light at higher
temperature. Magnesium reacts with most of acids and with
some alkalis. An alkali is a chemical with properties
opposite those of an acid. Sodium hydroxide and lime water
are example of alkali. Magnesium also combines easily
with many non-metals including nitrogen, Sulphur,
phosphorous, chlorine, fluorine, bromine and iodine.

APPEARANCE IN GROVE:

Abundance of magnesium in the earth’s crust is estimated

to be about 2.1 percent. It is second most common element
in the earth. It is also occurring in sea water. A cubic mile
of sea water is estimated to contain up to six million tons of
magnesium. There are many naturally occurring minerals of
magnesium. Some most important minerals are dolomite,
magnesite, carnallite, and epsomite. The largest producer of
magnesium ores is Turkey.

The Mg2+ cation is the second most abundant cation in sea

water (occurring at about 12% of the mass of sodium)
which makes sea water and sea-salt an attractive
 commercial source of Mg. To extract the magnesium,
calcium hydroxide is added to sea water to form
magnesium hydroxide precipitate,

Mgcl2 +Ca (OH)2 Mg (OH)2 +Cacl2

From magnesium chloride, electrolysis produces
magnesium. Magnesium is obtained by electrolysis of fused
magnesium chloride from brines, wells and sea water. At
the cathode, the Mg2+ ions are reduced by two electrons to
magnesium metal.

Mg2+ +2e
Mg

At the anode, each pair of Cl - ions is oxidized to

chlorine gas releasing two electrons to complete the circuit

2Cl - Cl2 (g) + 2e

The major world supplier of this metal, supplying 45% of world production even as
recently at 2005.
Magnesium has ability to react with water can be hardness to
produce energy and run a magnesium-based engine.
Magnesium also reacts exothermically with most acids, such
as hydrochloric acid (HCL). Magnesium is a highly
flammable metal, but while it is easy to ignite when
powdered or shaved into this trip, it is difficult to ignite in
mass or bulk. Magnesium ribbon was used in electrically
ignited flash bulb.

Magnesium oxide
reacts with sulphuric acid
to form magnesium
sulphate and water.

H2SO4 +MgO H2O + MgSO4

Nitric acid reacts

with magnesium oxide to
produce magnesium nitrate.

2HNO +MgO H2O +Mg (NO3)2

 Magnesium reacts
with silicon-di-oxide to
form magnesium
metasilicate.

MgO +SiO2 MgSiO2

Aluminium reacts
with magnesium oxide to
produce magnesium and
aluminium oxide.

2Al +3MgO 3Mg + Al2O3

STRUCTURE OF MAGMESIUM OXIDE:

Magnesium oxide is made up of Mg2+ and O2- ions are connected to each other by an
ionic bond. Magnesium has a simple hexagonal structure and silver color. It is a part of group
2 (beryllium family). Metallic bonding occurs between the atoms od metal element-Lithium,
Beryllium, Sodium, Magnesium, Aluminium and Calcium. Valency we can say that the net
charge in the molecules is zero and balanced where we further get one Magnesium atom and
one Oxygen atom Magnesium Oxide has a giant 3D lattice structure formed by strong
electrostatic force of attraction between the positively charged magnesium ions and the
negatively charged oxygen ions. These ionic bonds required a lot of energy. The substance
has a high melting point. The outer electron is delocalized (free to move). Magnesium oxide
is a double bond element. When the bond is made with four electrons. It is called double
bond. MgO is an ionic compound. The difference in electronegativity between Magnesium
and Oxygen is relatively higher than any two atoms in covalent compound. MgO in its pure
defect free state is known to be a non-metallic semiconductor.

In MgO the ionic bond is stronger than the NaCl because of more charge on the ionic
2
species in the former (Mg+2 and O +
as compared to Na+ and Cl-). Because of this the ionic
interactions are stronger in MgO than in NaCl. Magnesium oxide have a greater number of
charges and so form stronger ionic bonds than the Na+ and Cl- ions in Sodium Chloride.
There is a large difference in electronegatively between Magnesium and Oxygen. So that
form an ionic bond in place of covalent bonds.

APPLICATION OF MAGENISUM OXIDE:

IN METAL:
 o Magnesium is the third most commonly used structural metal following iron
and aluminium. It is called as lightest useful metal.

 The components of aluminium alloys in die-casting (alloyed with zinc), to

remove Sulphur in the production of iron and steel. The production of
titanium in the Kroll process.

 Magnesium in its pure form can be compared with aluminium.

 High grade car wheels of magnesium alloy are called “Mag wheels”.

USES OF METALS:

o Magnesium is flammable, burning at a temperature of approximately 31000C

and auto ignition temperature of magnesium ribbon is approximately 4730C.

o In form of turning or ribbon to prepare Grignard reagent which are useful in

organic synthesis.

o Magnesium hydroxide suspended in water is used in milk of magnesia

antacid and laxatives.

o Magnesium sulphate as the hepta hydrate called Epsom salt is used as bath
salt as a laxative and as a highly soluble fertilizer.

o Dead-burned magnesite (magnesium carbonate) is used for refractory

purposes such as brick and liners in furnaces and converters.

o Magnesium sulphite is used in the manufacture of paper.

o Magnesium phosphate is used to fire proof wood used in construction.

o Magnesium Hexa-Fluro-Silicate is used in moth proofing of textiles.

IN ELECTRONIC DEVICE:

o Low weight, good mechanical and electrical property.

o Magnesium is widely used for manufacturing of mobile phones, laptop,

computer, camera and other electrical components.

o Magnesium was one of the main aerospace construction metals and used for
Germany military aircraft.

BIOLOGICAL ROLE:

INPLANTS

o The interaction between phosphate and magnesium ions, are essential

 to basic between leaf veins.
nucleic acid.
They are
essential to all
cells of all
known living
organisms.

o Over 300
enzymes
require the
presence of
magnesium
ions for their
catalytic
action
including all
enzymes like
synthesizing
ATP etc.

o Nucleotides
to synthesis
DNA and
RNA.

o ATP exists in
cells
normally as a
chelate of
ATP and a
magnesium
ion.

o Plants have
additional use
for
magnesium in
that
chlorophyll
are
magnesium
centered
porphyrins.

o Magnesium
deficiency in
plants leads
to late reason
yellowing
 o Spices, nuts, cereals, coffee, cocoa, tea and vegetables are rich in
magnesium.

o Green leafy vegetables such as spinach are also rich in magnesium as they
contain chlorophyll.

IN
HUMAN:

o Magnesium is a vital component of a healthy human diet. Magnesium

deficiency in human relatively rare.

o Low level of magnesium leads to number of illnesses in human such as

asthma, diabetes and osteoporosis.

o Adult body contains 24g of magnesium with 60% in skeleton, 39% in

intracellular and 1% in extracellular.

o Intracellular magnesium is correlated with intracellular potassium.

o Magnesium is absorbed in the gastro intestinal tract.

USES OF MgO NANOPARTICLES:

o High- temperature dehydrating agent of MgO used for the production of

silicon steel sheet, high grade ceramic materials, electronic industry
material, adhesive and additive in the chemical raw material.

o It is used in automobiles and airplanes

o Coatings, nanowires, plastics and nanofibers.

o It is used as antacid to relieve heart burn.

o It is used as laxative for short term rapid empty of the bowel.

o Magnesium ignites easily in air and burns with the bright light it is used
in flares, fireworks and sparklers.

o The medical application of MgO is used in cell isolation, immune assay,

diagnostic testing and drug delivery.

o Magnesium is an essential element to use in the treatment of eclampsia,

preeclampsia, arrhythmia, severe asthma and migraine.

PREPARATION OF MAGNESIUM OXIDE:

 Now-a-days, the attention of many scientists is focused on the development of new
methods for synthesis and stabilization of nanoparticles. Moreover, special attention is paid to
nano dispersed and stable particles formation. Different metals, metal oxides, sulfides,
polymers, core-shell and composite nanoparticles can be prepared using a number of
synthetic techniques, which are broadly classified into two categories namely physical
methods and chemical methods.
CHEMICAL TECHNIQUES:

 Chemical vapor deposition

 Hydro-thermal synthesis
 Sol-gel technique
 Green synthesis
 Micro emulsion technique
 Chemical precipitation
 Co-precipitation method

HYDROTHERMAL SYNTHESIS:

Hydrothermal synthesis can be defined as a method of synthesis of single crystals

which depends on the solubility of minerals in hot water under high pressure. The crystal
growth is performed in an apparatus consisting of a steel pressure vessel called autoclave, in
which a nutrient is supplied along with water. A gradient of temperature is maintained at the
opposite ends of the growth chamber so that the hotter end dissolves the nutrient and the
cooler end causes seeds to take additional growth. Possible advantages of the hydrothermal
method over the other types of crystal growth include the ability to create crystalline phase
which are not stable at the melting point. Also, materials which have a high vapor pressure
near their melting points can also be grown by the large good-quality crystal while
maintaining good control over their composition.

CHEMICAL PRECIPITATION:

Certain soluble inorganic materials can be removed by the addition of suitable

reagents to convert the soluble impurities into insoluble precipitates. These precipitates can
be flocculated and removed by sedimentation. The extent of removal depends on the
solubility of the product and this is usually controlled by factors such as pH and temperature.
Chemicals precipitation can be used in industrial waste water treatment. The solid-state
process is the more common and widely used method for production of micron-sized
particles. In solid state synthesis of nanoparticles generally heat treatment followed by milling
is carried out to get an average particle size of 100 nm or less. Mechanical milling is one of
the most preferred and earliest technique to produce metallic microcrystalline powder. People
claims to get a nanoparticle of very small size of up to 30nm particle size by using media
milling methods used by different researchers includes dry millings and ball milling
technique.

MICROEMULSION TECHNIQUE:

This is a new technique, which allows, preparation of ultrafine metal particles within
the size range 5nm<particle diameter <50nm. The rate of particle nucleation is a function of
the percolation degree of microemulsion types and formation, we mainly focus on the
kinetics of metallic particle formation. Effects of stabilizer (emulsifier) type and
concentration and the type of continuous phase, reducing agent and additive on the particle
formation are summarized and evaluated. The influence of several other parameter such as
temperature, the incident light, the nature of metals salts and reaction condition are also
reviewed. These results indicate that the nature of the stabilizer emulsifier, the surface
activity of additives and the colloidal stability of microemulsion droplets play decisive role
on the particle size and distribution during the preparation of metal and particles.
SOL-GEL METHOD:

This method for forming fine particulates in a liquid media and consolidating them
after shaping to have homogeneous layers of fine particulates after drying and heating
treatment. The starting materials for sol-gel can be metal-organic compounds or metal salts.
Possibility of obtaining special products such as powders, films or coating, microspheres,
fibers. Sol-gel method offers a unique synthesis route to produce novel and tailor-made
nanomaterials with full control of morphology, size, composition etc., This method is used
for the fabrication of metal oxide, especially the oxides of silicon and titanium. Sol-gel
process is used to produce ceramic nanoparticles. The sol-gel coating technique consists of
the immersion of a substrate that is to be coated in the “sol” solution and the vertical
extraction of this substrate at a controlled speed. The rapid evaporation of the solvent during
the extraction of the substrate. Sol-gel is a method for preparing specialty metal glasses and
ceramics by hydrolyzing a chemical precursor or mixture of precursors that pass sequentially
through a solution state and a gel state before being dehydrated to a glass or ceramic.

ADVANTAGES OF SOL-GEL METHOD:

 Can produce thick coating to provide corrosion protection performance.

 Can easily shape materials into complex geometries in a gel state.
 Can have low temperature sintering capability, usually 200-6000 C.
 Can provide a simple, economic and effective method to produce high quality coating.

DISADVANTAGES OF SOL-GEL METHOD:

 Expensive starting compounds.

 Difficulties to obtaining large scale monolits, free from crack.
 Sol-gel reaction are not reversible and impossible to completely inhibit.

CO-Precipitation:

This method is also widely used for the synthesis of nanoparticles it is based on the
principle of precipitation and very often involves liquid-phase synthesis. Sodium Hydroxide
is commonly used as the precipitation agent. The basic principle is the Homogenization of
the precipitation reaction involving two process - Nucleation and Nuclei Growth

Principles based

1. Single nucleation and uniform growth, by diffusion.

2. Nucleation growth, and aggregation of smaller substance.
3. Multiple nucleation and Ostwald ripening growth.
 Co-precipitation method is a most useful and proper method for controlled sizes
magnetic nanoparticles synthesis method.
 This method is most useful and proper method for controlled sizes magnetic
 nanoparticles synthesis method.
 It is extensively used in the biomedical application because of the case of
application and harmless procedure.
In this method, MPNS are prepared from aqueous salt solution, by the addition of a under an inert
atmosphere at room temperature or at high temperature.
 The trouble with the synthesis of nanoparticles by this method is the tendency of
particles to agglomerate because of the extremely small size which have surface area
and surface technology.

ADVANTAGES OF CO-PRECIPITATION METHOD:

Low reaction temperature and short reaction

time. High yield, high productivity.

The lack of necessity to use organic

solvents. Easily reproducible.

Low cost.
The possibility of creating pure and homogeneous material.

DISADVANTAGES OF CO-PRECIPITATION METHOD:

o The product separation after precipitation and generation of the large volume of salt
containing solution.
o Low removal efficiency.
o High energy consumption.
o Production of toxic sludge.
o Uncontrollable shape and irregular size distribution.

GREEN SYNTHESIS:

Green synthesis is an emerging area in the field of bio-nanotechnology and provides

economic and environmental benefits as an alternative to chemical and physical methods. In
this method, nano- toxic safe reagent which are eco-friendly and bio safe used. Grenn
synthesis employs a clean, safe, cost effective and environmentally friendly process of
constructing nanomaterials. Microorganism such as bacteria, yeast, fungi, algae and certain
plants act as substrate for the green synthesis of nanoparticles. This method eliminates the use
of expensive chemical, consume less energy and generate environmentally benign product
and by products.
 CHAPTER-IV
CHARACTERIZATION
TECHNIQUES
INTRODUCTION:
Nanoparticles characterization is an important step of understanding control of
nanoparticles synthesis and application. Because of small size that is of the order of one
hundredth part of the wavelength of light the individual nanoparticles cannot be viewed by
the human eyes. Thus some specialized technique are required view the nanoparticles. Such
technique is called the characterization techniques.
Thus, techniques are also helpful to know the particle size distribution in the
materials surface morphology, interface volume ratio, lattice vibrational modes, band
structure and lattice constant etc., X-RAY DIFFRACTION METHOD:

XRD is one of the most important tools of solid-state chemistry, since it constitutes a
powerful and readily available method for determining atomic arrangements in matter. X-ray
diffraction method depend upon the fact that X-ray wavelength of the order of 1 nanometer
are readily available and that is the order of magnitude of atomic dimensions. When an X-ray
beam falls on matter, scattered waves spread out spherically from all the atoms in the sample,
and the interference effects of the scattered radiation from the different atoms cause the
intensity of the scattered radiation to exhibit maxima and minima in various direction. Crystal
structure and lattice constant of nanoparticles, nanowires, and thin film. This experimental
technique is also being used to determine the material is amorphous or crystalline in nature.
Crystalline phases can be identified by comparing the D values obtained from XRD data with
the fundamental data in joint committee on powder diffraction standard.

PRINCIPLE:

X-ray interacts with electrons in matter. When the beam of X-rays impinges
on a material it is scattered in various directions by the electron of the atoms. Interference
pattern occurs only if the wavelength of X-rays used is compared with the separation between
the atoms. For an order array of scattering centers (atoms or ions in a crystalline solid), gives
rise to interface maxima and minima. The wavelength of X-rays and used in XRD experiment
typically lies between 0.6 and 1.9 A0. Crystals are regular array of atoms, and X-rays can be
considered waves of electromagnetic radiations. Atoms scatter X-ray waves, primarily
through the atom electrons. A regular array of scatters produces a regular array of spherical
waves. Although these waves cancel one another out in most directions through destructive
interference, they add constructively in a few specific directions.
WORKING:

In 1916, Debye and Scherrer in Germany and Hull in USA independently

obtained X-ray diffraction patterns from sample in powder form. Therefore, sometime this
method is called Hull Debye Scherrer method. The monochromatic X-ray beam strikes the
powdered specimen kept in this walled capillary. The X-ray are diffracted from specific
planes making angle   with the beam and obeying Bragg’s law. The diffraction rays
generate cone, concentric with incident beam. The full opening angle of the diffraction cone
4ѳ is determined by measuring the distance S between diffraction lines corresponding to a
particular plane is related to the Bragg angle by the equation (4 ѳ = S/R radians).

Where R is the specimen to film distance, usually the radius of camera housing
the film. A list of  values can be obtained from the measured values of S. Since the
wavelength is known substitution of   and lambda gives a list of spacing d. Each spacing
d is the distance between neigbouring planes (hkl). This method is used to study structures of
metal and other commercially important solids. This method does not require single crystal.

By measuring the distance between symmetrical lines and the intensities

following information is obtained:

A crystalline substance can be distinguished from an amorphous one because the

former produce line on photographs the does not if photographs are made before and after
heat treatment, the comparison can reveal any alteration in the lattice with the aid of standard
photograph of known chemical compounds their presence may detected in an unknown
mixture. This size of unit cell and type of lattice may be determined.

X-ray diffraction is based on the construction interference of monochromatic X-ray

and a crystalline sample. These X-ray are generated by a cathode ray tube, filtered to produce
monochromatic radiation, collimated to concentrate, and directed towards the sample. THE
interaction of the incident rays with the sample produces constructive interference when
conditions of Bragg’s Law is satisfied.

2dsin =n

This law related wavelength of electromagnetic radiation to the diffraction

angle and lattice spacing in a crystalline sample. These diffraction X-rays are then
detected processed and counted. By scanning the sample through a range of 2  angles,
all possible diffraction direction of peaks to d-spacing allows identification of the mineral
because each mineral has a set of unique d- spacing. Typically, this is achieved by
comparison of d-spacing with standard reference patterns.
 Grain size determined by the broadening of X-ray diffraction peaks. This peak
broadening is normally caused by the finite size effect of crystalline. If the average
crystal size in powder is below a certain limit (200nm diameter), additional broadening
of diffraction beams occurs. The grain size can be calculated from the broadening of the
diffraction beam using the Scherrer’s formula,

D=K/cos