SYNTHESIS AND OPTICAL CHARACTERIZATION OF VANADIUM

CHROMIUM OXIDE (V2CrO7), COPPER CHROMIUM OXIDE

(CuCrO2), BARIUM CHROMATE (BaCrO4), IRON CHROMITE
(FeCr2O4) NANOPARTICLES AS A P-TYPE SEMICONDUCTOR BY
SOL-GEL METHOD

Submitted By
SANA EMAAN (SAP ID: 22654)
HUDA FATIMA (SAP ID: 23661)
Supervised By
Dr. Nasir Mehboob

Project report submitted in the partial fulfilment of the requirements

for the degree of
BACHELOR OF SCIENCE IN
PHYSICS
DEPARTMENT OF PHYSICS
FACULTY OF ENGINEERING AND APPLIED SCIENCES
RIPHAH INTERNATIONAL UNIVERSITY ISLAMABAD, PAKISTAN,
June, 2024
 APPROVAL SHEET SUBMISSION OF HIGHER RESEARCH DEGREE
DISSERTATION/THESIS

The following statement is to be signed by the candidate’s supervisor (s), Dean/ HOD and must
be received by the Controller of Examination, before the dispatch of the dissertation to the
approved examiners.

Candidate’s Name: Sana Emaan, Huda Fatima

SAP ID: 22654, 23661
Program Title: Bachelor of Science in Physics
Department/ Faculty: Physics
Dissertation Title: SYNTHESIS AND OPTICAL CHARACTERIZATION OF
VANADIUM CHROMIUM OXIDE (V2CrO7), COPPER
CHROMIUM OXIDE (CuCrO2), BARIUM CHROMATE
(BaCrO4), IRON CHROMITE (FeCr2O4) NANOPARTICLES
AS A P-TYPE SEMICONDUCTOR BY SOL-GEL
METHOD

I hereby certify that the above candidate’s work, including the Dissertation/thesis, has been
completed to my satisfaction and that the Dissertation/thesis is in a format and of an editorial
standard recognized by the department/faculty as appropriate for examination. The
Dissertation/thesis has been checked through Turn it in for plagiarism (test report attached).

Signature (s):
Supervisor:
Date:

The undersigned certifies

1.The candidate presented at a pre-completion seminar, an overview and synthesis of major
findings of the Dissertation/thesis, and that the research is of a standard and extent appropriate
for submission as a Dissertation/thesis.
2.I have checked the candidate’s Dissertation/thesis and its scope, format, and editorial
standards are recognized by the department/faculty as appropriate.
3.The plagiarism check has been performed. Report is attached

Signature (s):
Head of Department:
Dean of Faculty:
 Declaration

I SANA EMAAN and HUDA FATIMA certify that the research work presented in this
dissertation/thesis is to the best of my knowledge. All sources used and any help received in the
preparation of this dissertation/thesis have been acknowledged. I hereby declare that I have not
submitted this material, either in whole or in part, for any other degree at this or any other
institution.

Signature: ______________
Name: SANA EMAAN
Signature: ______________
Name: HUDA FATIMA
 ACCEPTANCE CERTIFICATE
SYNTHESIS AND OPTICAL CHARACTERIZATION OF VANADIUM
CHROMIUM OXIDE (V2CrO7), COPPER CHROMIUM OXIDE (CuCrO2),
BARIUM CHROMATE (BaCrO4), IRON CHROMITE (FeCr2O4)
NANOPARTICLES AS A P-TYPE SEMI-CONDUCTOR BY SOL-GEL
METHOD

By
SANA EMAAN
&
HUDA FATIMA
A dissertation submitted in partial fulfilment of the requirements for the degree of Master
of Philosophy in Physics.
We accept this dissertation as conforming to the required standard.

Examination Committee:

______________________ _____________________
Supervisor Internal Examiner
Dr. Nasir Mehboob Dr. Farooq Nasir
Assistant Professor Head, Department of Physics
Department of Physics Department of Physics
Riphah International University Riphah International University
Islamabad Islamabad

_____________________ ___________________
Dr. Irfan Qasim Prof. Dr. Jameel Ahmed
Riphah International University Dean, Faculty of Engineering and Applied
Islamabad Sciences
Riphah International University
Islamabad

DEPARTMENT OF PHYSICS
RIPHAH INTERNATIONAL UNIVERSITY,
ISLAMABAD, PAKISTAN,
June, 2024
 Acknowledgements

All gratitude and praises to Almighty ALLAH, the most benevolent, gracious, beneficent,
merciful and compassionate who blessed me with health, thoughts, and abilities and capacitate
me to achieve this goal. After Almighty ALLAH, praises are due his Prophet Muhammad (Peace
be upon him), the most glorious, who is forever a source of guidance and knowledge for the
whole of mankind and enabled us to identify our creator.
I am highly grateful to express my sincere admiration, heartiest gratitude and a deep sense of
obligation to my honorable supervisor Dr Nasir Mehboob for his sensible command, sympathetic
attitude, moral support and priceless suggestions. His kind help, bottomless inspiration,
generosity and perspective criticism enabled me to complete this work.
I have insufficient words to convey my sincere thankfulness to all my respected teachers and my
parents for their sincere cooperation during the completion of my research work. Their
contributions, endeavors, detailed comments and insight have been of great value to me.

SANA EMAAN HUDA FATIMA

 Abstract
This thesis presents the successful synthesis and detailed optical characterization of
Vanadium Chromium Oxide (V2CrO7), Copper Chromium Oxide (CuCrO2), Barium Chromate
(BaCrO4), and Iron Chromite (FeCr2O4) nanoparticles via the sol-gel method. Sol-gel method is
a versatile and cost-effective technique known for producing high-purity and homogeneous
materials. Following synthesis, a comprehensive suite of characterization techniques was
employed, including X-ray Diffraction (XRD), Ultraviolet-Visible (UV-Vis) spectroscopy and
Fourier Transform Infrared Spectroscopy (FTIR). The unique combination of structural, optical
and molecular properties identified in these chromium-based nanoparticles highlights their
potential for advanced technological applications. This study provides a foundation for further
research and development, innovations in energy conversion, environmental remediation, and
electronic devices.

Keywords: Semiconductors, Sol-gel Method, Doping, X-Ray Diffraction, UV-Vis

Spectroscopy, Fourier Transform Infrared Spectroscopy, Chromium Oxide.
Contents
1.1: NANOSCIENCE AND NANOTECHNOLOGY.........................................................................................1
1.2: NANOPARTICLES AND THEIR DIMENSIONS:......................................................................................2
1.2.1: Dimensions of nanoparticles:........................................................................................................3
1.3: SEMICONDUCTORS:..........................................................................................................................4
1.3.1. Types of Semi-Conductor:..........................................................................................................5
1.4. TRANSITION METALS IN NANO-MATERIALS:....................................................................................6
1.4.1: CHROMIUM OXIDE AND ITS PROPERTIES:.................................................................................7
1.4.2. DOPING:.....................................................................................................................................8
1.5. OXIDES:...........................................................................................................................................10
CHAPTER#02...........................................................................................................................................12
LITERATURE REVIEW..........................................................................................................................12
CHAPTER#03...........................................................................................................................................18
METHODOLOGY....................................................................................................................................18
3.1: SOL-GEL METHOD:..........................................................................................................................18
3.2: Stoichiometry and Calculation for sample:.....................................................................................19
3.3. STEPS FOR PREPARING SAMPLES:...................................................................................................22
3.3.1. Measuring Precursors:.............................................................................................................22
3.3.2. Stirring:....................................................................................................................................23
3.3.3. Heating and Drying:.................................................................................................................23
3.3.4. Crushing or Grinding:...............................................................................................................24
3.3.5.Storing:.....................................................................................................................................24
3.3.6 Sintering of sample:..................................................................................................................25
CHAPTER#04...........................................................................................................................................26
CHARACTRISATION TECHNIQUES....................................................................................................26
4.1. XRD (X-RAY DIFFRACTION):.............................................................................................................26
4.1.1. WORKING PRINCIPLE:..................................................................................................................27
4.2. UV-Vis SPECTROSCOPY:.................................................................................................................28
4.3.1. WORKING PRINCIPLE...............................................................................................................29
4.3. FTIR (Fourier Transform Infrared Spectroscopy):........................................................................31
4.4.1. FTIR operation:........................................................................................................................32
 4.4.2. Need for FTIR employment:.....................................................................................................33
CHAPTER 5..............................................................................................................................................34
RESULTS AND DISCUSSION....................................................................................................................34
5.1. Powder X-ray diffraction (XRD)...................................................................................................34
5.2. UV-Vis Spectroscopy...................................................................................................................37
5.3. FTIR Spectroscopy:......................................................................................................................39
CONCLUSION:........................................................................................................................................41

8
 CHAPTER#01
INTRODUCTION

1.1: NANOSCIENCE AND NANOTECHNOLOGY

The study of structures and chemicals at nanoscales, or between 1 and 100 nm, is known
as nanoscience, and the technology that applies this knowledge to real-world objects like gadgets
is known as nanotechnology [1].
Nanotechnology and nanoscience have emerged as critical fields for industrial and medical
applications, including drug delivery systems, imaging probes, and diagnostic biosensors, in a
matter of decades. For instance, nanoparticles have been used extensively in the food sector to
significantly improve nutrient output, packaging, shelf life, and bioavailability. A new generation
of hydrogen fuel cells, solar cells, and innovative hydrogen storage devices are being constructed
using nanomaterials to provide sustainable energy to nations that still rely on conventional, non-
renewable polluting fuels [2]
The science of nanotechnology is one that is growing quickly. Because of its interdisciplinary
nature, it benefits numerous branches of industry and science.

1
 FIGURE 1.PERCENTAGE SHARE OF NANOTECHNOLOGY IN VARIOUS FIELDS OF SCIENCE AND INDUSTRY

1.2: NANOPARTICLES AND THEIR

DIMENSIONS:
When compared to atoms and molecules, nanoparticles are incredibly small particles, often
measuring just a few nanometers. Because of their special qualities at such a small scale, they
may be manufactured from a variety of materials and are used in numerous industries, including
materials science, electronics, and medicine [3].
NPs have distinct physical and chemical properties due to their large surface area and nanoscale
size. Their reactivity, hardness, and other attributes are also determined by their particular size,
shape, and structure. Because of these qualities, they are ideal candidates for a wide range of
commercial and domestic applications, including catalysis, imaging, medicinal applications,
energy-based research, and environmental applications [4]

FIGURE 2.NANOPARTICLES

2
1.2.1: Dimensions of nanoparticles:

There is total four dimensions of nanoparticles.

 Zero-Dimension:

Zero-dimensional nanostructures are materials having all dimensions within the

nanoscale (no dimension is higher than 100 nm).
 One-Dimension:

Wires, rods, tubes, ribbons of metal/semimetals, oxides, sulfides, and halides are
examples of one-dimensional (1D) nanostructures, which have dimensions between 1 and
100 nm. Their morphologies, compositions, and structures vary greatly.
 Two-Dimension:

Two-dimensional nanomaterials (2D nanomaterials) are a sophisticated advanced class of

atomically thick nanomaterials made up of one to many layers of atoms. The lateral size
of 2D nanomaterials can exceed micrometers, and longer lengths can be achieved by
better synthesis processes.
 Three-Dimension:

A 3D material's dimensions are all more than 100 nm or outside the nanometer range, yet
the bulk material is built up of discrete nanoscale-scale blocks (1-100 nm), hence 3D
nanomaterials have three arbitrary dimensions above 100 nm.

3
 FIGURE 3.SCHEMATIC ILLUSTRATION OF ZERO-, ONE-, TWO-, AND THREE-DIMENSIONAL
NANOSTRUCTURED MATERIALS

1.3: SEMICONDUCTORS:

Materials with conductivity between non-conductors or insulators (like ceramics) and

conductors (usually metals) are known as semiconductors. Semiconductors can be pure materials
of silicon or germanium, or they can be compounds like gallium arsenide. The theories,
characteristics, and mathematical techniques pertaining to semiconductors are clarified by
physics.

FIGURE 4.BAND GAP

Germanium, silicon, and gallium arsenide are a few of the most widely utilized semiconductors.
Gallium arsenide is utilized in solar cells, laser diodes, and other devices, whereas silicon is

4
employed in the construction of electrical circuits. We are aware that an atom's electrons exist at
various energies. Each level of an atom has to split into N stages of the solid when we attempt to
create a structure made up of N atoms. Energy Bands are created when sharp, closely spaced
energy levels split apart. A band gap is the space between adjacent bands that indicate an
electron-free range of energies [5].

1.3.1. Types of Semi-Conductor:

There are two types of Semiconductors.

 Intrinsic Semi-conductor:

An intrinsic semiconductor, sometimes referred to as a pure semiconductor, is one in

which the quantity of charge carriers is determined by the characteristics of the material
and is not significantly affected by dopant species. If donors and acceptors are doped
equally, this can be sustained even after doping, permitting specific conductors to be both
external and internal [6]

 Extrinsic Semi-conductor:

Polluting an extrinsic semiconductor with a substance to give it differing electrical

characteristics from intrinsic semiconductors is known as extrinsic doping. Electric
current has charge carriers in the crystal lattice thanks to the foreign dopamine atoms.
Extrinsic semiconductors come in two varieties: p-type (an electrode receiver atoms),
which produce positive holes and electrons, and n-type (electrode donor elements), which
release negative electrons [7]

There are two types of extrinsic semi-conductor.

 P-Type semiconductor:

5
 Because positive holes make up nearly all of the charge carriers in the glass, an
extrinsic semiconductor that has been treated with accepting electrons atoms is referred to
as a p-type semiconductor.

 N-Type semiconductor:

An element that releases a mobile conducting electron into the crystal lattice upon
incorporation is known as an electron donor dopant. Since negative electrons make up the
majority of the charge carriers in the crystal, an external semiconductor doped with
donated electrons atoms is referred to as an n-type semiconductor.

FIGURE 5.SEMI-CONDUCTORS

1.4. TRANSITION METALS IN NANO-

MATERIALS:
Transition metals are significant in nanomaterials because of their distinct electrical,
magnetic, and optical properties. Nanomaterials are materials with at least one nanoscale
dimension, often ranging from 1 to 100 nanometers. Transition metals, which include iron,
copper, gold, silver, and titanium, have been employed in a wide range of nanomaterials,
including nanoparticles, nanowires, and nanotubes. Iron is a transition metal that is commonly
employed in nanomaterials.

6
Iron nanoparticles’ magnetic characteristics have made them useful in biological applications
such as medication delivery and imaging agents.
Copper is another transition metal used in nanomaterials, notably copper oxide nanoparticles,
which have antibacterial properties and are employed in a wide range of medical and industrial
applications. Gold and silver nanoparticles are also frequently utilized in nanomaterials due to
their optical capabilities, which include the capacity to absorb and scatter light. These qualities
make them helpful in a wide range of applications, including imaging and sensing. Titanium
dioxide is another transition metal extensively employed in nanomaterials, notably in the form of
nanotubes and nanowires, because of its great strength and electrical conductivity. Overall,
transition metals play an important role in the creation and implementation of nanomaterials, as
they have unique features that can be used in a variety of disciplines including health,
electronics, and energy.

FIGURE 6 TRANSITION METALS IN PERIODIC TABLE

1.4.1: CHROMIUM OXIDE AND ITS PROPERTIES:

7
Chromium oxide has the chemical formula CrO2, which means that it has one chromium (Cr)
atom for every two oxygen (O) atoms. It is also known as chromium (II) oxide to describe the
oxidation state of chromium, which are +2 in this molecule. Chromium oxide is often seen as a
green crystalline solid. It has a high melting point and is insoluble in water. Color variations in
chromium oxide might be green, black, or brown, depending on particle size and crystal
structure. [8]
Applications: Chromium oxide has many applications in various industries:

Pigment:

It is extensively used as a green pigment in paints, ceramics, and plastics due to its bright color
and chemical stability.
Abrasive:

Chromium oxide is used to polish and grind metals and ceramics.

Its high melting point and chemical inertness make it ideal for use as a refractory material in
furnace linings and ceramic crucibles.
Catalysis:

Chromium oxide is used as a catalyst in many chemical reactions, including oxidation and
hydrogenation, in industries such as petrochemicals and environmental remediation.
Magnetic properties:

While chromium oxide is not significantly magnetic, it does display modest antiferromagnetic
activity at low temperatures. This feature is of interest in the science of magnetism and could
have potential uses in Magnetic data storage.
1.4.2. DOPING:

Chromium Oxide doped with transition metal like Vanadium (V2CrO7), Barium (BaCrO3), Iron
(FeCr2O4) and Copper (CuCrO2). This is done by using SOL-GEL method.

a. Copper-doped with Chromium oxide(CuCrO2):

8
Copper chromium oxide materials are classified into a variety of classifications, each with its
own set of features and potential applications in science and technology. Copper-doped
chromium oxide materials may potentially display semiconductor properties, especially if the
doping affects the electronic band structure of CrO2. Depending on the concentration and
arrangement of dopants, these materials can exhibit variable electrical conductivity, bandgap
engineering, and charge carrier mobility.

Copper-doped chromium oxide materials may have use in spintronics, which uses electron spin
for information processing and storage. Depending on the magnetic and electrical properties
imparted by the dopants, these materials can be classed as suitable for spin injection, spin
transport, or magnetic tunneling junctions.
a. Barium-Doped with chromium oxide(BaCrO4):

Barium-doped with chromium oxide, abbreviated BaCrO3, is a perovskite oxide (Perovskites are
a class of functional materials defined by the ABX3 formula. In this formula, X indicates a halide
(Cl−, Br−, I−) or an oxygen ion, hence perovskites can be separated into perovskite halides and
oxide) [8]. This material exhibits intriguing features because of the inclusion of barium (Ba)
atoms into the crystalline lattice of chromium oxide (CrO2). Barium-doped chromium oxide is a
promising class of materials with tunable characteristics and numerous applications in
electronics, energy storage, catalysis, and sensing. Further research into the synthesis,
characterization, and uses of BaCrO3 is required to realize its full potential in many technological
domains.

b. Iron-Doped with chromium oxide(FeCr2O4):

FeCr2O4 belongs to the spinel group of minerals and has a cubic crystal structure. Iron and
chromium ions occupy the tetrahedral and octahedral positions in the crystal lattice, respectively.
The arrangement of ions creates its distinctive spinel structure, which can affect its physical and
chemical properties.
Iron doping can also affect the electrical conductivity of FeCr2O4. The presence of iron ions can
inject new charge carriers into the material, altering its electrical resistivity and conductivity. This

9
feature is useful in applications including solid oxide fuel cells, oxygen sensors, and electrical
devices.
Iron-doped chromium oxide materials are typically thermally stable, making them ideal for high-
temperature applications. FeCr2O4 can resist high temperatures without major structural changes
or degradation, making it suitable for use in refractories, thermal barrier coatings, and high-
temperature catalysis. Iron doping introduces magnetic moments within the chromium oxide
lattice, which causes ferrimagnetic behavior. FeCr2O4 has ferrimagnetic ordering, which means
opposing magnetic moments align in parallel and antiparallel configurations inside the crystal
structure. Magnetic behavior is used in a variety of applications, including magnetic recording
media, magnetic sensors, and magnetic nanoparticles for biological purposes.

c. Vanadium-Doped with chromium oxide (V2CrO7):

Vanadium-doped chromium oxide, also known as V2CrO7, is a compound formed by substituting

vanadium (V) ions for chromium (Cr) ions in the chromium oxide (Cr2O3) lattice. V2CrO7
generally has a layered or lamellar crystal structure. Vanadium ions replace chromium ions in the
crystal lattice, altering the material's structural arrangement and characteristics. The physical,
chemical, and electrical properties of a material can be influenced by its crystal structure and
atomic arrangement. Vanadium doping can alter the magnetic properties of chromium oxide.
V2CrO7 may have intriguing magnetic properties, depending on the oxidation state of vanadium,
the concentration of dopants, and the crystal structure. These magnetic properties, which include
paramagnetism, anti-ferromagnetism, and ferrimagnetism, are important for applications in
magnetic recording medium, spintronics, and magnetic sensors.

Vanadium-doped chromium oxide may have different electrical conductivity than pure
chromium oxide. The presence of vanadium ions can inject new charge carriers into the material,
influencing its electrical resistivity and conductivity. This feature has potential applications in
electronic devices, solid oxide fuel cells, and electrochemical sensors.

1.5. OXIDES:

10
Oxides are substances created through the chemical combination of oxygen and other elements.
These molecules normally contain oxygen in the - 2 oxidation state, but there may be exceptions.
Oxides serve important roles in a variety of physical processes, including corrosion, combustion,
and mineral formation. They play a significant role in domains like as materials science and
environmental science.
Oxides are made up of oxygen atoms linked to other elements. These elements can vary greatly,
resulting in a large spectrum of oxides with distinct properties and applications. For example,
carbon dioxide (CO2) is an oxide made up of carbon and oxygen atoms, but silicon dioxide
(SiO2) is made up of silicon and oxygen. Similarly, Chromium oxide (CrO2) consists of
chromium and oxygen atoms. The chemical and physical properties of an oxide compound are
determined by its precise elemental combination.
One exciting characteristic of oxides in physics is their catalytic activity. Oxides can operate as
catalysts, accelerating chemical reactions without being consumed in the process. Transition
metal oxides, such as chromium oxide (CrO2), are commonly employed in catalysis. Chromium
oxides have been intensively studied because of their potential industrial applications as
catalysts, although little emphasis has been placed on the structural relationship to catalytic
characteristics [9].

11
 CHAPTER#02
LITERATURE REVIEW

AVNISH KUMAR ARORA et al. Chromium oxide nanoparticles (NPs) were produced
using ammonia as a precipitating agent and studied using X-ray diffraction (XRD), UV-Visible
absorption (UV), and infrared spectroscopy (IR).

The study uses electron microscopy and X-ray diffraction to analyze the formation and size of
chromium oxide nanoparticles (Cr2O3). The nanoparticles, ranging from 20 to 70 nm in size,
have an average crystalline size of 45 nm. They are thermally stable up to 1000°C. The synthesis
process involves precipitation gelation, sol gel, mechanochemical reaction, chromium oxidation
in oxygen, and sonochemical technique. The X-ray diffraction map reveals peaks from Cr2O3,
confirming the nanoparticle nature and the sharpness of the peaks.

t = K/ B cos

SEM analysis reveals white chromium oxide particles. TEM scans show particle sizes ranging
from 20-70 nm. Hexagonal chromium oxide nanoparticles are produced using ammonia
precipitation. XRD tests show chromium oxide was produced as Cr2O3, not CrO2 [10].

N Shahmir al et. This study reveals the green production and characterization of barium

chromate nanoparticles using Glycyrrhiza glabra extract as a natural surfactant. The resulting
BaCrO4 nanoparticles were analyzed using UV-Vis, FT-IR, XRD, and SEM techniques. Greener
processes in chemistry and chemical technology are gaining popularity due to environmental
concerns. The FT-IR spectra show significant chromate group absorption bands. The study
reveals that XRD patterns and scanning electron microscopy (SEM) analysis of BaCrO4
nanoparticles reveal a narrow size distribution of 30-60 nm. The synthesis of these
nanoparticles is facilitated by Glycyrrhiza glabra extract, which consists of macromolecules with
ionic hydrophilic and hydrophobic regions. The hydrophilic ends absorb Ba2+ ions, allowing for

12
the formation of nanoparticles. The green BaCrO4 nanoparticles are orthorhombic and belong
to the Pnma space group [11].

Oscar Restrepo et al. This paper synthesizes a nano-pigment with a spinel structure using
CrZ03 and Fe304 precursors. The nanoparticles are produced at high temperatures and
undergo characterization using X-ray diffraction, spectroscopy, thermal analysis, scanning
electron microscopy, UV-VIS spectrophotometry, colorimetry, CTEL *a*b*, and magnetic
susceptibility testing. Spinel structures produce nanoparticles smaller than 100nm, with
reflective spectra varying based on phase, crystallinity, cation spacing, and magnetic properties.
Spinals with transition metal ions have significant commercial value due to their unique
structural, electrical, and magnetic properties. Ceramic pigments with specific properties, such
as structural durability and color transfer, are used in the ceramic industry for decoration and
practical enamels. The study synthesized CrFe204 compositions using an auto-combustion
technique, involving citrate precursors of metals mixed in solution [12].

Ahlam Zekaik et al. The study investigates the effect of copper incorporation
on the structural, morphological, optical, and electrical properties of Cr 2O3 thin films
synthesized using a sol-gel dip-coating technique. The Cr source was Chromium (III) Nitrate
Nonahydrate, while the dopant was Cu(NO3)2. The crystal structure, optical, and electrical
characteristics were investigated. XRD analysis revealed that the films with a high degree of
crystallinity were rhombohedral Cr2O3 phases. The size of the crystallites decreased as the Cu
doping fraction increased. The AFM results showed that the doped Cr 2O3: Cu thin films have a
lower surface roughness. The UV-Vis spectra of the Cu doped-Cr2O3 films showed remarkable
transparency in the visible region. The optical band gap in Cr2O3 thin films reduces as the Cu
doping rate increases. The equivalent circuit of Cu doped-Cr2O3 films is a parallel circuit RpCp.
As the concentration of Cu increases, resistance RP decreases and capacitance Cp increases.

Chromium (III) oxide has been the subject of numerous researches and studies due to its unique
and varied properties, including thermodynamic stability at high temperatures, chemical
resistance, hardness, catalytic, medicinal, and antiferromagnetic properties. Thin films of

13
chromium dioxide can display either p or n-type semiconductor activity, making them highly
stressed functional materials in various applications. The sol-gel method has emerged as one of
the finest ways for synthesizing metal oxide materials with important characteristics.

The surface morphology of Cu-doped chromium (III) oxide thin films is significantly influenced
by Cu content, as they appear more porous. FT-IR spectra show consistent peaks at the same
wavenumber, indicating structural bonding remains unchanged with doping. Absorption bands
under 800 cm−1 indicate the production of crystalline chromium (III) oxide. The study
investigates the effect of copper doping on the structural, optical, and electrical properties of
Cu: Cr2O3 thin films deposited on glass substrates using a sol-gel dip coating method. Results
show that increased copper content improves transparency and reduces optical band gap
energy, while copper ions create oxygen point defects controlling film densification [13].

M. Zzaman et al. This study investigates the magnetic properties of Cr doped VO2,
V1−xCrxO2 (VCO) thin films, focusing on their structural, electronic, and magnetic properties. The
researchers used X-ray absorption spectroscopy and magnetic circular dichroism to study the
origin of matrix enhancement with Cr-substitution. The results show that V and Cr ions are
ferromagnetic at room temperature, indicating a ferromagnetic insulating state and charge-
ordered V and Cr sites.

The metal to insulator transition (MIT) in oxide materials like vanadium dioxide (VO 2) is a
fascinating phenomenon with potential applications in sensors, actuators, thermochromic
devices, thermometers, and other multifunctional electronic devices. The MIT temperature of
VO2 is around 340 K, close to room temperature, and its first-order MIT from insulating
monoclinic (RT) M1phase to metallic rutile (high-temperature) R-phase makes it a promising
material for developing ultrafast switching and sensing in advanced technology devices. The
MIT temperature can be tuned by substitution of other elements in VO2, which can modify its
electronic and magnetic properties and study the physics of Peierls and Mott transition. VO2 and
CrO2 are examples of anti-ferromagnetic insulators and ferromagnetic metals, respectively. For
Cr substitution (10-20%) in the rutile phase, VO2 has initiated to behave as a ferromagnetic
insulator. This study investigates the effect of Cr-substitution in VO2 films, V1−xCrxO2, on its

14
electronic and magnetic properties using X-ray absorption spectroscopy (XAS) and soft X-ray
magnetic circular dichroism (XMCD).
VCO films of 40 nm thickness were produced on R-sapphire substrates using the PLD approach
(KrF excimer laser, wavelength = 248 nm, recurrence rate: 5 Hz, ease: ~1.1 J cm−2) at 500 °C in
an oxygen environment of 10 mTorr. The crystal structure and lattice characteristics of the films
were analyzed using a method called X-ray diffraction (GIXRD, He D8) with Cu Kα radiation at
a dipping incoming angle of 0.2° with an optical step size of 0.0025°[14].

By using the sol-gel process, J.H. Li et al. investigated the diluted magnetic semiconductor
ZnMnO nanocluster. The elements Mn, Zn, and O were present in the XPS spectra. Based on
XPS data, calculations indicate Zn0.9Mn0.1O and ZnMn2O4 are both present in our sample. It is
probable that the powder contains three different types of Mn ions, as indicated by the visible
signal of Mn2+ in the EPR pattern with g 14 1:9961. The coercivity value and remnant
magnetization are found to be, respectively, 144.44 Oe and 7.75 106 emu, using a hysteretic loop
at room temperature. The magnetization curve indicates that the ferromagnetic ordering most
likely starts in ZnMn2O4 [15]

K. Omri et al. Mn-doped ZnO were created using the sol-gel technique with ethyl
alcohol dried under supercritical conditions. The structure, morphology, optical, magnetic, and
transmission electron microscopy (TEM), as well as UV measurements and a superconducting
quantum interference device (SQUID), were investigated for the as-prepared nanoparticles. The
structural features of the undoped and Mn-doped ZnO nanoparticles revealed their hexagonal
wurtzite structure. Optical tests showed that when Mn concentration increased, the transmittance
in the UV region decreased. [16]

M. El-Hilo et al. investigated the effects of oxygen vacancies on the ferromagnetic

coupling of Mn ions using two distinct preparation techniques: method (I) and method (II).
Whereas technique (II) employed a closed environment for preparation, method (I) used an open
one. To produce long-range ferromagnetic order, these samples must have defects that mediate
the FM coupling. The FM seen in this work could be explained by the presence of oxygen
vacancies, which mediate the ferromagnetic exchange between the coupled Mn ions. This is
consistent with the concept of bound magnetic polarons (BMP), which states that long-range

15
ferromagnetic order in dilute magnetic semiconductors is generated by overlapping polarons
caused by defects such as oxygen vacancies (DMS) [17]

Tokeer Ahmed et al. this study covered the most current discoveries in systems based on
ZnO and CdO materials as well as the optical properties and experimental developments of
oxide-based DMSs. Transition metal (TM)-doped ZnO, CdO, and dilute magnetic semiconductor
nanoparticles exhibit red shifts in their energy band gaps [18].

The structural and magnetic characteristics of Mn and Ni co-doped ZnO nanoparticles were
investigated by Vijayaprasath et al. XRD analysis revealed that the only phase of all the
nanoparticles was the wurtzite type of pure and co-doped ZnO with Mn and Ni, with a size range
of 26 to 38 nm. Optical spectroscopies in the UV and FTIR disclosed the dopant composition of
zinc oxide nanoparticles. When a transition metal is doped, photoluminescence intensities
change because there are more oxygen vacancies. The ferromagnetic behavior of the dopant
material at room temperature was confirmed by M-H loop using VSM. These results showed that
doping transition metal with nanoparticles enhances the performance of magnetic and spintronic
devices [19].
ZnO nanoparticles were used in a sol-gel method for Mn doping by Bououdina et al.The
powdered nanoparticles were created by autoclaving the fluid at a predetermined temperature.
TEM revealed that the crystallite's size was between 30 and 50 nm. Rietveld refinements
demonstrated an effective synthesis that doped less Mn with ZnO. It was discovered that the
lattice parameters increased as Mn increased. Research on magnetic materials has shown that
heavily doped Mn does not improve the long-range order of ferromagnetism; instead, it just
increases the paramagnetic component in a sample. The magnetic moment of uncoupling was
produced by a linear rise in the susceptibility of paramagnetic materials with an increase in Mn
concentration [20].
The utilisation of the sol-gel process to produce ZnO-doped Mn nanoparticles was investigated
by Pairot Moontragoon et al. Through XRD analysis, the hexagonal wurtzite structure with a
single phase was verified. The optical properties of the dopant zinc oxide nanoparticles were
confirmed using UV analysis, which also revealed their bandgap of 1.97 eV. Using VSM,
magnetic characteristics were verified, demonstrating how the dopant substance changed the

16
material's behaviour to become ferromagnetic. Due to the rise in spinning moment and magnetic
behaviour, a very high magnetic dipole moment was also found in the dopant material [21].

17
 CHAPTER#03

METHODOLOGY

There are numerous uses for transition metal oxide nanoparticles as adsorbents,
superconducting materials sensors, and catalytic. An important family of materials used in
environmental research, biology, electricity, chemical sensors, magnetism, and other domains is
metal-oxides. The significance of chromium oxides in science and engineering has garnered a lot
of attention lately. Chromium can create a variety of oxides because it has several stable
oxidation modes.
They can be synthesized through several methods which are given below,
 Solid-state reaction
 Sol-Gel method
 Combustion synthesis

For this, the Sol-Gel process has been employed.

3.1: SOL-GEL METHOD:

SOL is simply a liquid with floating colloidal particles in it. A precursor that is either fully
or partially soluble in a solvent can create it.
GEL is a somewhat rigid material that resembles a solid and has a network of particles
called colloidal that trap solvent.
GEL comes in two varieties:
i Colloidal gel (having network of colloidal particles).
ii Polymeric gel (having network of polymers).
A more chemical (wet chemistry method) for creating different nanostructures, particularly metal
oxide nanoparticles, is the sol-gel procedure. This process involves dissolving the molecular
precursor (often metal alkoxide) in alcohol or water, heating it, and stirring it to cause
18
breakdown or alcohol hydrolysis to turn it into gel. whichever are the required qualities and
intended use of the gel, the wet or damp gel formed from the hydrolysis/alcoholysis process
should be dried using the suitable techniques. The sol-gel process is economical and offers
considerable control across products' chemical composition because of its low reaction
temperature. For instance, burning alcohol completes the drying process in the case of an ethanol
solution. The generated gels are pulverized and then calcined following the drying phase. The
sol-gel process is economical and offers considerable control over the products' chemical
makeup because of its low reaction temperature. The sol-gel technique has several advantages as
an intermediary between thin layers of metal oxides and can be utilized as a molding material in
earthenware production. Many optical, electronic, energy, surface engineering, biosensor,
medicinal, and separated technologies (like chromatography) use materials derived from the sol-
gel process [22].

A common and industrial technique for creating nanoparticles with varying chemical
compositions is the sol-gel method. The creation of a homogenous sol from the precursors and its
transformation into a gel form the foundation of the sol-gel process. After that, the gel's solvent
is extracted from its gel-like structure, and the gel that remains is dried. The drying process has a
major impact on the dried gel's characteristics. Stated differently, the choice of the "removing
liquid method" is contingent upon the intended usage of the gel.
Dried gels have application in a variety of industries, including surface coating, insulation in
buildings, and specialty garment manufacturing. It is important to note that nanoparticles can be
obtained by processing the gel in specialized mills [23].

3.2: Stoichiometry and Calculation for sample:

 For CuCrO2

First, we calculate the molecular weight;

Chromium Nitrate (Cr(NO3)3.9H2O)= 400.21g

Copper Nitrate (Cu(NO3)2.3H2O) = 241.63g

19
Total Weight = 400.21g+241.63g = 641.84g

For Cu1, Cr1:

(Cr(NO3)3.9H2O)=1 x atomic weight of Cr=1 x 52u = 52u

(Cu(NO3)2.3H2O)=1 x atomic weight of Cu =1 x 63.5u = 63.5u

Total weight = 52u + 63.5u =115.5u

For 20grams:

20 grams/mol contain Cr = (52 x 20)/115.5=9.00gm/mol

20 grams/mol contain Cu = (63.5 x 20)/115.5=11.00gm/mol

Now the atomic weight of CuCrO2 = (52) (1) + (63.5) (1) + (16) (2) = 147.5gm
Water quantity for 20-gram solution:
For 1 molar solution: (1 x 20)/147.5=0.135 x 1000=135.5 ml
For half molar solution :(135.5/2) =67.7 ml

 For V2CrO7
First, we calculate the molecular weight;

V2O5 = 181.88g

(Cr (NO3)3.9H2O) = 400.21g

Total Weight = 181.88g + 400.21g = 582.09g

For V2, Cr1:

V2O5 = 2 x atomic weight of vanadium = 2 x 50.94u = 101.88u

(Cr (NO3)3.9H2O) = 1 x atomic weight of chromium =1 x 52u = 52u

Total Weight = 101.88u + 52u =153.88u

For 20grams:

20
20 grams/mol contain Cr = (52 x 20)/153.88=6.76gm/mol

20 grams/mol contain V = (101.88 x 20)/153.88=12.8gm/mol

Now the atomic weight of V2CrO7 = (52) (1) + (181.88) (2) + (16) (7) = 265.88gm

Water quantity for 20-gram solution:

For 1 molar solution: (1 x 20)/265.88 =0.075x 1000=75.22 ml

For half molar solution :(75.22/2) =37.61 ml
 For BaCrO4

First, we calculate the molecular weight;

Chromium Nitrate (Cr (NO3)3.9H2O) = 400.21g

Barium Nitrate (Ba (NO3)2) = 261.34g

Total Weight = 400.21g+261.34g = 661.55g

For Ba1, Cr1:

Ba(NO3)2 = 1x atomic weight of barium = 1 x 137.327u = 137.327u

(Cr(NO3)3.9H2O) = 1 x atomic weight of chromium = 1 x 52u = 52u

Total Weight = 137.327u + 52u =189.327u

For 20grams:

20 grams/mol contain Cr = (52 x 20)/189.327=5.49gm/mol

20 grams/mol contain Ba = (137.325 x 20)/189.325=14.5gm/mol

Now the atomic weight of BaCrO3 = (52) (1) + (137.325) (1) + (16) (3) = 237.325gm

Water quantity for 20-gram solution:

21
For 1 molar solution: (1 x 20)/237.325 =0.085x 1000=85.00 ml
For half molar solution :(85/2) =42.13 ml

3.3. STEPS FOR PREPARING SAMPLES:

FIGURE 7 :SOL-GEL METHOD

i Measuring Precursors
ii Stirring
iii Heating and Drying
iv Grinding or Crushing
v Storing
vi Annealing

3.3.1. Measuring Precursors:

The computed weights mentioned above were determined using an electronic balance, a
digital tool for determining an object's mass or weight. Also referred to as an electronic weighing
scale, it is a development over conventional mechanical weighing scales that used springs and

22
levers to determine weight.

3.3.2. Stirring:

Using the magnetic hot plate, we first added some distilled water to a beaker and dissolved
each measured substance one at a time while stirring continuously. To regulate the pH, a certain
quantity of ammonium nitrate was applied. At room temperature, this stirring was done for
fifteen minutes.

3.3.3. Heating and Drying:

23
 After that, the "heat switch" is activated and the beaker is set on a magnetic hot plate. A
thermometer is inserted and the solution is kept at 90 degrees Celsius. Following four to five

hours of heating, a variety of gasses are eliminated, and finally combustion occurs. Gel is created
as a result of combustion, as seen below.

3.3.4. Crushing or Grinding:

Ultimately, a mortar and pestle were used to smash the dried gel into a fine powder, which
was then stored in sample tubes for subsequent steps.

3.3.5.Storing:

24
 The grinded powdered was kept into jars and vials.

3.3.6 Sintering of sample:

The powdered form sample was then putted into boats and sintered at 400-900 oC for 3-4 hours.

25
 CHAPTER#04

CHARACTRISATION TECHNIQUES

Due to their wide range of applications, nanostructures, a rapidly expanding class of

materials, have sparked intense interest. The size, crystal structure, elemental content, and many
other physical characteristics of nanoparticles have been described using a number of methods.
Certain physical qualities can be assessed using multiple methods in various situations. Selecting
the best methodology is typically complicated by the various advantages and disadvantages of
each technique, necessitating a combinatorial characterisation approach. Additionally, given the
growing importance of nanoparticles in fundamental research and applications, it is imperative
that scientists from various fields overcome the difficulties associated with reliably and
reproducibly characterizing nanomaterials following their synthesis and subsequent processing
stages (such as annealing).
Characterization techniques refer to the various methods and approaches used to understand
and describe the properties, structure, and behavior of materials, substances, or systems. These
techniques are commonly employed in fields such as materials science, chemistry, physics,
biology, and engineering. Here are some commonly used characterization techniques .

4.1. XRD (X-RAY DIFFRACTION):

One popular method for figuring out a sample's makeup or crystalline structure is
diffraction of X-rays. The atom arrangement of bigger crystals, like macromolecules and
inorganic compounds, can be ascertained using this method. It may determine stage purity,
structure, and crystallinity if the crystal size is too small.
Using this method, x-ray beams are passed through it. Instead of utilizing considerably longer
wavelengths that are which would remain unchanged by the spacing between atoms, X-ray
beams are chosen because their wavelength is similar to the spacing between atoms in the
sample. As a result, the angle of diffraction will be modified by the space of the atoms in the
molecular structure. Following their passage through the sample, the x-rays "bouncing" off of the

26
atoms in the structure cause the beam to change directions at an angle, theta, that differs from the
initial beam. This is the diffraction angle. While some of these diffracted beams cancel each
other out, positive interference happens when the beams have similar durations.
When two x-ray beams with whole number integer wavelengths combine to form a new beam
with a larger amplitude, this is known as constructive interference. For this particular angle of
reflection, a larger signal corresponds with a larger wave amplitude. The difference between
atomic planes can then be calculated using the angle of diffraction and Bragg's rule,
nλ
sin θ=
2d
where d is the distance between atomic planes, lambda is the wavelength to be stated that and
theta is the angle of diffraction. The composition or crystalline structure can then be ascertained
by measuring the distance among atomic planes [24].

FIGURE 8 BRAGG'S LAW REFLECTION.

4.1.1. WORKING PRINCIPLE:

While X-rays are thought of as electromagnetic radiation waves, crystals are regular
arrangements of atoms. Incident X-rays are scattered by crystal atoms, mostly as a result of

27
interactions with their electrons. The electron is referred to as the scatterer in this occurrence,
which is called elastic scattering. A regular array of spherical waves is generated by a regular
array of scatterers. These waves cancel each other out destructively by interference in most
directions, but according to Bragg's law, they add constructively in a few particular directions
[25].

4.2. UV-Vis SPECTROSCOPY:

The analytical method known as UV-Vis spectroscopy counts the number of distinct UV or
visible light frequencies that a sample absorbs or transmits when compared to a reference or
blank sample. The composition of the sample affects this feature, which may reveal information
about the contents and concentrations of the sample. Since light is used in this spectroscopy
approach, let's start by talking about what light is made up of.

An energy level for light is inversely proportional to its wavelength. As a result, light has a
greater energy at shorter wavelengths and less at longer wavelengths. In order for us to perceive
absorption, something's electrons must be promoted to a higher energy state with a certain
amount of energy. To move electrons to a higher energy state, a substance's electrons in various
bonding settings need distinct amounts of energy. This explains why various compounds absorb
light at different wavelengths. Humans are able to see a range of visible light wavelengths, from
around 380 nm, or violet, to 780 nm, or red.1 UV light has wavelengths that are about 100 nm
shorter than visible light's. Consequently, the wavelength of light can be used to characterize it.
This can be helpful in UV-Vis spectroscopy to identify or study various compounds by
identifying the precise wavelengths that correlate to maximal absorbance.

28
 FIGURE 3. SCHEMATIC DRAWING OF THE OPTICAL SETUP OF A MONOCHROMATIC UV/VIS
SPECTROPHOTOMETER

4.3.1. WORKING PRINCIPLE: Although there are numerous varieties of the UV-Vis
spectrophotometer, let's take a closer look at its major parts to better understand how they
operate.

LIGHT SOURCE: Since this method relies on light, having a consistent source that can
produce light in a variety of wavelengths is crucial. For both UV and visible
wavelengths, a single xenon lamp is frequently utilized as a high intensity light source.
However, compared to carbide and halogen lamps, neon lamps are more expensive and
less stable.
When using two lamps in a gadget, the visible light is usually produced by a tungsten or
halogen lamp, while the UV light is often produced by a deuterium lamp.2. The light
source of the device must swap during measurement since two distinct light sources are
required to scan both of the UV and visible wavelengths. In actuality, this transition
usually takes place in the range between 300 and 350 nm, when both light sources emit
light similarly and the change may be accomplished more seamlessly.
WAVELENGTH SELECTION:
29
The next stage involves choosing from among the wide range of light wavelengths that
the light source emits those that are appropriate for the type of sample and analyte for
detection for sample inspection. There are several approaches that can be used for this.

 Monochromaters-The monochromator divides light's wavelengths into a small

range. Most frequently, it is based on dispersion gratings, which may be rotated
to select the required light wavelength by adjusting the incoming and reflected
angles.1, 2 The number of grooves per millimeter, or groove frequency, is a
common way to quantify the diffraction grating. An increased grooved
frequency results in an enhanced optical resolution; nevertheless, the useable
wavelength range is reduced. Although the useable wavelength range is greater
with a lower groove frequency, the optical resolution is decreased. For UV-Vis
spectroscopy, 300–2000 grooves per mm are useful, while 1200 grooves per mm
is the usual minimum. Physical flaws in the optical setup and diffraction device
can affect the quality of those spectroscopic observations.
 Absorption filters: Usually constructed of tinted glass or plastic, absorption
filters are intended to capture specific light wavelengths.2.
 Dichroic filters, also known as interference filters, are widely used filters
consisting of many dielectric layers where interference arises between the thin
material layers. By destructively interfering with desired wavelengths, these
filters can be utilized as wavelength selectors.1, 2
 Cutoff filters: Cutoff filters let light through at wavelengths that are either
below (shortpass) or above (longpass). Interference filters are often used to
implement these.
 Bandpass filters: By combining shortpass and longpass filters, bandpass
filtering enable a range of frequencies to pass through.

Due to their versatility, monochrome filters are most frequently utilized in this
technique. To increase the ratio of signal to noise and restrict the further picked
light wavelengths for more accurate measurements, filters are frequently
employed in conjunction with monochrome detectors.
SAMPLE ANALYSIS:
30
 The light then travels through a sample in the spectrum analyser, depending on the
wavelength of the selector that is being used. Measuring a reference sample—also
known as the "blank sample"—such as a cuvette filled with the same solvent used to
create the sample is essential for all studies. The aqueous buffered solution devoid of the
item of interest is utilized as the reference if an aqueous buffered solution containing the
sample is used for analyses. Sterile culture medium would be the standard for analysing
bacterial cultures. The equipment then automatically uses the signal from the sample
being studied to assist in determining the actual absorbance values of the analytes.

Understanding the materials and conditions utilized in UV-Vis spectroscopy

investigations is crucial. For example, because plastic absorbs UV radiation in general,
most plastic cuvettes are not suitable for UV absorption research. Glass can function as
a filter, frequently letting some UVA (315–400 nm)2 through while absorbing the
majority of UVC (100–280 nm)2 and UVB (280–315 nm)2. Since quartz is transparent
to most UV light, sample containers made of quartz are necessary for UV testing.
Because molecular oxygen in the air absorbs light wavelengths shorter than roughly 200
nm, air can also be thought of as a filter.
Identification:
A detector is used to transform the light into a readable electronic signal once it has
passed through the sample. Typically, semiconductors or photoelectric coatings serve as
the foundation for detectors.

4.3. FTIR (Fourier Transform Infrared

Spectroscopy):
Transform of Fourier FTIR analysis, sometimes referred to as Infrared Spectroscopy
Analysis, is an analytical method for classifying materials as organic, polymers, and
occasionally inorganic. Infrared light is used in the FTIR analysis procedure to scan test
materials and evaluate chemical characteristics.

31
 FIGURE 4. THE SCHEMATIC REPRESENTATION OF FTIR

4.4.1. FTIR operation:

When infrared light between 10,000 and 100 cm-1 is sent through a sample by the FTIR
gadget, some of the heat gets absorbed and some is sent through. The sample molecules
transform the absorbed radiation into vibrational and/or rotational energy. The final
signal at the detector is a range that shows up as the sample's chemical fingerprint and
usually ranges from 4000 cm-1 to 400 cm-1. The spectrum fingerprints that each
molecule or chemical structure produces are unique, which makes FTIR analysis an
excellent tool for chemical recognition [26].

32
 FIGURE 5. SCHEMATIC REPRESENTATION OF THE WORKING PRINCIPLE OF FTIR[43]

4.4.2. Need for FTIR employment:

When assessing industrially created material, FTIR spectroscopy is a well-established

method for quality control that is frequently used as the initial step in the material
examination process. A shift in the distinctive absorption band pattern unmistakably
suggests that the material's composition has changed or that contamination is present.
FTIR microanalysis is usually used to identify the source of a product's faults if they are
detected through visual inspection. This method works effectively for examining bigger
surface areas and tiny particles (usually 10–50 microns) to determine their chemical
makeup.

With FTIR analysis, one can:

• Determine the identity and properties of unknown materials, such as liquids,

solids, films, or powders.
• Determine whether a substance is contaminated (e.g., by particles, fibers,
powders, or liquids).
• After being extracted from a polymer matrix, identify the additives.
• Determine whether oxidation, breakdown, or uncured monomers are present in
failure analysis inquiries.

33
CHAPTER 5
RESULTS AND DISCUSSION
This chapter presents the findings from the comprehensive analysis conducted using various
advanced characterization techniques, including X-ray Diffraction (XRD), Ultraviolet-Visible
(UV-Vis) Spectroscopy, Fourier Transform Infrared (FTIR) Spectroscopy, and Scanning
Electron Microscopy (SEM). The XRD analysis revealed detailed information about the
crystalline structure and phase composition, enabling us to identify and quantify the
crystallographic phases present. The UV-Vis spectroscopy results highlighted the optical
properties, including band gap energy and light absorption characteristics, essential for
understanding the electronic behavior of the materials. FTIR spectroscopy provided a molecular-
level view, identifying functional groups and chemical bonds present. SEM analysis offered
high-resolution images of the surface morphology, providing critical insights into the
topographical features and particle size distribution.

5.1. Powder X-ray diffraction (XRD)

XRD analysis (V2CrO7):

The XRD analysis of V2CrO7 annealed at 450°C is shown in figure and the distance between
atomic layers in a crystal, d was observed as 4.363 Å. The 2θ peaks were observed at (111),
(200), (210), (211), (220), (311), (321), (420) and (422) in the range of 10°-60°. The crystal
resulted in a cubic structure with lattice parameters to be a=b=c= 8.72Å. The volume of the
lattice was found to be 636.06Å3.

34
XRD analysis (FeCr2O4):
Similarly, results below show the XRD analysis of FeCr2O4 annealed at 650°C. 2θ peaks of the
sample were observed at (110), (113), (202), (205), (211), (214), (203), (211) and (202). The d
length was found to be 3.63Å which resulted in the rhombohedral crystal structure with crystal
lattice being a=b= 5.11Å and c=12.13Å. The volume of the lattice was found to be 316.73Å3.

XRD analysis (CuCrO2):

The XRD results for CuCrO2 annealed at 900°C is shown in figure 1. The distance between
atomic layers of the crystal, d is given by 2.85Å. It can be seen that resulting structure of CuCrO 2
is trigonal with lattice parameters of a=b=2.96Å and c=17.1Å. The volume of this structure is
129.75Å3.

35
XRD analysis(BaCrO4):

Similarly, the XRD data for BaCrO3 annealed at 150°C can be seen in figure 2. Average d-
spacing for the compound is given by 4.30Å. The structure of BaCrO3 is orthorhombic with
lattice parameters given by a=5.40Å, b=7.41Å and c=9.3Å. The volume of this orthorhombic
structure is given by 372.13Å

Materials a b c d-spacing Volume

CuCrO2 2.96Å 2.96Å 17.1Å 2.85Å 129.73Å3

BaCrO4 5.40Å 7.41Å 9.3Å 4.3Å 372.13Å3

FeCr2O4 5.11Å 5.11Å 12.13Å 3.62Å 316.73Å3

V2CrO7 8.72Å 8.72Å 8.72Å 4.363Å 636.06Å3

36
 Table.1: Structural Parameters calculated from XRD data

5.2. UV-Vis Spectroscopy

UV-Vis spectroscopy (V2CrO7):

The UV-Vis spectroscopy provided following results where the bandgap of vanadium chromium
oxide (V2CrO7) was found to be 4.95eV. The incest graph shows the Tauc Plot that is used to
calculate bandgap.

UV-Vis spectroscopy (FeCr2O4):

Result below shows a relation between absorption and wavelength for a solution of iron
chromium oxide FeCr2O4 in ethanol. Incest graph shows Tauc plot through which the bandgap of
FeCr2O4 is found to be 5.30eV

37
UV-Vis spectroscopy (CuCrO2):
The UV-Vis spectroscopy provided following results where the bandgap of Copper Chromium
Oxide (CuCrO2) was found to be 5.4eV. The incest graph shows the Tauc Plot that is used to
calculate bandgap.

UV-Vis spectroscopy (BaCrO4):

Finally, the result below shows a relation between absorption and wavelength for a solution of
Barium Chromium Oxide (BaCrO4) in ethanol. Incest graph shows Tauc plot through which the
bandgap of BaCrO4 is found to be 5.60eV

38
5.3. FTIR Spectroscopy:

FTIR spectroscopy (V2CrO7):

FTIR spectroscopy is used to identify and analyze the chemical composition of materials by
measuring the absorption of infrared light, which provides information about molecular
vibrations and functional groups. Figure below shows FTIR spectra for vanadium chromium
oxide (V2CrO7). The different vibrations of the sample's bonds when exposed to infrared
radiation from the electromagnetic spectrum are responsible for the absorption peaks. In the
infrared spectrum, the wavenumber is often drawn between 4000 and 400 cm-1.

FTIR spectroscopy (FeCr2O4):

Following result shows a relation between Wavenumber and Transmittance for the sample of
iron chromium oxide FeCr2O4. Groups like C=O, O-H, and C-H are small groups of bonds that
are assigned group frequencies. These kinds of bonds are usually exclusive to a particular bond
or functional group within a structure, and they can be seen at 1500–400 cm-1 in the infrared
spectrum.

39
FTIR spectroscopy (CuCrO2):

FT-IR spectrum of the CuCrO2 nanoparticles is shown in following figure.it can be seen that one weak
(∼941 cm−1) and two strong bands (∼743 and 536 cm−1) are representing the CrIII–O and M–O bond
stretching frequencies of the CuCrO2 nanoparticles, respectively.

FTIR spectroscopy (BaCrO4):

Simple hetero-oxy compounds can be found within the range of 1000-1500 cm-1. In the data below, the
largest peak observed is in between the range of 1300-1500 cm-1 which represents the presence of
Aliphatic nitro compounds, Organic nitrates and Aromatic nitro compounds.

40
CONCLUSION:
In this thesis, we successfully synthesized and characterized Vanadium Chromium Oxide
(V2CrO7), Copper Chromium Oxide (CuCrO2), Barium Chromate (BaCrO4), and Iron Chromite
(FeCr2O4) nanoparticles using the sol-gel method. The comprehensive analysis using X-ray
Diffraction (XRD) and Ultraviolet-Visible (UV-Vis) spectroscopy provided information
regarding the structural and optical properties of these materials.

The XRD analysis revealed the lattice parameters for V2CrO7, CuCrO2, BaCrO4, and FeCr2O4 as
8.72Å, 2.96Å, 5.40Å, and 5.11Å, respectively. The crystal structures were identified as cubic for
V2CrO7, trigonal for CuCrO2, orthorhombic for BaCrO4, and rhombohedral for FeCr2O4. These
structural properties are critical as they influence the material's stability, reactivity, and overall
performance in potential applications.

The UV-Vis spectroscopy results indicated that the band gaps of the synthesized nanoparticles
were 4.95 eV for V2CrO7, 5.4 eV for CuCrO2, 5.60 eV for BaCrO4, and 5.30 eV for FeCr2O4.
These wide band gaps suggest that these materials have significant potential for applications in
optoelectronic devices, including UV detectors, photocatalysts, and solar cells, due to their
ability to absorb and emit light efficiently at specific wavelengths. Additionally, the large band
gaps also indicate their suitability for applications requiring high-energy photon interactions.

The successful synthesis and detailed characterization of these chromium-based nanoparticles

highlights their potential in many advanced technological applications. For instance, V 2CrO7,
with its cubic structure and considerable band gap, can be explored for use in high-performance
UV detectors and photocatalytic processes. CuCrO2, with its trigonal structure and band gap,
holds promise for transparent conducting oxides in optoelectronic devices. BaCrO4, characterized
by its orthorhombic structure and notable band gap, is a potential candidate for photonic and
optoelectronic applications. FeCr2O4, with its rhombohedral structure, offers potential uses in
magnetic materials and high-energy photonic applications.

The findings from this study not only demonstrate the successful synthesis of these novel
nanoparticles but also provide a foundation for further research and development. The unique
structural and optical properties identified in this study pave the way for further exploration in
fields such as energy conversion, environmental remediation, and advanced electronic devices.

41
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