Synthesis and Characterization of Copper Ferrite Nanoparticle

FINAL REPORT

Submitted in fulfillment of the requirements for the degree of

BACHELOR OF SCIENCE
in
[PHYSICS, CHEMISTRY, MATHEMATICS]

Submitted by

NANDANA B (R19PC032)
POSHITH L (R19PC035)
R. YASHWANTH (R19PC036)

Under the guidance of

Dr. Sathish Reddy

Professor, School of Applied Sciences (Chemistry)

REVA University
Rukmini Knowledge Park, Kattigenahalli, Yelahanka, Bangalore-560064
2021-22

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 Rukmini Knowledge Park, Kattigenahalli,
Yelahanka, Bangalore-560 064

 Name of the Candidates:

 Address and contact details, email ID:

 Name of the Guide:

 Address and contact details, email:

Students Registration No (SRN) : R19PC032, R19PC035, R19PC036

School : SCHOOL OF APPLIED SCIENCES

Title of the Proposal : Synthesis and characterization of copper ferrite

nanoparticle

Date: Date:

Signature of the Candidate’s Signature of Guide

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CONTENTS pages

1. Introduction………………………….……………………........4-25
1.1:Abstract
1.2:Introduction to Nanomaterials.
1.3:Methods of synthesis of Nanoparticles.
1.4:Introduction to Copper Ferrite Nanoparticle.
1.5:Introduction to spectroscopic methods.

2. Material and methods………………………………………...26-27

2.1:Chemical reagents.
2.2:Synthesis of Copper ferrites (CuFe2O4) nanoparticles.

3. Characterization………………………………………………28-34
3.1:UV-Visible spectra
3.2:FT-IR spectra
3.3:Scanning electron microscope (SEM)
3.4:Energy dispersive X-ray Analysis(EDAX)
3.5:Powder X-Ray diffraction study

4. Results and conclusion………………………………………. 35-35

5. References……………………………………………………. 35-37

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1.INTRODUCTION

1.1 Abstract

In this study, copper ferrite (CuFe2O4) nanoparticles were successfully

synthesized by the co-precipitation method. Crystalline structure, band gap, metal
oxides vibrational stretching, the elemental composition of the compound, and
size of the nano particles was studied by X-ray diffraction (XRD), UV-visible
spectrometer, FT-IR spectrometer, energy dispersive X-ray analysis (EDAX) and
scanning electron microscope (SEM) respectively.

1.2 Introduction to nanomaterials

A nanoparticle is a small particle that ranges between 1 to 100 nanometers
in size. Undetectable by the human eye, nanoparticles can exhibit significantly
different physical and chemical properties to their larger material counterparts.
The material properties change as their size approaches the atomic scale. This is
due to the surface area to volume ratio increasing, resulting in the material’s
surface atoms dominating the material performance. Owing to their very small
size, nanoparticles have a very large surface area to volume ratio when compared
to bulk material, such as powders, plates and sheets. This feature enables
nanoparticles to possess unexpected optical, physical and chemical properties, as
they are small enough to confine their electrons and produce quantum effects.[1]

For example, copper is considered a soft material, with bulk copper bend-
ing when its atoms cluster at the 50nm scale. Consequently, copper nanoparticles
smaller than 50nm are considered a very hard material, with drastically different
malleability and ductility performance when compared to bulk copper. The
change in size can also affect the melting characteristics; gold nanoparticles melt

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at much lower temperatures (300 °C for 2.5 nm size) than bulk gold (1064 °C).
Moreover,

absorption of solar radiation is much higher in materials composed of nano-

particles than in thin films of continuous sheets of material.[1]

Nanoparticles occur widely in nature and are

objects of study in many sciences such
as chemistry, physics, geology and biology.
Being at the transition between bulk materials
and atomic or molecular structures, they often
exhibit phenomena that are not observed at either
scale. They are an important component
of atmospheric pollution, and key ingredients in many industrialized products
such as paints, plastics, metals, ceramics, and magnetic products. The production
of nanoparticles with specific properties is a branch of nanotechnology.

In general, the small size of nanoparticles leads to a lower concentration of point

defects compared to their bulk counterparts,[2] but they do support a variety
of dislocations that can be visualized using high-resolution electron microscopes.
[14]
 However, nanoparticles
exhibit different dislocation
mechanics, which, together
with their unique surface
structures (Fig.1), results in
mechanical properties that are
different from the bulk
material.[3][4][5]

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Fig.1 showing increase in surface area of nanoparticles.

1.2.1 Classifications of nanomaterials

The classification of nanomaterials mainly depends on the morphology and

their structure (Fig.2), they are classified into two major groups as consolidated
materials and nano dispersions. Consolidated nanomaterials are further classified
into several groups. The one-dimensional nano dispersive systems are termed
nanopowders and nanoparticles. Here the nanoparticles are further classified as
nanocrystals, nanoclusters, nanotubes, supermolecules, etc.

For the nanomaterials, the size is an important physical attribute. Nanomaterials

are often classified depending upon the number of their dimensions falls under
nanoscale. The nanomaterial whose all the three dimensions are of nanoscale and
the is significantly no difference between the longest and shortest axes, are called
nanoparticles. Materials with their two dimensions in the nanoscale are called
nanofibers. Hollow nanofibers are known as nanotubes and the solid ones are
known as nanorods. Materials with one dimension in the nanoscale are known as
nanoplates. nanoplates with two different longer dimensions are known as nanor-
ibbons.

Based on the phases of matter contained by the nanostructured materials they are
classified as nanocomposite, nanofoam, nanoporous and nanocrystalline materi-
als. Solid materials containing at least one physically or chemically distinct re-
gion with at least one region with dimensions in the nanoscale are called nano
Composites. Nanofoams contain a liquid or solid matrix, filled with a gaseous
phase and one of the two phases has dimensions in the nanoscale. Solid materials

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with nanopores, cavities with dimensions on the nanoscale are considered as

nanoporous materials. nanocrystalline materials have crystal grains in the

nanoscale.[6]

Fig.2 showing different types of nanomaterials.

Accordingly, in zero-dimensional (0D) nanomaterials all the dimensions are

measured within the nanoscale (no dimensions are larger than 100 nm). Most
commonly, 0D nanomaterials are nanoparticles (Fig.3).
In one-dimensional nanomaterials (1D), one dimension is outside the nanoscale.
This class includes nanotubes, nanorods, and nanowires(Fig.3).
In two-dimensional nanomaterials (2D), two dimensions are outside the nano-
scale. This class exhibits plate-like shapes and includes graphene, nanofilms, nan-
olayers, and nanocoatings (Fig.3).
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Three-dimensional nanomaterials (3D) are materials that are not confined to the
nanoscale in any dimension. This class can contain bulk powders, dispersions of
nanoparticles, bundles of nanowires, graphite’s and nanotubes as well as
multi-nanolayers (Fig.3)..[7]

Fig.3 showing examples of OD,1D,2D,3D nanomaterials

The chart below shows the distribution of nanomaterial dimensionality in com-

mercialized products. Data show that 3D nanomaterials are the most abundant
(85% of all materials), in particular nanoparticles, which are currently present in
78% of all nanoproducts.[7]

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1.3 Methods of synthesis of nanoparticles

1.3.1 Top-down approach

The top-down approach uses initial macroscopic structures. The methods

begin with larger particles which are reduced to nanoparticles after a sequence of
operations performed over them (Fig.4). Main shortcomings of these methods are
that they involve large installations and hug capital is required for set up. The
methods are quite expensive and not suitable for large-scale production. The
method is suitable for laboratory experimentation. The approach is based upon
the grinding of materials. These methods are not suitable for soft samples.[8]

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Methods in top-down approach:
1. Physical vapour deposition.

2. Chemical vapour deposition

3. Ion implantation

4. Electron beam lithography

5. X-ray lithography.[9]

Fig.4 showing process involved in top-

down approach

1.3.2 Bottom-up approach

Bottom-up approaches of production of nanomaterials comprise the mini-

aturization of materials constituents to the atomic level with the additional pro-
cedure leading to the development of
nanostructures. Throughout the further
progression, the physical forces work-
ing at nanoscale combined simple units
into larger stable structures. The meth-
odology is principally based on the prin-
ciple of molecular recognition (self-as-
sembly). Self-assembly means growing

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more things about one's kind from themselves (Fig.5). Many of these techniques
are still under development or are just beginning to be used for the commercial
production of nanoparticles.[8]

Methods in a bottom-up approach:

1. Sol-gel synthesis

2. Co-precipitation method

3. Hydrothermal synthesis

4. Organometallic chemical route

5. Electrodeposition.

Fig.5 showing process involved in bottom-up approach

Fig.6 schematic representation of top-down and bottom-up process

1.3.3 Coprecipitation method:

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 It is one of the method under bottom-up approach which we have used to
prepare nanomaterial. The main aim in coprecipitation is to prepare
multicomponent materials through the formation of intermediate precipitates,
usually hydrous oxides or oxalates, so that an intimate mixture of components is
formed during precipitation and chemical homogeneity is maintained
on calcination. In the typical process of coprecipitation, aqueous metal salts are
mixed at sufficient temperatures with a base, which acts as a precipitating agent.
This method is widely employed for synthesis of nanoparticles (Fig.7).

Fig.7 showing process involved in coprecipitation method.

Advantages:
 High productive
 Low cost
 No need to use any organic
solvents
 Less time consuming

1.4 Introduction to Copper

Ferrite Nanoparticle.
Copper ferrite (CuFe2O4)
nanoparticles are one of the most
considerable or promising metal-
oxide nanomaterials due to their
novel magnetic properties.[10] Hence, they were used successfully in a various
application like photocatalyst, ferrofluids technology, high-energy density
magnetic recording[11],magnetic imaging[12], biomedical drug delivery systems,

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biosensors, data storage[13], magneto-optical devices[14], gas sensors and other
magnetic applications.

In general ferrites have chemical formula of MFe 2O4 (M= Mn, Fe, Co, Ni, Cu
etc.) have outstanding electrical ,optical, catalytic and magnetic properties [11].
Typically, copper ferrite (CuFe2O4) is an important effective material like other
spinel ferrites.

 IUPAC Name: copper;oxido(oxo)iron

 Structure:

 Molecular Formula: CuFe2O4

 Molecular weight: 239.23g/mol
 Colour: Black, brown and grey in
reflected light

Fig.8 cubic structure of copper ferrite NPs.

[Copper ions only occupies octahedral sites in the structure and iron ions are split
between the octahedral and tetrahedral sites in the structure,[15][16] as shown in
fig(8).Cuprospinel (Copper ferrite) adopts both cubic and tetragonal phase at
room temperature.][15][16]

The synthesis conditions and preparative methods of ferrite nanoparticles

plays a vital role. Copper ferrite nanoparticles have been synthesized through
various bottom-up approach techniques such as reverse micelle,
chemical co-precipitation, microemulsion and sol-gel methods. On comparing

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with conventional synthesis methods, chemical coprecipitation method has more
advantages and it is very simpler technique by avoiding usages of large
experimental setup with instruments. Consequently, these studies exhibit that, in
the copper ferrite synthesis, the morphology, phase and size composition of the
obtained product completely depends on the basis of synthesis condition and
preparative method. which often failed to provide the desired result.

In the present work, Copper ferrite (CuFe2O4) nanoparticle was successfully

synthesized by co-precipitation method and the prepared CuFe 2O4 is
characterized using several spectroscopic techniques such as UV-Vis
spectroscopy, IR spectroscopy, SEM, EDAX and X-Ray diffraction.

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1.5 Introduction to spectroscopic methods

1.5.1 UV-Visible Spectroscopy

1.5.1.1 Introduction to UV-Visible spectroscopy

UV spectroscopy is type of absorption spectroscopy in which light of ultra-

violet region (200-400 nm.) is absorbed by the molecule. Absorption of the ultra-
violet radiations results in the excitation of the electrons from the ground state to
higher energy state. The energy of the ultra-violet radiation that are absorbed is
equal to the energy difference between the ground state and higher energy states
( ΔE=hϑ ).
Generally, the most favoured transition is from the highest occupied molecular
orbital (HOMO) to lowest unoccupied molecular orbital (LUMO). For most of
the molecules, the lowest energy occupied molecular orbitals are s orbital, which
correspond to sigma bonds. The p orbitals are at somewhat higher energy levels,
the orbitals (nonbonding orbitals) with unshared paired of electrons lie at higher
energy levels.

The unoccupied or antibonding orbitals (pie * and sigma*) are the highest energy
occupied orbitals. In all the compounds (other than alkanes), the electrons un-
dergo various transitions. Some of the important transitions with increasing ener-
gies are: nonbonding to pie*, nonbonding to sigma*, pie to pie*, sigma to pie* and
sigma to sigma*.[17]

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1.5.1.2 Principle of UV-Visible spectroscopy

UV spectroscopy obeys the Beer-Lambert law, which states that: when a

beam of monochromatic light is passed through a solution of an absorbing sub-
stance, the rate of decrease of intensity of radiation with thickness of the absorb-
ing solution is proportional to the incident radiation as well as the concentration
of the solution.
The expression of Beer-Lambert law is-
A = log (I0/I) = Ecl
Where, A = absorbance
I0 = intensity of light incident upon sample cell
I = intensity of light leaving sample cell
C = molar concentration of solute
L = length of sample cell (cm.)
E = molar absorptivity
From the Beer-Lambert law it is clear that greater the number of molecules
capable of absorbing light of a given wavelength, the greater the extent of light
absorption. This is the basic principle of UV spectroscopy (Fig.9).

1.5.1.3 Instrumentation and working of UV-Visible spectroscopy

Fig.9 showing process involved in UV-Visible spectroscopy.

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Light Source- Tungsten filament lamps and Hydrogen-Deuterium lamps are
most widely used and suitable light source as they cover the whole UV region.
Tungsten filament lamps are rich in red radiations; more specifically they emit
the radiations of 375 nm, while the intensity of Hydrogen-Deuterium lamps falls
below 375 nm.
Monochromator- Monochromators generally composed of prisms and slits. The
most of the spectrophotometers are double beam spectrophotometers. The radia-
tion emitted from the primary source is dispersed with the help of rotating prisms.
The various wavelengths of the light source which are separated by the prism are
then selected by the slits such the rotation of the prism results in a series of con-
tinuously increasing wavelength to pass through the slits for recording purpose.
The beam selected by the slit is monochromatic and further divided into two
beams with the help of another prism.
Sample and reference cells- One of the two divided beams is passed through the
sample solution and second beam is passé through the reference solution. Both
sample and reference solution are contained in the cells. These cells are made of
either silica or quartz. Glass can't be used for the cells as it also absorbs light in
the UV region.
Detector- Generally two photocells serve the purpose of detector in UV spec-
troscopy. One of the photocell receives the beam from sample cell and second de-
tector receives the beam from the reference. The intensity of the radiation from
the reference cell is stronger than the beam of sample cell. This results in the gen-
eration of pulsating or alternating currents in the photocells.
Amplifier- The alternating current generated in the photocells is transferred to
the amplifier. The amplifier is coupled to a small servometer. Generally current
generated in the photocells is of very low intensity, the main purpose of amplifier
is to amplify the signals many times so we can get clear and recordable signals.[17]

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1.5.2 FT-IR spectroscopy
1.5.2.1 Introduction
IR spectroscopy (which is short for infrared spectroscopy) deals with the
infrared region of the electromagnetic spectrum, i.e., light having a longer
wavelength and a lower frequency than visible light. Infrared Spectroscopy
generally refers to the analysis of the interaction of a molecule with infrared light.

The IR spectroscopy concept can generally be analysed in three ways: by

measuring reflection, emission, and absorption. The major use of infrared
spectroscopy is to determine the functional groups of molecules, relevant to both
organic and inorganic chemistry.

1.5.2.2 Principle of infrared spectroscopy

The IR spectroscopy theory utilizes the concept that molecules tend to

absorb specific frequencies of light that are characteristic of the corresponding
structure of the molecules. The energies are reliant on the shape of the molecular
surfaces, the associated vibronic coupling, and the mass corresponding to the
atoms.

For instance, the molecule can absorb the energy contained in the incident light
and the result is a faster rotation or a more pronounced vibration.[18]

1.5.2.3 IR spectroscopy instrumentation

The instrumentation of infrared spectroscopy is illustrated below (Fig.10).

First, a beam of IR light from the source is split into two and passed through the
reference and the sample respectively.

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Now, both of these beams are reflected to pass through a splitter and then through
a detector. Finally, the required reading is printed out after the processor
deciphers the data passed through the detector.[18]

Fig.10 showing process involved in IR spectroscopy.

1.5.3 Scanning electron microscope (SEM)

1.5.3.1 Introduction

A scanning electron microscope (SEM) is a type of electron micro-

scope that produces images of a sample by scanning the surface with a focused
beam of electrons. The electrons interact with atoms in the sample, producing
various signals that contain information about the surface topography and compo-
sition of the sample. The electron beam is scanned in a raster scan pattern, and
the position of the beam is combined with the intensity of the detected signal to
produce an image. In the most common SEM mode, secondary electrons emitted
by atoms excited by the electron beam are detected using a secondary electron

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detector (Everhart–Thornley detector) (Fig.11). The number of secondary elec-
trons that can be detected and thus the

signal intensity, depends, among other things, on specimen topography. Some

SEMs can achieve resolutions better than1 nanometer.

Fig.11 showing ejection of secondary electrons due to incident beam(electron).

1.5.3.2 Working of SEM

The main SEM components include:

a) Source of electrons
b) Column down which electrons travel with electromagnetic lenses
c) Electron detector
d) Sample chamber
e) Computer and display to view the images
Electrons are produced at the top of the column, accelerated down, and passed
through a combination of lenses and apertures to produce a focused beam of
electrons which then strikes the surface of the sample. The sample itself is
mounted on a stage in the chamber area and (unless the microscope is designed to
operate at low vacuums) both the column and the chamber are evacuated by a

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combination of pumps. The level of the vacuum will depend on the design of the
microscope.[19]

The position of the electron beam on the sample is controlled by scan coils
situated above the objective lens. These coils allow the beam to be scanned over
the surface of the sample. This beam rastering or scanning enables information
about a defined area on the sample to be collected. As a result of the electron-
sample interaction, a number of signals are produced. These signals are then
detected by appropriate detectors.

1.5.4 Energy dispersive analysis of X-rays(EDAX)

1.5.4.1 Introduction
Energy-dispersive X-ray spectroscopy (Fig.12) (also known as EDS, EDX,
or EDXA) is a powerful technique that enables the user to analyse the elemental
composition of a desired sample. The major operating principle that allows EDS
to function is the capacity of high energy electromagnetic radiation (X-rays) to
eject 'core' electrons (electrons that are not in the outermost shell) from an atom.
This principle is known as Moseley's Law, which determined that there was a
direct correlation between the frequency of light released and the atomic number
of the atom.

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 Fig.12 showing working of EDAX

Removing these electrons from the system will leave behind a hole that a higher
energy electron can fill in, and it will release energy as it relaxes. The energy re-
leased during this relaxation process is unique to each element on the periodic
table, and as such bombarding a sample with X-rays can be used to identify what
elements are present, as well as what proportion they are present in.[20]

Shown below in a fig(13) is an example of how EDS works. The letters K, L, and
M refer to the n value that electrons in that shell have (K electrons, closest to the
nucleus, are n=1 electrons), while α and β indicate the size of the transition. The
relaxation from M to L or L to K are therefore described as Lα or Kα, while go-
ing from M to K would be a Kβ transition. The means that are used for describing
these processes as a whole are known as Siegbahn notation.[21]

Fig.13 showing ejection of electron from k shell.

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1.5.4.2 Accuracy of EDAX

EDAX can be used to determine which chemical elements are present in a

sample and can be used to estimate their relative abundance. EDAX also helps to
measure multi-layer coating thickness of metallic coatings and analysis of various
alloys. The accuracy of this quantitative analysis of sample composition is
affected by various factors. Many elements will have overlapping X-ray emission
peaks (e.g., Ti Kβ and V Kα, Mn Kβ and Fe Kα). The accuracy of the measured
composition is also affected by the nature of the sample. X-rays are generated by
any atom in the sample that is sufficiently excited by the incoming beam. These
X-rays are emitted in all directions (isotropically), and so they may not all escape
the sample. The likelihood of an X-ray escaping the specimen, and thus being
available to detect and measure, depends on the energy of the X-ray and the
composition, amount, and density of material it has to pass through to reach the
detector. Because of this X-ray absorption effect and similar effects, accurate
estimation of the sample composition from the measured X-ray emission
spectrum requires the application of quantitative correction procedures, which are
sometimes referred to as matrix corrections.[21]

1.5.4.3 Advantages of EDAX

 Detection of all the elements
 Isotope sensitivity
 High speed data collection


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1.5.5 Powder X-Ray diffraction study
1.5.5.1 Introduction
X-ray powder diffraction (XRD) is a rapid analytical technique primarily
used for phase identification of a crystalline material and can provide information
on unit cell dimensions. The analyzed material is finely ground, homogenized,
and average bulk composition is determined.

1.5.5.2 Fundamental principles of X-ray powder diffraction (XRD)

X-ray diffraction is based on constructive interference of monochromatic X-rays

and a crystalline sample. These X-rays are generated by a cathode ray tube,
filtered to produce monochromatic radiation, collimated to concentrate, and
directed toward the sample. The interaction of the incident rays with the sample
produces constructive interference (and a diffracted ray) when conditions
satisfy Bragg's Law (nλ=2d sin θ).[22] This law relates the wavelength of
electromagnetic radiation to the diffraction angle and the lattice spacing in a
crystalline sample. These diffracted X-rays are then detected, processed and

counted (Fig.14).

Fig.14 showing diffracted x rays and Bragg’s law equation

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By scanning the sample through a range of 2θangles, all possible diffraction
directions of the lattice should be attained due to the random orientation of the
powdered material. Conversion of the diffraction peaks to d-spacings allows
identification of the mineral because each mineral has a set of unique d-spacings.
Typically, this is achieved by comparison of d-spacings with standard reference
patterns.

All diffraction methods are based on generation of X-rays in an X-ray tube. These
X-rays are directed at the sample, and the diffracted rays are collected. A key
component of all diffraction is the angle between the incident and diffracted rays.
Powder and single crystal diffraction vary in instrumentation beyond this.

1.5.5.3 Instrumentation and working of XRD

X-rays are generated in a cathode ray tube by heating a filament to produce
electrons, accelerating the electrons toward a target by applying a voltage, and
bombarding the target material with electrons. When electrons have sufficient en-
ergy to dislodge inner shell electrons of the target material, characteristic X-ray
spectra are produced. These spectra consist of several components, the most
common being Kα and Kβ. Kα consists, in part, of Kα1 and Kα2. Kα1 has a slightly
shorter wavelength and twice the in-
tensity as Kα2. The specific wave-
lengths are characteristic of the tar-
get material (Cu, Fe, Mo, Cr). Filter-
ing, by foils or crystal monochrome-

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ters, is required to produce monochromatic X-rays needed for diffraction
(Fig.15).
Fig.15 showing working of XRD

Kα1and Kα2 are sufficiently close in wavelength such that a weighted aver-

age of the two is used. Copper is the most common target material for single-
crystal diffraction, with CuKα radiation = 1.5418Å. These X-rays are collimated
and directed onto the sample. As the sample and detector are rotated, the intensity
of the reflected X-rays is recorded. When the geometry of the incident X-rays im-
pinging the sample satisfies the Bragg Equation, constructive interference occurs
and a peak in intensity occurs. A detector records and processes this X-ray signal
and converts the signal to a count rate which is then output to a device such as a
printer or computer monitor.
The geometry of an X-ray diffractometer is such that the sample rotates in the
path of the collimated X-ray beam at an angle θ while the X-ray detector is
mounted on an arm to collect the diffracted X-rays and rotates at an angle of 2θ.
The instrument used to maintain the angle and rotate the sample is termed
a goniometer. For typical powder patterns, data is collected at 2θ from ~5° to 70°,
angles that are present in the X-ray scan.[22]

1.5.5.4 advantages of XRD

 It is a rapid and powerful technique for identifying unknown minerals and

materials.
 It only requires preparation of a minimal sample for analysis.
 Interpreting the resulting data is relatively straightforward.
 XRD measurement instruments are widely available.
 Identification of fine-grained minerals such as clays and mixed layer
clays that are difficult to determine optically
 Determination of unit cell dimensions
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 Measurement of sample purity

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2. Material and methods

2.1 Chemical reagents

Laboratories ltd. Deionized (DI) water were used throughout the

experiment for experimental part, Iron (III)chloride (FeCl3,97.0%), copper
(II)sulphate (CuSO4,99.0%) and sodium hydroxide (NaOH,97.0%) were
purchased from SDFCL (s d fine-chem limited), Acetone (CH3COCH3, 99.9%)
was purchased from changshu hongsheng fine chemicals co. ltd.

2.2 Synthesis of Copper ferrites (CuFe2O4) nanoparticles

Copper ferrite nanoparticle was synthesised by co-precipitation method. In
a typical experiment, 25ml of 0.4M FeCl 3 and 25ml of 0.2M CuSO4 are taken in a
beaker and then they were dissolved by continuous magnetic stirring. In continu-
ous magnetic stirring two solutions were mixed until a homogenous solution is
formed. Then 25ml of 1.5 M NaOH was added drop by drop to the above mix-
ture. The colour of the solution changes and precipitate formation takes place.
The obtained precipitate is filtered, dried and calcined at 600 oC for 3hours to get
well crystallized copper ferrite. Then the obtained precipitate was washed with
acetone to make free of impurities and dried in a hot air oven at 50 o C. finally
grained to get a fine powder CuFe2O4 using agate motor (Fig.16).

Fig16. Schematic representation of the experimental procedure:

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Reactions:

Change in color is due to the formation of metal hydroxides (CuFe2(OH)8).

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3. Characterization

 The synthesised copper ferrite nanoparticle was characterized by X-ray dif-

fraction (XRD), UV-visible spectrometer, FT-IR spectrometer, Energy dis-
persive X-ray analysis (EDAX) and Scanning electron microscope (SEM).
 The UV-Visible absorption spectra of the copper ferrite nano particle were
performed using Evolution 201 UV-Visible spectrophotometer.
 SEM and EDAX measurement were conducted by Tescan Vega 3 operat-
ing at 30kv.
 XRD analysis was carried out by using Panalytical X’Pert 3 powder system
operating at 30kv and 40mA.

3.1 UV-Visible spectra of copper ferrite(CuFe2O4) NPs:

The copper ferrite nano particle was characterized by UV–visible
absorption spectroscopy. The UV–visible absorption spectra of the
prepared CuFe2O4 NPs dispersed in ethanol solution and scanned in the
wavelength between 200–800nm range, shows the maximum absorbance
at 402nm (fig17(A)) and we found the energy band gap of CuFe 2O4 at 3.06eV
(fig17(B)).

Fig.17 (A) UV-Visible spectra for CuFe2O4 and (B) Energy band gap calculated
graph for CuFe2O4.
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3.1.1 Band gap calculation:

Using the formula Ebg = hc/λ where,

h = Planck’s constant
c = velocity of light
λ = wavelength
the obtained value i.e., Ebg=3.09ev was
evident when compared to the previously
reported work [23] using same formula.

3.2 FT-IR spectra of copper ferrite(CuFe2O4) NPs:

The FTIR spectra was recorded for the CuFe 2O4 NPs shows absorption
band at approximately 410-580 cm-1. Absorption band at 462 cm-1 indicates the
(Cu-O) copper oxide Vibrational stretching and absorption band at 572 cm -1
indicates the Vibrational stretching of (Fe-O) iron oxide (fig(18)). These
connections prove the bond formation between copper and oxygen and iron and
oxygen respectively. Which was found to be evident When compared to the
reference[24]. In fact, functional group [OH] was not recorded at 3500cm -1 which
was present in reference[24] indicating the purity of compound prepared.
Therefore, the copper ferrite (CuFe2O4) nano particle has been successfully
synthesised by using co-precipitation method.

Page | 32
 Fig.18 IR spectra for CuFe2O4

3.3 SEM image of copper ferrite(CuFe2O4) NPs:

Page | 33
 Fig.19(A) SEM images of CuFe2O4 NPs

Fig.19(B) SEM images of CuFe2O4 NPs

Scanning electron microscopic observation of the CuFe2O4 nanoparticles show

that particle size is less than 100nm (Fig.19 (A) & (B)). This value is in
accordance with that obtained from Xrd measurement. SEM images show
particles are like a cube shaped and distributed uniformly.

3.4 EDAX of copper ferrite nano particle(CuFe2O4)

Page | 34
 Fig.20 (A) graph showing elemental composition of CuFe2O4

Figure.20, shows the EDAX analysis and provides information about

elemental composition of CuFe2O4. It confirms the presence of all the three
elements like copper, iron and oxygen in the ratio 6.22%, 31.76%, 62.02%
respectively. Fig 20(B) slected area in SEM image and Fig 20 (C) shows the
percentage of metals.

eZAF Smart Quant Results

Element Weight % Atomic %

OK 31.39 62.02

FeK 56.11 31.76

CuK 12.50 6.22

Fig.20(B) Is elemental composition of CuFe2O4 NPs calculated area and 20(C) is

the table containing elemental composition of different elements present in
CuFe2O4 NPs.

3.5 X-Ray diffraction study of copper ferrite(CuFe2O4) NPs

CuFe2O4 calcinated at 600oC show to have XRD peaks at

2ϴ=33.155, 35.645, 40.865, 43.975, 49.535, 54.185, 62.465, 64.055 [25][26]

which are in accordance to crystal planes of the CuFe 2O4 NPs and indexed to
(220), (311), (222), (400), (331),(422), (511), (531), and (442),
respectively, other low intensity peaks are also observed (fig(21)). All peaks,

Page | 35
including high and low intensity peaks are in agreement with standard JCPDS file
no.34-0425[26].

The average crystallite size is estimated to be 70.7nm calculated using Debye-

Scherrer's formula. The sharp peaks suggest that copper ferrite nano particles are
good crystallized.

Fig.21 XRD pattern of copper ferrite CuFe2O4 NPS

0.9 λ
Debye-Scherrer formula : D= β cos θ where,

D=the average crystallize size

ϴ=angle of diffraction

k=Scherrer constant(0.9)

Page | 36
 λ = wavelength of x-ray used (0.154nm)

β=Full width at half maximum ¿ ) In terms of radians.

3.5.1 Table showing size of the nanomaterial:

6

Page | 37
4. Results and conclusion

In this study the copper ferrite (CuFe 2O4) nanoparticles were synthesized
successfully by coprecipitation method. Synthesized CuFe 2O4 nanoparticles were
characterized by UV-Visible spectra, FT-IR spectra, SEM, EDAX, and XRD. All
the obtained spectra were in agreement with the previously published paper. This
indicate copper ferrite (CuFe2O4) is highly pure compound. Prepared CuFe 2O4
nanoparticles shows blue shift (402 nm) and increased energy band gap (3.06 eV)
as compared with bulk CuFe2O4. SEM results show that particle having cube
shaped with less 100 nm size. XRD results exhibits that particle are crystalline in
nature and average crystalline size is found to be 70 nm with face centered cubic
structure. Prepared copper ferrite NPs are of more interest because of their vari-
ous applications. This method is useful for commercial production of copper fer-
rites in industrial scale.

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