CARBON AND RICE HUSK ASH INFUSED WITH SPIONS FOR

PHOTOCATLYTIC DEGRADATION
Project work submitted in partial fulfillment of the requirements
for the award of the Degree of
MASTER OF SCIENCE

IN

PHYSICS

by

THATCHAYANI A

REG No: 181220659

DEPARTMENT OF PHYSICS

MEENAKSHI COLLEGE FOR WOMEN

(AUTONOMOUS)

CHENNAI – 600 024.

APRIL 2021
 BONAFIDE CERTIFICATE

This is to certify that the project work entitled SYNTHESIS, GROWTH,

OPTICAL AND DIELECTRIC PROPERTIES OF 2-AMINO-3-

PROPANOIC 4- THYLBENZENESULFONATE (2A3PMS) SINGLE
CRYSTAL GROWN BY SLOW EVOPORATION TECHNIQUE is a
bonafide work carried out by Ms.THATCHAYANI A in the partial fulfillment of the
requirement for the award of degree of Master in Science in Physics for the academic year
2019–2020, under the external guide Dr. P.ARULMOZHICHELVAN , Associate
Professor & Head , PG and Research Department of Physics, Pachaiyappa’s College Chennai
– 600 030 and the internal guide Mrs. SUBA CHANDRASEKAR, Assistant Professor,
Department of Physics, Meenakshi College for Women (Autonomous), Kodambakkam,
Chennai-600 024.

Internal guide External

guide
Mrs. Suba Chandrasekar Dr.
P.ARULMOZHICHELVAN
Assistant Professor Associate Professor &
Head
Department of Physics PG and Research Department of
Physics
Meenakshi College for Women (Autonomous) Pachaiyappa’s
College
Kodambakkam Chennai – 600
030
Chennai - 600 024

Head of the Department External

Examiner
Mrs. V.Vijayashri
Associate Professor
Department of Physics
Meenakshi College for Women (Autonomous)
Kodambakkam
Chennai – 600 024
DECLARATION

Certified that this project work entitled SYNTHESIS, GROWTH, OPTICAL

AND DIELECTRIC PROPERTIES OF 2-AMINO-3-PROPANOIC 4-

THYLBENZENESULFONATE (2A3PMS) SINGLE CRYSTAL GROWN
BY SLOW EVOPORATION TECHNIQUE is a bonafide record of independent
work done by me under the supervision of external guide Dr. P.ARULMOZHICHELVAN,
Associate Professor & Head , PG and Research Department of Physics, Pachaiyappa’s
College Chennai – 600 030 and internal guide Mrs. SUBA CHANDRASEKAR, Assistant
Professor, Department of Physics, Meenakshi College for Women (Autonomous),
Kodambakkam, Chennai-600 024. Certified that the work reported here is not from part of
any other thesis or dissertation on the basis of which a degree for award was conferred
earlier.

THATCHAYANI A

Place: Chennai II M.Sc.

Physics
Date: Meenakshi College for Women
(Autonomous)
Chennai - 600
024.
 HYPERTHERMIA
TABLE OF CONTENTS
CHAPTER 1

1.INTRODUCTION
1.1NANOSCIENCE AND NANOTECHNOLOGY
1.2 NANOPARTICLES
1.2.1. SUPER PARAMAGNETIC IRON OXIDE NANOPARTICLES(SPIONS)
1.3. CLASSIFICATION OF NANOPARTICLES
1.3.1.
1.3.2.
1.3.3.
1.4. SYNTHESIS OF NANOPARTICLES
1.4.1.
1.4.2.
1.4.3.
1.5. SYNTHESIS OF IRON OXIDE NANOPARTICLES
1.6. PROPERTIES OF NANOPARTICLES
1.6.1. PHYSICAL PROPERTIES
1.6.2. CHEMICAL PROPERTIES
1.6.3. BIOLOGICAL PROPERTIES
1.6.4. MECHANICAL PROPERTIES
1.6.5. MAGNETIC PROPERTIES
1.6.7. OTHER PROPERTIES
1.7. APPLICATIONS OF NANOPARTICLES
CHAPTER 2
2.1. MATERIALS AND METHODS
2.1.1. BRIEF INFORMATION ABOUT THE MATERIALS USED
2.2. SYNTHESIS OF IRON OXIDE NANOPARTICLES
2.3.
CHAPTER 3
3.RESULTS AND DISCUSSION
3.1. UV SPECTROSCOPY
3.2. X-RAY DIFFRACTION
3.3. FT-IR SPECTROSCOPIC ANALYSIS
3.4. FE-SEM WITH EDAX
CHAPTER 4
4.CONCLUSION

CHAPTER 1

1.INTRODUCTION
1.1 NANOSCIENCE AND NANOTECHNOLOGY
Nanoscience is the study of phenomena and manipulation of materials at atomic,
molecular and macromolecular scales when properties differ significantly from those at larger
scales. Nanotechnology is the design, characterisation, production of and application of
structures, devices and systems by controlling shape and size at the nanometres scale.
Nanoscience is an interdisciplinary field at the boundaries of most science and engineering
areas. At the minimum you need chemistry to make the materials, physics to understand the
properties, and engineering to develop applications.
1.2 NANOPARTICLES
Nanotechnology is a known field of research since last century. Since ‘‘nanotechnology”
was presented by Nobel laureate Richard P. Feynman during his well famous 1959 lecture
‘‘There’s Plenty of Room at the Bottom” (Feynman, 1960), there have been made various
revolutionary developments in the field of nanotechnology. Nanotechnology produced
materials of various types at nanoscale level. Nanoparticles (NPs) are wide class of materials
that include particulate substances, which have one dimension less than 100 nm at least.
Depending on the overall shape these materials can be 0D,1D, 2D or 3D. The importance of
these materials realized when researchers found that size can influence the physiochemical
properties of a substance e.g. the optical properties. A 20-nm gold (Au), platinum (Pt), silver
(Ag), and palladium (Pd) NPs have characteristic wine red colour, yellowish grey, black and
dark black colours, respectively.
Nanoparticles (NPs) are at the forefront of rapid development in nanotechnology. Their
exclusive size-dependent properties make these materials indispensable and superior in many
areas of human activities. Being the most current transition metal in the Earth’s crust, iron
stands as the backbone of current infrastructure. Iron and oxygen chemically combine to
form iron oxides (compounds), and there are ~16 identified iron oxides. In nature, iron(III)
oxide is found in the form of rust. Generally, iron oxides are prevalent, widely used as they
are inexpensive, and play an imperative role in many biological and geological processes.
They are also extensively used by humans, e.g., as iron ores in thermite, catalysts, durable
pigments (coatings, paints, and coloured concretes), and haemoglobin. The three most
common forms of iron oxides in nature are magnetite (Fe3 O4 ), maghemite (g-Fe2 O3 ), and
hematite (α-Fe2 O3).
Magnetic materials include elemental metals, alloys, oxides, and other chemical compounds
that are magnetized by an external magnetic field. This is an important phenomena normally
present only in NP systems.2,6 Due to their low toxicity, superparamagnetic properties, such
as surface area and volume ratio, and simple separation methodology, magnetic iron oxide
(Fe3 O4 and g-Fe2 O3 ) NPs have attracted much attention and are especially interesting in
biomedical applications for protein immobilization, such as diagnostic magnetic resonance
imaging (MRI), thermal therapy, and drug delivery. Iron’s reactivity is important in
macroscopic applications (particularly rusting), but is a dominant concern at the nanoscale.
Finely divided iron is considered pyrophoric. These are the reasons that iron NPs could not
capture much attention. The extreme reactivity of iron makes it difficult to study and
inconvenient for applications. However, potent magnetic and catalytic properties have
diverted the attention toward iron’s potential. Iron oxide NPs can be easily and promptly
induced into magnetic resonance by self-heating, applying the external magnetic field, and
also by moving along the field of attraction. Synthetic methods, crystallization, size, shape,
and quality of the iron oxide NPs greatly affect these behaviours. It is obvious that these
approaches toward the synthesis of well-crystallized and size-controlled iron oxide NPs offer
more prospects for these applications. The shapes of nanomaterials (NMs) also exert
tremendous impact on their properties, including catalysis. Shape change shows crystal
facets, and the atomic arrangements in each facet have reflective effects on its properties. The
development of protocols for desired morphology, size, and shape is under consideration.
Iron oxide NPs have been synthesized using mechanochemical (i.e., laser ablation arc
discharge, combustion, electrodeposition, and pyrolysis) and chemical (sol–gel synthesis,
template-assisted synthesis, reverse micelle, hydrothermal, coprecipitation, etc) methods.
Various shapes of iron oxides (i.e., nanorod, porous spheres, nano husk, nano cubes, distorted
cubes, and self-oriented flowers) can be synthesized using nearly matching synthetic
protocols, by simply changing the precursor iron salts. These novel protocols are easy to
implement, economical, and control shape, in a sustainable manner.
NPs are broadly divided into various categories depending on their morphology, size and
chemical properties. Based on physical and chemical characteristics, some of the well
known classes of NPs are given as below.
1.Carbon-based NPs

Fullerenes and carbon nanotubes (CNTs) represent two major classes of carbon-based NPs.
Fullerenes contain nanomaterial that are made of globular hollow cage such as allotropic
forms of carbon. They have created noteworthy commercial interest Nanoparticles due to
their electrical conductivity, high strength, structure, electron affinity, and versatility. These
materials possess arranged pentagonal and hexagonal carbon units, while each carbon is sp2
hybridized.
The rolled sheets can be single, double or many walls and therefore they named as single-
walled (SWNTs), double-walled (DWNTs) or multi-walled carbon nanotubes (MWNTs),
respectively. They are widely synthesized by deposition of carbon precursors especially the
atomic carbons, vaporized from graphite by laser or by electric arc on to metal particles.
Lately, they have been synthesized via chemical vapor deposition (CVD) technique. Due to
their unique physical, chemical and mechanical characteristics, these materials are not only
used in pristine form but also in nanocomposites for many commercial applications such as
fillers, efficient gas adsorbents for environmental remediation, and as support medium for
different inorganic and organic catalyst.

2.2. Metal NPs

Metal NPs are purely made of the metal precursors. Due to well-known localized surface
plasmon resonance (LSPR) characteristics, these NPs possess unique optoelectrical
properties. NPs of the alkali and noble metals i.e., Cu, Ag and Au have a broad absorption
band in the visible zone of the electromagnetic solar spectrum. The facet, size and shape
controlled synthesis of metal NPs is important in present day cutting-edge materials. Due to
their advanced optical properties, metal NPs find applications in many research areas. Gold
NPs coating is widely used for the sampling of SEM, to enhance the electronic stream, which
helps in obtaining high quality SEM images.

2.3. Ceramics NPs

Ceramics NPs are inorganic non-metallic solids, synthesized via heat and successive cooling.
They can be found in amorphous, polycrystalline, dense, porous or hollow form. Therefore,
these NPs are getting great attention of researchers due to their use in applications such as
catalysis, photocatalysis, photodegradation of dyes, and imaging applications.

2.4. Semiconductor NPs

Semiconductor materials possess properties between metals and nonmetals and therefore they
found in various applications. Semiconductor NPs possess wide bandgaps and therefore
showed significant alteration in their properties with bandgap tuning. Therefore, they are very
important materials in photocatalysis, photo optics and electronic devices. As an example,
variety of semiconductor NPs are found exceptionally efficient in water splitting applications,
due to their suitable bandgap and band edge positions.

2.5. Polymeric NPs

These are normally organic based NPs and in the literature a special term polymer
nanoparticle (PNP) collective used for it. They are mostly nanospheres or nano capsular
shaped. The former are matrix particles whose overall mass is generally solid and the other
molecules are adsorbed at the outer boundary of the spherical surface. In the latter case the
solid mass is encapsulated within the particle completely.
Different types of nanoparticles

Nanoparticles can be classified into different types according to the size, morphology,
physical and chemical properties. Some of them are carbon-based nanoparticles, ceramic
nanoparticles, metal nanoparticles, semiconductor nanoparticles, polymeric nanoparticles and
lipid-based nanoparticles.

Carbon-Based Nanoparticles

Carbon-based nanoparticles include two main materials: carbon nanotubes (CNTs) and
fullerenes. CNTs are nothing but graphene sheets rolled into a tube. These materials are
mainly used for the structural reinforcement as they are 100 times stronger than steel.

CNTs can be classified into single-walled carbon nanotubes (SWCNTs) and multi-walled
carbon nanotubes (MWCNTs). CNTs are unique in a way as they are thermally conductive
along the length and non-conductive across the tube.

Fullerenes are the allotropes of carbon having a structure of hollow cage of sixty or more
carbon atoms. The structure of C-60 is called Buckminsterfullerene, and looks like a hollow
football. The carbon units in these structures have a pentagonal and hexagonal arrangement.
These have commercial applications due to their electrical conductivity, structure, high
strength, and electron affinity.

Ceramic Nanoparticles

Ceramic nanoparticles are inorganic solids made up of oxides, carbides, carbonates and
phosphates. These nanoparticles have high heat resistance and chemical inertness. They have
applications in photocatalysis, photodegradation of dyes, drug delivery, and imaging.

By controlling some of the characteristics of ceramic nanoparticles like size, surface area,
porosity, surface to volume ratio, etc, they perform as a good drug delivery agent. These
nanoparticles have been used effectively as a drug delivery system for a number of diseases
like bacterial infections, glaucoma, cancer, etc.

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Metal Nanoparticles

Metal nanoparticles are prepared from metal precursors. These nanoparticles can be
synthesized by chemical, electrochemical, or photochemical methods. In chemical methods,
the metal nanoparticles are obtained by reducing the metal-ion precursors in solution by
chemical reducing agents. These have the ability to adsorb small molecules and have high
surface energy.

These nanoparticles have applications in research areas, detection and imaging of

biomolecules and in environmental and bioanalytical applications. For example gold
nanoparticles are used to coat the sample before analyzing in SEM. This is usually done to
enhance the electronic stream, which helps us to get high quality SEM images.

Semiconductor Nanoparticles
Semiconductor nanoparticles have properties like those of metals and non-metals. They are
found in the periodic table in groups II-VI, III-V or IV-VI. These particles have wide
bandgaps, which on tuning shows different properties. They are used in photocatalysis,
electronics devices, photo-optics and water splitting applications.

Some examples of semiconductor nanoparticles are GaN, GaP, InP, InAs from group III-V,
ZnO, ZnS, CdS, CdSe, CdTe are II-VI semiconductors and silicon and germanium are from
group IV.

Polymeric Nanoparticles

Polymeric nanoparticles are organic based nanoparticles. Depending upon the method of
preparation, these have structures shaped like nanocapsular or nanospheres. A nanosphere
particle has a matrix-like structure whereas the nanocapsular particle has core-shell
morphology. In the former, the active compounds and the polymer are uniformly dispersed
whereas in the latter the active compounds are confined and surrounded by a polymer shell.

Some of the merits of polymeric nanoparticles are controlled release, protection of drug
molecules, ability to combine therapy and imaging, specific targeting and many more. They
have applications in drug delivery and diagnostics. The drug deliveries with polymeric
nanoparticles are highly biodegradable and biocompatible.

Lipid-Based Nanoparticles

Lipid nanoparticles are generally spherical in shape with a diameter ranging from 10 to
100nm. It consists of a solid core made of lipid and a matrix containing soluble lipophilic
molecules. The external core of these nanoparticles is stabilized by surfactants and
emulsifiers. These nanoparticles have application in the biomedical field as a drug carrier and
delivery and RNA release in cancer therapy.

Thus, the field of nanotechnology is far from being saturated and it is, as the statistic says,
sitting on the staircase of an exponential growth pattern. It is basically at the same stage as
the information technology was in the 1960s and biotechnology in the year of 1980s. Thus it
can easily be predicted that this field would witness a same exponential growth as the other
two technological field witnessed earlier.
3. Synthesis of nanoparticles

Various methods can be employed for the synthesis of NPs, but these methods are broadly
divided into two main classes i.e. (1) Bottom-up approach and (2) Top-down approach. These
approaches further divide into various subclasses based on the operation, reaction condition
and adopted protocols.

3.1. Top-down syntheses

In this method, destructive approach is employed. Starting from larger molecule, which
decomposed into smaller units and then these units are converted into suitable NPs. Examples
of this method are grinding/milling, CVD, physical vapor deposition (PVD) and other
decomposition techniques. This approach is used to synthesized coconut shell (CS) NPs. The
milling method was employed for this purpose and the raw CS powders were finely milled
for different interval of times, with the help of ceramic balls and a well known planetary mill.
They showed the effect of milling time on the overall size of the NPs through different
characterization techniques. It was determined that with the time increases the NPs crystallite
size decreases, as calculated by Scherer equation. They also realized that with each hour
increment the brownish colour faded away due to size decrease of the NPs. The SEM results
were also in an agreement with the Xray pattern, which also indicated the particle size
decreases with time. One study revealed the spherical magnetite NPs synthesis from natural
iron oxide (Fe2O3) ore by top-down destructive approach with a particle size varies from 20
to 50 nm in the presence of organic oleic acid. A simple top-down route was employed to
synthesize
colloidal carbon spherical particles with control size. The synthesis technique was based on
the continuous chemical adsorption of polyoxometalates (POM) on the carbon interfacial
surface. Adsorption made the carbon black aggregates into relatively smaller spherical
particles, with high dispersion capacity and narrow size distribution. It also revealed from the
micrographs, that the size of the carbon particles become smaller with sonication time. A
series of transition-metal dichalcogenide nanodots (TMD-NDs) were synthesized by
combination of grinding and sonication top-down techniques from their bulk crystals. It was
revealed that almost all the TMD-NDs with sizes <10 nm show an excellent dispersion due to
narrow size distribution. Lately, highly photoactive active Co3O4 NPs were prepared via top-
down laser fragmentation, which is a top-down process. The powerful laser irradiations
generate well-uniform NPs having good oxygen vacancies. The average size of the Co3O4
was determined to be in the range of 5.8 nm ± 1.1 nm.

3.2. Bottom-up syntheses

This approach is employed in reverse as NPs are formed from relatively simpler substances,
therefore this approach is also called building up approach. Examples of this case are
sedimentation and reduction techniques. It includes sol gel, green synthesis, spinning, and
biochemical synthesis. Mogilevsky et al. synthesized TiO2 anatase NPs with graphene
domains through this technique. They used alizarin and titanium isopropoxide precursors to
synthesize the photoactive composite for photocatalytic degradation of methylene blue.
Alizarin was selected as it offers strong binding capacity with TiO2 through their axial. More
recently, solvent-exchange method is used to achieve limit sized low density lipoprotein
(LDL) NPs for medical cancer drug delivery purpose by Needham et al. In this method
nucleation is the bottom approach followed by growth which is the up approach. The LDL
NPs were obtained without using phospholipid and possessed high hydrophobicity, which is
essential for drug delivery applications.
The monodispersed spherical bismuth (Bi) NPs were synthesized by both top-down and
bottom-up approaches. These NPs have excellent colloidal properties. In the bottom-up
approach bismuth acetate was boiled within ethylene glycol, while in top-down approach the
bismuth was converted into molten form and then the molten drop was emulsified within the
boiled diethylene glycol to produce the NPs. The size of the NPs obtained by both methods
was varied from 100 nm to 500 nm. Green and biogenic bottom-up synthesis attracting many
researchers due to the feasibility and less toxic nature of processes. These processes are cost-
effective and environmental friendly, where synthesis of NPs is accomplished via biological
systems such as using plant extracts. Bacteria, yeast, fungi, Aloe vera, tamarind and even
human cells are used for the synthesis of NPs. Au NPs have been synthesis from the biomass
of wheat and oat and using the microorganism and plant extracts as reducing agent.

5. Physicochemical properties of NPs

As discussed earlier, various physicochemical properties such as large surface area,

mechanically strong, optically active and chemically reactive make NPs unique and suitable
applicants for various applications. Some of their important properties are discuss in the
following section.

5.1. Electronic and optical properties

The optical and electronic properties of NPs are interdependent to greater extent. For
instance, noble metals NPs have size dependent optical properties and exhibit a strong UV–
visible extinction band that is not present in the spectrum of the bulk metal. This excitation
band results when the incident photon frequency is constant with the collective excitation of
the conduction electrons and is known as the localized surface plasma resonance (LSPR).
LSPR excitation results in the wavelength selection absorption with extremely large molar
excitation coefficient resonance Ray light scattering with efficiency equivalent to that of ten
fluorophores and enhanced local electromagnetic fields near the surface of NPs that enhanced
spectroscopies. It is well established that the peak wavelength of the LSPR spectrum is
dependent upon the size, shape and interparticle spacing of the NPs as well as its own
dielectric properties and those of its local environment including the substrate, solvents and
adsorbates. Gold colloidal NPs are accountable for the rusty colours seen in blemished glass
door/windows, while Ag NPs are typically yellow. Actually, the free electrons on the surface
in these NPs (d electrons in Ag and gold) are freely transportable through the nanomaterial.
The mean free path for Nanoparticles 921Ag and gold is 50 nm, which is more than the NPs
size of these materials. Thus, no scattering is expected from the bulk, upon light interaction,
instead they set into a standing resonance conditions, which is responsible for LSPR in these
NPs.

5.2. Magnetic properties

Magnetic NPs are of great curiosity for investigators from an eclectic range of disciplines,
which include heterogenous and homogenous catalysis, biomedicine, magnetic fluids, data
storage magnetic resonance imaging (MRI), and environmental remediation such as water
decontamination. The literature revealed that NPs perform best when the size is <critical
value i.e. 10–20 nm. At such low scale the magnetic properties of NPs dominated effectively,
which make these particle priceless and can be used in different applications. The uneven
electronic distribution in NPs leads to magnetic property. These properties are also dependent
on the synthetic protocol and various synthetic methods such as solvothermal coprecipitation,
micro-emulsion, thermal decomposition, and flame spray synthesis can be used for their
preparation.

5.3. Mechanical properties

The distinct mechanical properties of NPs allow researchers to look for novel applications in
many important fields such as tribology, surface engineering, nanofabrication and
nanomanufacturing. Different mechanical parameters such as elastic modulus, hardness,
stress and strain, adhesion and friction can be surveyed to know the exact mechanical nature
of NPs. Beside these parameters surface coating, coagulation, and lubrication also aid to
mechanical properties of NPs. NPs show dissimilar mechanical properties as compared to
microparticles and their bulk materials. Moreover, in a lubricated or greased contact, the
contrast in the stiffness between NPs and the contacting external surface controls whether the
NPs are indented into the plan surface or deformed when the pressure at contact is
significantly large. This important information could divulge how the NPs perform in the
contact situation. Decent controls over mechanical features of NPs and their interactions with
any kind of surface are vital for enlightening the surface quality and elevating material
removal. Fruitful outcomes in these fields generally need a deep insight into the basics of the
mechanical properties of NPs, such as elastic modulus and hardness, movement law, friction
and interfacial adhesion and their size dependent characteristics.

5.4. Thermal properties

It is well-known fact that metals NPs have thermal conductivities higher than those of fluids
in solid form. For example, the thermal conductivity of copper at room temperature is about
700 times greater than that of water and about 3000 times greater than that of engine oil.
Even oxides such as alumina (Al2O3) have thermal conductivity higher than that of water.
Therefore, the fluids containing suspended solid particles are expected to display significantly
enhanced thermal conductivities relative to those of conventional heat transfer fluids.
Nanofluids are produced by dispersing the nanometric scales solid particles into liquid such
as water, ethylene glycol or oils. Nanoparticles to those of conventional heat transfer fluids
and fluids containing microscopic sized particles. Because the heat transfer takes place at the
surface of the particles, it is desirable to use the particles with large total surface area. The
large total surface area also increases the stability suspension. Recently it has been
demonstrated that the nanofluids consisting of CuO or Al2O3 NPs in water or ethylene
exhibit advance thermal conductivity.

CHAPTER 2
INTRODUCTION:
From the last quarter half of the 20 th century, photo catalytic degradation of dyes has
been pursued in-depth in their research (Olga sacco et al., M.Z.B.Mukhtish et al., Khan
mamun reza et al., AK.Khataee et al., Akpan et al., M.A.Rauf et al and S.Salman et al.,
M.A.Rauf et al). The use of organic dyes in various industrial process, including paper, pulp,
plastic, dyeing, leather and printing industries, has increased extensively over the last few
decades. Worldwide, 450 000 ton of organic dyes are produced annually and more than 11%
are lost in effluents during the manufacturing and application processes. Most of the organic
dyes are toxic and potentially carcinogenic. Improper effluent disposal into aquatic systems
leads to a decrease in sunlight penetration, which in turns diminishes photosynthetic activity,
resulting in acute toxic effects on the aquatic fauna and low dissolved oxygen concentrations.
Therefore, the removal of dyes from industrial effluents is a major environmental problem.
Various methods have been suggested to handle the removal of dyes from the wastewater,
including biodegradation, coagulation, adsorption, etc., Among them, the photocatalytic
degradation technique is superior to than other traditional techniques, because of their ability
to degrade the dyes in wastewater both quickly and economically viable. Over the past few
decades, titanium dioxide (TiO2, titania) and carbon nanomaterials have received much
attention as interesting materials in this field. These nanomaterials have made a substantial
contribution toward the generation of dye removal. In that, Heterogeneous photo catalysis is a
unique method which has been widely used for the degradation of dyes or bleaching of dyes
(V.K.Pandit et al), especially this reaction is mainly accelerated through light while a
heterogeneous reaction consist of two phases. Eg. a liquid and a solid (9). It is the most
promising technology for the removal of dyes from waste water. Therefore, it has great
importance in and as eco-friendly, low-cost and sustainable technology. (10) Nowadays, the
synthetic dyes are extensively used in daily used products like clothes, leather accessories,
and furniture and in also plastic products. During the dyeing process approximately 20% of
this wastage enters into the environment and nearly 12% of these dyes will exclude as a
waste. [11]
Azo-dye is the largest group of dyes. In the presence of HCL+ NaNO 2 at freezing
temperature, it produce a diazonium salt, usually it is a diazotisation of a primary amine, then
it was coupled with aromatic compounds and it produces an azo dye.[12]Using azo-dye (Rh
B) dye degradation process is done. Generally Azo-dye is a large class of synthetic dyes
whose molecules contain two adjacent nitrogen atoms between carbon atoms. Azo-dyes are
organic compounds that bearing the functional group R-N=N-R’. (i.e,) R and R’ are aryl.
Chemically azo-dyes are azo-pigments, which is insoluble in water and other solvents. Azo-
dyes are widely treated as a textiles, and in some foods.
Many dyes and pigments are hazardous and may be toxic or human. Dyes with high
concentration may cause ulceration of skin, severe irritation in respiratory tracks, dermatitis,
pain, haemorrhage and diarrhoea. [13]
Activated carbon also known as activated charcoal (AC) is a highly porous form of
carbon with porosity spanning the macro- (λ>50 nm), meso (0.5–1µm) and micro (<1 µm)
pore ranges and very high-surface typically up to 900–1200 m 2 g-1.343. It is generally produced
from cheap carbonaceous source materials such as nutshells, coconut husk, peat, wood, coir,
lignite, coal, and petroleum pitch. Use of activated carbon is the most common method
applied for dye removal by adsorption. In particular, 80 activated carbon (AC) has been
extensively researched as a support for heterogeneous catalysis, Due to its higher
effectiveness, it has been applied on adsorbing cationic, mordant, and acid dyes and to
dispersed, vat, direct, pigment and reactive dyes on a slightly lesser extent. Effective
performance using activated carbon mainly dependents upon the type of carbon being used
and the characteristics of the aqueous solution containing various 90 chemicals and non-
targeted contaminants. Regeneration or reuse can result in a steep reduction in performance,
and efficiency of dye removal. Activated carbon, like many other dye-removal treatments is
considered suitable for one particular type of pollutant or waste system and ineffective on
another. Although, 95 activated carbon is expensive it comes with the advantage of
regeneration. However, this reactivation usually results into 10-15% loss of the sorbent.
Arana et al, prepared AC and TiO2 catalysts having varying proportion. The results showed
that the AC in addition to increasing surface area can also modify the acid–base properties
and the UV spectrum of TiO2. It was reported that activity of AC was increased under solar
irradiation. In AC-TiO2 system, the adsorption capacity of AC enhances the chances of high
concentration of reactants to come in contact with TiO2 and possibly turning them into their
intermediates as explained. Zhang et al proposed a similar illustration for the photocatalyzed
mineralization of methyl orange to understand the effect of presence of AC onto TiO2 for
effective dye degradation.
Carbon blacks, a very pure form of soot, constitute a group of materials that are
characterized by having nearly spherical carbon particles of colloidal size (diameter less than
50nm) that may aggregate and form agglomerates (~250nm). Carbon black is a widely used
support for heterogeneous electro-catalysts due to its high surface area, porosity, stability in a
variety of liquid media, and good electrical conductivity. However, its instability under the
highly acidic or alkaline conditions of a fuel cell, resulting in the corrosion of the carbon
support and detachment of the catalyst nanoparticles, may present itself as a limitation in its
use in photocatalytic degradation applications. Carbon black presents an alternative to its
more popular counterpart-activated carbonas a photocatalyst support. The removal of toxic
organic compounds from waste water by means of adsorption onto activated carbon is a well-
konown process. The use of carbon as a suportive material, which would provide
simultaneous adsorption and catalytic degradation of toxic organic polutants.
Rice is one of the oldest ancient crops, which was initially planted thousands of years
ago. Nowadays, rice is cultivated over 100 countries and consumed as staple food by more
than half of the world’s population. In the past 20years, the output of rice increased by almost
50%.The kernel of rice mainly consists of endosperm, husk, bran, and germ, in which the
endosperm accounts for 70%, rice husk (RH) for 20–21%, rice bran for 6–8%, and rice germ
for 1%, respectively, of the total seed weight. During production of milled rice, large
quantities of RH are produced as by products. Theoretically, about 41.64 million tons of RH
are generated in China alone, which is a major issue for the rice milling industry. Currently,
most RH is underutilized or left unused. It is difficult to use RH efficiently due to the intrinsic
properties of RH such as hard surface, poor nutritive value, high silicon content, low bulk
density, and difficult to decompose with bacteria. Previous treatment of RH including onsite
burning to produce steam or electricity, open dumping, or land-filling also led to serious
environmental pollution including smog, dust, and a greenhouse effect.On the other hand,
when RH is burned, vast amounts of rice husk ash (RHA) are produced, which could be
another source of pollution. Therefore it is important to utilize RH/RHA comprehensively
and efficiently.RH is a potential material, either in its raw form or in ash form, for production
of many value-added products.
This introduces the utilization of RH/RHA as a bioadsorbent.. RHA is a general term
describing all types of ash produced by combustion of RH. When RH is incinerated, it
produces 17%–20% of RHA, which is a lightweight, bulky, and highly porous material with a
density of around 180–200kg/m3. There are two types of RHA, that is, white rice husk ash
(WRHA) and black rice husk ash (BRHA), depending on whether the combustion is complete
or incomplete (Ugheoke and Mamat, 2012a). The controlled combustion of RH in the
atmosphere can lead to production of WRHA containing almost pure silica (>95%) in a
hydrated amorphous form with high porosity and reactivity (Vlaev et al., 2003). The
controlled pyrolysis of RH in nitrogen or inert atmosphere results in production of BRHA
containing different amounts of carbon and silica (Ghaly and Mansaray, 1999). After
combustion of RH, the obtained RHA mainly contains SiO2 and carbon, and still retains a
cellular structure skeleton with large specific surface area and high porosity.
RHA is insoluble in effluent, and exhibits good chemical stability and high
durability, therefore it has tremendous potential as a bioadsorbent for removal of fatty
acids and pigments in the vegetable oil refining process, and heavy metals, dyes,
pesticides, and other organic pollutants from waste water.Contamination of air, water,
and soil with heavy metal ions is hazardous to the Earth. Many efforts have been made
to use RH/RHA as a cheap and low-cost adsorbent in the removal of heavy metals from
the aqueous environment. The most investigated metals include Cd, Pb, Zn, Cu, Co, Ni,
and Hg from waste water. The capability and rate of absorption of RH/RHA are
dependent on various parameters such as the effect of pH, initial concentration,
agitation rate, sorbent dosage, contacting time, and temperature.As a low-cost
bioadsorbent, RH/RHA could effectively remove metals including Cd, Pb, Zn, Cu, Co,
Ni, and Hg from waste water. Moreover, RHA has been used in vegetable oil refining
process for adsorption of free fatty acid, phospholipids, and pigments. Nowadays, the
use of RH and its thermal degradation product (RHA) is still a hot topic in many
studies, but most of them have been performed on a laboratory scale. Compared with
the huge amount of RH produced worldwide each year, the comprehensive applications
of RH/RHA are relatively underutilized. Therefore the opportunities for RH/RHA in
incorporation into silica and silicon-based materials, building materials, bioenergies,
bioadsorbents, and even foods are vast. It could be assumed that the production and
usage of RH/RHA and its constituents will continue to competitively increase. As a
natural, sustainable, and renewable biomass resource, RH/RHA could become a
potential precursor for the production of high value-added silica or silicon-based
materials for practical applications. The comprehensive utilization of RH/RHA not only
facilitates utilization of an abundantly available agro-waste to value-added products but
also helps to reduce the environmental pollution. Rice husk contains organic molecules
such as cellulose, Lignin, D-xylose,Larabinose, methyl glucuronic acid, D-galctose,
[21]
 Rice husk ash also contains Silica in the form of SiO2, Calcium in the form
CaO,magnicium in the form of MgO, aluminium, iron, Mn, potassium as K2O, sodium
as Na2O, potassium as P2O5 and Sulphur as SO4. [22]

DYE DEGRADATION:
Dye degradation is done by Rhodamine B which is chemical compound and also a dye.
To determine the rate and flow of water. It is often used as a tracer dye. Rhodamine B
dyes are fluoresce and it can be easily detected using fluorometer. It is widely used in
application such as fluorescence microscopy, ELISA, flow cytometry and fluorescence
correlation spectroscopy.[23]

RHODAMINE B STRUCTURE[24]
IUPAC NAME: [9-(2-carboxyphenyl)-6-diethylamino-3-xanthenylidene]-
diethylammonium chloride.

Other names:

Rhodamine 610, C.I. Pigment Violet 1, Basic Violet 10, C.I. 45170

FIGURE 2:

Rhodamine

USES:[27]
Rhodamine is fused into the animal’s whiskers and tee. It is adaptable around
610nm when it sis used as a laser dye. As one of the most commonly used dyes,
Rhodamine B (RhB) is widely used in industrial purposes, such as printing and dyeing
in textile, paper, paints, leathers etc. However, the organic dyes will cause serious
environmental and biological problems, even capable to induce irritation to the skin,
eyes. Thus, the removal of dye from water is a great challenge and a pressing task. The
convention methods for removal of RhB contains biochemical and physical-chemical
methods, such as liquid membrane, ozonation and adsorption, which are expensive and
not very effective. Based on Semiconductor heterogeneous photocatalysis,
photocatalysts present promising application for the organic dye decomposition with
superior activity.

CARBON:
Based on two facts, carbon is an Astonishing element “It is a basic element
which is used for all living purpose” and “It can occur in various allotropic forms[28].
Carbon is responsible for creating the most diverse variety of compounds. When
comparing to other element, it has more allotropes. The most recent additions to this list
are fullerenes and nanotubes. The sp2 hybridized state of carbon was 2-dimensional and
most studied of them is its allotrope carbon nanotubes and graphite. Special importance
is given to graphite and nanotubes. And they play important role in nanomaterilas,
including conductive and high-strength composites[29], nnanometrer-sized
semiconductor devices[30],probes[31], hydrogen storage media[32], interconnects[33],
energy conversion and storage devices[31], drug delivery[34], sensors[35], and
radiation sources[36]. The first person to detect and described CNTs was Radushkevish
and Lukyanovich in 1952.[37], the CNTs consist of a graphene layer which is rolled on
into a cylindrical shape. When the graphene was tube like and it is a single molecule.
Each single molecules is made up of a hexagonal network of covalently bonded carbon
atoms. In some cases, the hexagons are arranged In a spiral form. A graphene sheet can
be rolled more than one way by producing different types of carbon nanotubes[38]. It
can be characterised on the basis of their lengths, types of spiral, and finally number of
layers. They are Armchair, Zig-Zag and Chiral. Based on the number of layers carbon
nanotubes are classified into SWCNT and MWCNT. It has been shown that carbon
nanotubes exhibit strong adsorption affinities to a wide range of aromatic and aliphatic
contaminants in water, due to their large and hydrophobic surface areas. They also
showed similar adsorption capacities as activated carbons in the presence of natural
organic matter. As a result, they have been suggested as promising adsorbents for
removal of contaminant in water and wastewater treatment systems. Moreover,
membranes made out of carbon nanotube arrays have been suggested as switchable
molecular sieves, with sieving and permeation features that can be dynamically
activated/deactivated by either pore size distribution (passive control) or external
electrostatic fields (active control).
METHODS AND MATERIALS:

MATERIALS:
Rhodamine B, Ash (Rice husk ash), Carbon, FeCl 2 –IRON (II) CHOLRIDE
TETRAHYRATE. It is a product of Germany.

METHODS:
While burning the rice husk it gives ash, and it contains high amount of
crystalline silica. Producing activated RHA by low cost method for pozzolanic ash
suitable for masonry brides was patented in 1980.( IN 154,384 CL. C04B7/24),20
OCT,1984),Appl.80/DE397, 30 MAY 1980,10pp. Then ash was finely grained into
powder in Granite Mortar and pestle.

PREPARATION OF NANOPARTICLES:
Iron Nanoparticles are prepared by making use of Fecl2. About 100ml L-1 of iron
nanoparticles solution were prepared by dissolving an appropriate amount of FeCl2 in
distilled water.

Sodium hydroxide(NaOH) were used to adjust pH of the iron solution.

 After it attains pH 12 leave the solution for one complete day to settle down the
nanoparticles without disturbing the solution.

Finally the particles settle down at the bottom of the beaker which was known as
nanoparticles.

The clear solution is said to be a super natant. Then super natant was completely discard
and then nanoparticles were collected separately.

Nanoparticle

DRYING PROCESS:
The ash and carbon is mixed well with collected nanoparticles and distilled
water and kept in oven under 60 0C per day to dry it completely. The dried nanoparticles
are finally ready for characterisation.

DEGRADATION PROCESS:
 For various measurement of Rh B dye has taken in several test tubes.
Simultaneously by mixing ash and carbon separately into the tubes, and they allowing
to degrade under sunlight for a complete day. After degradation the settled particles in
those test tubes has taken and make them to dry. The dried nanoparticles are taken for
characterization.
CHARACTERIZATION:

UV–vis spectroscopy
To check the absorbance, the mixture was monitored by periodic sampling of aliquots
(2mL) of the aqueous component. The measurement was carried out on a Shimadzu dual-
beam spectrophotometer (model UV-1601 PC) operated at a resolution of 1 nm. The
measurements were performed in semimicro UV cuvettes (Brand GmbH) in the range 200-
700 nm.

FTIR ANALYSIS:
The FTIR spectra of the samples were recorded over the range 4000- 500 cm -1
on a Shimadzu FTIR-8400 spectrometer using the KBr pellet technique. Fourier
transform infrared (FTIR) spectrophotometer was used to analyze chemical bonds on
the surface of NP.

XRD ANALYSIS:
The mineralogical characteristics of RHAs were determined qualitatively by X-
ray diffraction (XRD). The technique analyzes the scattering pattern of an X-ray beam
striking through the sample. The pattern is caused by the constituent organized
structures of the material (crystals), and contributes important insights into the sample’s
crystalline morphology. The diffractograms were obtained using monochrome Cu Ka
radiation for ground samples.

SEM WITH EDAX ANALYSIS:

SEM is a type of device (electron microscope) that produce an image of the
sample by scanning the surface with a focused beam. The SEM image of Rice husk ash
was received with magnification. Scanning electron microscopy (SEM) is one of the
promising techniques for the morphology studies of the samples and gives important
information regarding the shape and size of the particles. Morphological characteristics
of the samples were analyzed by scanning electronic microscopy (SEM) to observe the
material’s topographic structure in a high-vacuum electron microscope (EVO MA15,
Zeiss) with secondary electron detectors.

The elemental analysis of prepared nanoparticles was performed using the

energy-dispersive X-ray (EDX) spectroscopy arranged on the SEM. In energy-
dispersive X-ray analysis (EDXA) the specimens were cast in resin along with a thin
slice of a quartz standard and polished down to 0.05 μm A1 203 before coating. An
accelerating potential of 15 kV was selected to give adequate penetration into both the
rice husk ash (15 μm) and the quartz standard (2.5 μm).

RESULTS AND DISCUSSION:

EDAX ANALYSIS

A quantitative analysis using EDXA was employed in this study to shed light on the
existing conflict in the literature localization of silica in the rice hull and Plant Burt Soot
carbon. An inherent problem in analyzing RHA quantitatively is the nonuniformity of
composition as well as the localization of silica preferentially within the outer epidermis.(S.
Yoshida et al,1975). Furthermore, the composition of the organic ash matrix is not uniform
throughout the process. There is a wide variation in the values reported for the major
constituents of the rice husk, Rice husk ash contains Silica in the form of SiO2, Calcium in
the form CaO,magnicium in the form of MgO, aluminium, iron, Mn, potassium as K2O,
sodium as Na2O, potassium as P2O5 and Sulphur as SO4. As indicated in EDAX mapping , a
rice husk ash can be regarded as consisting of SiO, imbedded in a matrix whose approximate
average composition is 51 wt% carbon, 7 wt% hydrogen, and 42 wt% oxygen.

SEM ANALYSIS:

The SEM image reveals that the rice husk ash still maintains its cellular
structure. After being ground, RHA consists of very irregular-shaped particles with porous
cellular surface. The SEM images of RHA showing their morphological characteristics of
roughness and porosity. (P. Chindaprasirt et al,2008)

The RHA nanoparticles have unifrom morphology with diameter less than 100 nm.
However, agglomeration of nanoparticles was occurred. The agglomeration may be due to
van der Waals attraction as suggested by M. J.Mayo,1996. Morphology of the nanopowder
after heated at 1000°C is shown in Fig.(a) The coarsening of crystallites on heating was
illustrated the particles which approach each other closer due to the increased van der Waals
force or presence of liquid phase within the granules. It can be seen from Fig.(b) that
although the individual particles were loosely aggregated into spherulites, the grain size of
SiO2 powder remains less than 100 nm. Concentration of trace elements in the SiO2
nanopowder are alumina, iron, calcium, sodium, potassium, manganese and phosphorus.
After heat treatments at 1000°C, the nanopowder presented the high silica of >95% purity.
(A. Ruksudjarit et al,2008)

Figure 6. SEM analysis of carbon FeNps, RHA, FenPs.

 Figure 7. EDAX analysis of Rice husk ash

UV-ANALYSIS:

Figure 8. UV analysis of Carbon materials

 The absorption peak at 300 nm is independent of the heating temperature, in
contrast to the shifts of the 220 nm absorption peak. Therefore, the origin of the
absorption is different. The origin of the absorption around 220 nm is attributed to the
graphitic structure of carbon.(Y.Kimura et al,2004)

FTIR ANALYSIS:

Figure 9. functional analysis of carbon, Carbon with iron nanoparticles and rice
husk ash

FTIR CARBON

Fourier transform infrared (FTIR) spectra were acquired to determine their surface
state. As shown in Fig.,In FTIR spectrum, peak at 3436 cm -1(m) is for O-H stretch, peak at
2146 cm-1 is for C-H stretch in alkane or in aromatic compounds. A very weak peak at 1630
is for C=C aromatic stretch. Peaks at 1465, 1383 and 1327 cm -1 are for C-H bend in CH 3 and
the peak at 1118 cm-1 is for C-O stretch. (Mohammad Abul Hossain et al,2013)

FTIR CARBON Fe
In the FTIR spectra two characteristic absorption peaks at 1629 cm -1 and 1384 cm-1
(X.Yang et al, 2018) are due to C=O vibrations. The IR bands at 539 and 448 cm −1 in sample
are characteristic of hematite and related to the band near 635 cm −1 in maghemite. (D.
Kostyukova, 2016)

FTIR ASH Fe
The FTIR spectra of the samples are shown in Fig. Peaks at 1214 cm −1 (shoulder) and
1070 cm−1 are assigned to Si asymmetrical stretching. The peak at 792 cm −1 is due to Si
symmetrical stretching bands for the rice husk ash, as observed earlier (Vempati et al., 2006).
The rice husk ash as a rich source of silica. The high silica content corroborates the
predominant silica phase observed in the XRD result.

According to the Flanigen–Khatami–Szymanski correlation, the vibrational modes

near 1100, 800 and 450 cm–1 (E.M. Flanigen,1971) are assigned to internal vibrations of Si
and are also observed in silica, quartz and cristobalite, while the vibra-tional modes near 550
and 1230 cm–1 are due to the double-rings tetrahedra vibration and to the asymmetric
stretching of Si, respectively. Besides those bands, the samples also show a small band at 620
cm–1, corresponding to the characteristic vibration of cristobalite.

XRD ANALYSIS OF CARBON BLENDED IRON OXIDE:

 Figure 10. XRD analysis of carbon and RHA with Iron nanoparticles blend

XRD fe203
The diffraction peaks at 2𝜃 = 33.1°, 35.6°, 40.8°, 49.4°, 54.0°, 57.5°, 62.4°, and
64.0°, indexed to the rhombohedral structure of hematite (𝛼-Fe2O3) with lattice constants 𝑎
= 5.0370Å, 𝑏 = 5.0370Å, and 𝑐 = 13.7710Å (reference code 01-089-0596). The phase
transformation occurred in sample calcined at 530° C. (D. Kostyukova, 2016)

XRD ash fe
The XRD pattern of RHA Figure indicates the presence of quartz (22.85 O, 26.63O and
42.47O 2θ peaks) and crysto-balite (21.91O, 35.99O and 69.50O 2θ peaks). Anorthite phase is
also found (27.91O and 29.42O 2θ peaks). It has been reported (Agarwal, 1989) that at low
temperature (873-973 K) silica in RHA is amorphous, and crystallization occurs when
temperature goes above 973 K (Agarwal, 1989). The presence of crystobalite phase indicates
that RHA is produced above 973 K. At high temperature, quartz is transformed to tridymite
(Metha et al., 1976) which is favored in presence of impurities in RHA (Metha and Pith
1974). As the peaks represent the synthesized RHA contains impurities in the sample. The
Portlandite peaks are encountered in the positions of 2θ-18.03°; 34.12°; 47.04°, 50.85°,
54.32°, 62.60° and 64.22°, which indicates the composition of mineral in the sample as
reported by L.W.O. Soares et al,2015

XRD carbon fe

The characteristic diffraction peaks at 2θ of 30.4°, 35.8°, 43.1°, 53.7°,56.9° and 63.1°
could be assigned to the (220), (311), (400), (422), (511) and (400) planes of SPION,
indicating that the nanoparticles had been formed successfully. The strong and narrow nature
of the peaks indicated that the well-crystallized detonation products with high purity were
obtained after cleaning and drying. The peaks at 43.1° & 63.1° can be attributed to the
corresponding 1 1 0 & 2 0 0 reflections of bcc-iron, according to the JCPDS No. 06-0696,
Obviously diffraction peak can be also seen at about 26.40°, this peak is assigned to the 0 0 2
reflection of the hexagonal graphite structure of carbon. (N. Luo et al,2010)

DYE DEGRADATION ANALYSIS:

UV absorbance measurement of Rhodamine B solution were noted at different

timing.The visible spectrum of Rhodamine B decreases slowly with time especially the
absorbance at 560 nm (λmax of RhB). The discoloration process is very slow when
compared to other dyes as reported in A. H. Mcheik et al,2013.The slow decrease in the
intense peaks of RhB at 560nm and 260nm is accompanied by the increase in
absorbance at 470nm and 370nm. Then the decrease continues in the whole spectrum,
which is shown in Fig. 11.

A typical SEM image of RHA is presented in Fig. 3. The SEM results reveal the
siliceous nature of the ash, which is also confirmed by the presence of quartz in the
XRD. Close examination of the SEM photomicrograph also suggests that RHA is
highly porous which is in agreement with others (Zhang and Malhotra 1996). The
porous nature of Rice Husk Ash is responsible for its high specific surface and makes it
suitable for making insulating brick.

The elemental composition analysis of synthesized Fe3O4 NPs was performed by the
energy-disperse X-ray spectroscopy (EDAX) method. The EDAX data of weight % of
as-synthesized Fe3O4 nanoparticles are; Fe: 50.51%, O: 43.93% and C: 5.57%. This
EDAX spectrum shows only Fe (iron) and O (oxygen) elements with 5.57% impurities
of calcium. EDAX graph indicated elemental signal for iron, which is specific for the
absorption of metallic iron nanocrystallites resulting from surface plasmon resonance.

The above EDAX spectrum of synthesized Fe3O4 nanoparticles. The EDAX data of
weight % of as-synthesized Fe3O4 nanoparticles are; Fe: 55.62% and O: 44.38%. The
EDAX spectrum shows only Fe (iron) and O (oxygen) elements without any impurities.
Hence, the EDAX analysis states that the as-synthesized Fe3O4 nanoparticles are in
perfect stoichiometry. From the morphology, it shows that the particles were
homogeneous, with sizes of approximately 5 nm with near cubic structure. The particle
size observed from FE-SEM image is comparable with the XRD crystallite size
calculations. The elemental analysis (Fig. 4.5b), confirms the presence of Ca, O and Fe
as similar to the Ferrous sulphate Heptahydrate chemical formula – FeSO4.7H2O.