Synthesis of Copper Ferrite Nano Particles
Synthesis of Copper Ferrite Nano Particles
Synthesis of Copper Ferrite Nano Particles
FINAL REPORT
BACHELOR OF SCIENCE
in
[PHYSICS, CHEMISTRY, MATHEMATICS]
Submitted by
NANDANA B (R19PC032)
POSHITH L (R19PC035)
R. YASHWANTH (R19PC036)
REVA University
Rukmini Knowledge Park, Kattigenahalli, Yelahanka, Bangalore-560064
2021-22
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Rukmini Knowledge Park, Kattigenahalli,
Yelahanka, Bangalore-560 064
Date: Date:
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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.
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
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1.INTRODUCTION
1.1 Abstract
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,
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Fig.1 showing increase in surface area of nanoparticles.
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
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1.3 Methods of synthesis of nanoparticles
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Methods in top-down approach:
1. Physical vapour deposition.
3. Ion implantation
5. X-ray lithography.[9]
down approach
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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]
1. Sol-gel synthesis
2. Co-precipitation method
3. Hydrothermal synthesis
5. Electrodeposition.
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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).
Advantages:
High productive
Low cost
No need to use any organic
solvents
Less time consuming
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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.
[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]
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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.
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1.5 Introduction to spectroscopic methods
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
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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.
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]
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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]
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detector (Everhart–Thornley detector) (Fig.11). The number of secondary elec-
trons that can be detected and thus the
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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.
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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]
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1.5.4.2 Accuracy of EDAX
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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.
counted (Fig.14).
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.
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ters, is required to produce monochromatic X-rays needed for diffraction
(Fig.15).
Fig.15 showing working of XRD
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2. Material and methods
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Reactions:
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3. Characterization
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:
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Fig.18 IR spectra for CuFe2O4
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Fig.19(A) SEM images of CuFe2O4 NPs
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Fig.20 (A) graph showing elemental composition of CuFe2O4
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,
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including high and low intensity peaks are in agreement with standard JCPDS file
no.34-0425[26].
0.9 λ
Debye-Scherrer formula : D= β cos θ where,
ϴ=angle of diffraction
k=Scherrer constant(0.9)
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λ = wavelength of x-ray used (0.154nm)
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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.
5. References
1. Kazemi, N., Mahdavi Shahri, M. Magnetically Separable and Reusable
CuFe2O4 Spinel Nanocatalyst for the O-Arylation of Phenol with Aryl Halide
Under Ligand-Free Condition. J Inorg Organomet Polym 27, 1264–1273
(2017). https://doi.org/10.1007/s10904-017-0574-0
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sional imaging of dislocations in a nanoparticle at atomic resolution". Na-
ture. 496, 74–77(2013). doi:10.1038/nature12009.
10.https://www.smacgigworld.com/blog/design-and-working-uv-vis-
spectrophotometer.php
12.Sugimoto, M. The Past, Present, and Future of Ferrites. J. Am. Ceram. Soc.
82, 269–280 (1999).
13.Zhen, L., He, K., Xu, C. Y. & Shao, W. Z. Synthesis and characterization of
single-crystalline MnFe2O 4 nanorods via a surfactant-free hydrothermal
route. J. Magn. Magn. Mater. 320, 2672–2675 (2008).
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15.Jamon, D. et al. Experimental investigation on the magneto-optic effects of
ferrofluids via dynamic measurements. J. Magn. Magn. Mater. 321, 1148–
1154 (2009).
17.Estrella, Michael; Barrio, Laura; Zhou, Gong; Wang, Xianqin; Wang, Qi;
Wen, Wen; Hanson, Jonathan C.; Frenkel, Anatoly I.; Rodriguez, José A. In
Situ Characterization of CuFe2O4 and Cu/Fe3O4 Water−Gas Shift Catalysts,
The Journal of Physical Chemistry C. 113 (32): 14411–14417(2009).
doi:10.1021/jp903818q.
18.https://www.smacgigworld.com/blog/design-and-working-uv-vis-spectropho-
tometer.php
19. https://byjus.com/chemistry/infrared-spectroscopy/
20.https://www.purdue.edu/ehps/rem/laboratory/equipment%20safety/Research
%20Equipment/sem.html
21.https://chem.libretexts.org/Courses/Franklin_and_Marshall_College/Introduc-
tion_to_Materials_Characterization__CHM_412_Collaborative_Text/Spec-
troscopy/Energy-Dispersive_X-ray_Spectroscopy_(EDS)
22. https://en.wikipedia.org/wiki/Energy-dispersive_X-ray_spectroscopy
23.https://serc.carleton.edu/msu_nanotech/methods/
XRD.html#:~:text=Fundamental%20Principles%20of%20X%2Dray
%20Powder%20Diffraction%20(XRD)&text=X%2Dray%20diffraction%20is
%20based,and%20directed%20toward%20the%20sample.
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24. Meidanchi, A, Ansari, H. Copper Spinel Ferrite Superparamagnetic
Nanoparticles as a Novel Radiotherapy Enhancer Effect in Cancer Treatment.
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