PROJECT REPORT ON SYNTHESIS

AND CHARACTERISATION OF
Fe3O4-PVA NANOCOMPOSITE

Submitted by: Submitted to:

Shreya Sharma Prof. S.K. Tripathi
M.Sc. (HS) Physics Department of Physics
2nd year (2018-19) Panjab University
Panjab University Chandigarh
Chandigarh
 ACKNOWLEDGEMENT
I genuflect to “The Almighty” the unseen force who is the cause of the
effect of this whole endeavor. Words elude me to express my profound
indebtness to my esteemed supervisor Prof. S. K. Tripathi for his
erudite guidance and constructive criticism in executing this arduous
task from its beginning to its completion. It has been my proud privilege
to work under him.
I am highly obliged to Prof. NAVDEEP GOYAL, Chairperson,
Department of Physics, Panjab University, Chandigarh for providing me
all the facilities which enabled me to complete my work.
Very special thanks to Mr. NAVJOT SINGH, PhD scholar in Physics
Department, who was the prime force behind the work and guided me at
every step thereby correcting the unseen mistakes.
I am fully indebted to Mr. SUKHDEEP SINGH and Ms JYOTI
KAUSHAL, PhD scholars in Physics Department, for providing me
constructive ideas and valuable inputs throughout the study.
All of them with their words of precision and perfection helped in
achieving smooth completion of the study.
Finally, it has been a great pleasure, satisfaction and honor for me to be
a postgraduate student of this reputed institute.

SHREYA SHARMA
 CONTENTS
1. Introduction

2. Nanoparticles

3. Nanocomposites

4. Characterization Techniques

5. Experimental Work

6. Results and Discussion

7. Conclusion

8. References
1. INTRODUCTION:
1.1. Nanotechnology:
Nanotechnology is science, engineering, and technology conducted at the
nanoscale, which is about 1 to 100 nanometers. Nanoscience and nanotechnology
are the study and application of extremely small things and can be used across all
the other science fields, such as chemistry, biology, physics, materials science, and
engineering.

1.2. How it started:

The ideas and concepts behind nanoscience and nanotechnology started with a talk
entitled “There’s Plenty of Room at the Bottom” by physicist Richard Feynman
at an American Physical Society meeting at the California Institute of Technology
(CalTech) on December 29, 1959, long before the term nanotechnology was used.
In his talk, Feynman described a process in which scientists would be able to
manipulate and control individual atoms and molecules. Over a decade later, in his
explorations of ultra precision machining, Professor Norio Taniguchi coined the
term nanotechnology. It wasn't until 1981, with the development of the scanning
tunneling microscope that could "see" individual atoms that modern
nanotechnology began. It’s hard to imagine just how small nanotechnology is. One
nanometer is a billionth of a meter, or 10-9 of a meter. Here are a few illustrative
examples:
 There are 25,400,000 nanometers in an inch.

 A sheet of newspaper is about 100,000 nanometers thick.

 On a comparative scale, if a marble were a nanometer, then one meter would be
the size of the earth.
Nanoscience and nanotechnology involve the ability to see and to control
individual atoms and molecules. Everything on Earth is made up of atoms—the
food we eat, the clothes we wear, the buildings and houses we live in, and our own
bodies. But something as small as an atom is impossible to see with the naked eye.
In fact, it’s impossible to see with the microscopes typically used in a high school
science classes. The microscopes needed to see things at the nano-scale were
invented relatively recently—about 30 years ago. Once scientists had the right
tools, such as the scanning tunneling microscope (STM) and the atomic force
microscope (AFM), the age of nanotechnology was born. Although modern
nanoscience and nanotechnology are quite new, nanoscale materials were used for
centuries. Alternate-sized gold and silver particles created colors in the stained
glass windows of medieval churches hundreds of years ago. The artists back then
just didn’t know that the process they used to create these beautiful works of art
actually led to changes in the composition of the materials they were working with.

Today's scientists and engineers are finding a wide variety of ways to

deliberately make materials at the nanoscale to take advantage of their enhanced
properties such as higher strength, lighter weight, increased
control of light spectrum, and greater chemical reactivity than their larger-scale
counterparts.

2. NANOPARTICLES:

A nanoparticle (or nanopowder or nanocluster or nanocrystal) is a microscopic

particle with at least one dimension less than 100 nm. Nanoparticle research is
currently an area of intense scientific research, due to a wide variety of potential
applications in biomedical, optical, and electronic fields. Nanoparticles are of
great scientific interest as they are effectively a bridge between bulk materials and
Ferroelectric materials smaller than 10 nm can switch their magnetization direction
using room temperature thermal energy, thus making them useless for memory
storage. Suspensions of nanoparticles are possible because the interaction of the
particle surface with the solvent is strong enough to overcome differences in
density, which usually result in a material either sinking or floating in a liquid.

Nanoparticles often have unexpected visible properties because they are small
enough to confine their electrons and produce quantum effects. For example, gold
nanoparticles appear deep red to black in solution. Nanoparticles have a very high
surface area to volume ratio. This provides a tremendous driving force for
diffusion, especially at elevated temperatures. Sintering can take place at lower
temperatures, over shorter time scales than for larger particles.

This theoretically does not affect the density of the final product, though flow
difficulties and the tendency of nanoparticles to agglomerate complicates matters.
The large surface area to volume ratio also reduces the incipient melting
temperature of nanoparticles.

3. NANOCOMPOSITES:

Nanocomposites are materials that incorporate nano-sized particles into a matrix of

standard material. The result of the addition of nanoparticles is a drastic
improvement in properties that can include mechanical strength, toughness and
electrical or thermal conductivity. The effectiveness of the nanoparticles is such
that the amount of material added is normally only between 0.5 and 5% by weight.

Nanocomposites are found in nature, for example in the structure of the abalone
shell and bone. The use of nanoparticle-rich materials long predates the
understanding of the physical and chemical nature of these materials. Jose-
Yacaman investigated the origin of the depth of color and the resistance to acids
polymer solutions (e.g. as paint viscosifiers) or the constitution of gels (e.g. as a
thickening substance in cosmetics, keeping the preparations in homogeneous
form). By the 1970s polymer/clay composites were the topic of textbooks although
the term "nanocomposites" was not in common use.

3.1. Improved Properties:

Nanocomposites can dramatically improve properties like:

1. Mechanical properties including strength, modulus and dimensional stability

2. Electrical conductivity

3. Decreased gas, water and hydrocarbon permeability

4. Thermal stability

5. Chemical resistance

6. Surface appearance

7. Optical clarity

3.2. Fundamentals of nanocomposites:

Nanoparticles have an extremely high surface to volume ratio which dramatically

changes their properties when compared with their bulk sized equivalents. It also
changes the way in which the nanoparticles bond with the bulk material. The result
is that the composite can be many times improved with respect to the component
parts. Some nanocomposite materials have been shown to be 1000 times tougher
than the bulk component materials.
 Figure 1 Nanocomposite with embedded nanoparticles

Figure 1 shows the nanocomposite with embedded nanoparticles that how the
nanoparticles are distributed in a matrix of polymer or a metal. There are metal-
matrix nanocomposites, polymer-matrix nanocomposites and magnetic
nanocomposites.

Nanocomposites, a high-performance material exhibit unusual property

combinations and unique design possibilities. With an estimated annual growth of
25% and fastest demand to be in engineering plastics and elastomers, their
potential is so striking that they are useful in several areas ranging from packaging
to biomedical applications.

The experimental work deals with the synthesis of polymer nanocomposites, so the
next article deals with the brief introduction about polymer nanocomposite.
3.2.1. Polymer Nanocomposites:

Polymer nanocomposites are materials in which nanoscopic inorganic particles,

typically 10-100 A⁰ in at least one dimension, are dispersed in an organic polymer
matrix in order to dramatically improve the performance properties of the polymer.
Systems in which the inorganic particles are the individual layers of a lamellar
compound - most typically a smectite clay or nanocomposites of a polymer (such
as nylon) embedded among layers of silicates - exhibit dramatically altered
physical properties relative to the pristine polymer. For instance, the layer
orientation, polymer-silicate nanocomposites exhibit stiffness, strength and
dimensional stability in two dimensions (rather than one). Due to nanometer length
scale which minimizes scattering of light, nanocomposites are usually transparent.
Polymer nanocomposites represent a new alternative to conventionally filled
polymers. Because of their nanometer sizes, filler dispersion nanocomposites
exhibit markedly improved properties when compared to the pure polymers or their
traditional composites. These include increased modulus and strength, outstanding
barrier properties, improved solvent and heat resistance and decreased
flammability.

Figure 2
4. CHARACTERISATION TECHNIQUES:

4.1 X-Ray Diffraction Technique:

XRD is an effective method for determining the crystal structure of materials.
Materials can be crystalline or amorphous. X-rays are electromagnetic radiations
having wavelength range from 0.01 nm-0.7 nm which is comparable with the
spacing between lattice planes in the crystal. In this technique, the atoms of the
material cause a beam of incident X-rays to diffract and constructively interfere in
specific directions. By measuring the angles and intensities of these diffracted
beams, one can determine the crystal structure and various other parameters linked
to lattice configuration.

The main components of a diffractometer are:

 X-Ray source
 Goniometer: the platform that holds and move the sample
 Sample holder
 Detector : to detect the scattered X-rays

Figure 3 Bragg’s X-Ray spectrometer

4.1.1 Bragg’s Law

The X-ray beams incident on a crystalline solid will be diffracted by the crystal
planes. Bragg’s law gives the condition for diffraction, which can be given as

n𝜆= 2d sin𝜃 (1)

where d is the spacing between two planes, n is an integer and 𝜆 is wavelength of

X-ray used. In diffractometer, the X-ray wavelength being fixed, the spacing
between diffracting planes of the atoms determines the peak positions. By
continuously changing the incident angle of the X-ray beam, a spectrum of
diffraction intensity versus twice the angle of incidence is recorded.

Figure 4 Diffraction through various planes of a crystal

The ‘𝜃’ is the angle between X-ray source and the sample whereas 2𝜃 is the angle
between the incident and the diffracted beam. The incident angle is always half of
the detector angle 2𝜃. The basic function of a diffractometer is to detect X-rays
scattered from materials and to record the diffraction intensity as a function of
diffraction angle 2𝜃. The position, intensity, shape and width of the peaks give
information about the sample.

4.1.2 Applications:

1. Spacing between atomic planes of a crystal: Inter planer spacing can be

obtained if the diffracted rays interfere constructively. The plane spacing of
a cubic crystal is related to the lattice parameter (a) as:
a
d (2)
h2  k 2  l 2

2. Determination of average crystallite size: Ideally, a Bragg diffraction peak

is a line without width. In reality, diffraction from a crystal produces a peak
with certain width. The peak width depends on the size of crystals. Peak
width is inversely related to crystal size. According to Debye-Scherrer, the
crystallite size D is calculated using,
0.9
D (3)
Cos

Where 𝛽 = peak broadening in radians, 𝜃 is Bragg’s angle, 𝜆 the X-ray

wavelength (1.54Ao)

The diffraction corresponding to most intense peak is selected to calculate

the average crystallite size.
3. If there are sharp peaks in the XRD-spectra, then the sample is crystalline
and if there is a broad bump, then the sample is amorphous. Thus XRD helps
us in identifying whether the sample is crystalline or amorphous.
4. One can identify the number of phases present along with their composition.
4.2 UV-Visible Spectroscopy:
UV region of electromagnetic radiation encompasses the wavelengths ranging
from ~10 nm – ~400 nm while visible region encompasses the wavelengths from
~400 nm to ~780 nm. The absorption of UV and visible light is through the
transition of an electron in the molecule from lower to a higher energy molecular
orbital.

4.2.1 Instrumentation:
Figure 5 below shows a schematic diagram of a double-beam spectrophotometer.
The light enters the instrument through an entrance slit, is collimated and focused
on to the dispersing element, typically a diffraction grating. The light of desired
wavelength is selected simply by rotating the monochromator and impinged on the
sample. The intensity of the radiation transmitted through the sample is measured
and converted to absorbance or transmittance. Double beam spectrophotometers
overcome certain limitations of the single beam spectrophotometers and are
therefore preferred over them. In a single beam spectrophotometer, all of the light
passes through the sample cell, Io must be measured by removing the sample cell.
A double beam spectrophotometer has two light beams, one of which passes
through the sample while other passes through a reference cell. One beam is used
as the reference; the other beam passes through the sample. Any fluctuation in the
light source or instrument electronics appears in both reference and the sample and
therefore can easily be removed from the sample spectrum by subtracting the
reference spectrum. Modern instruments can perform this subtraction
automatically. The most commonly used detectors in the UV-Visible
spectrophotometers are the photomultiplier tubes (PMT). Modern instruments also
use photodiodes as the detection systems.
Transmittance is another way of describing the absorption of light. Transmittance
(T) is simply the ratio of the intensity of the radiation transmitted through the
sample to that of the incident radiation. Transmittance is generally represented as
percentage transmittance (%T):

%𝑇= 𝐼/𝐼𝑜 × 100

Figure 5 Double beam spectrometer

4.2.2 Applications:

 Determination of molar absorption coefficient: From Beer-Lambert law,

A = εcl, it is straightforward to calculate the molar absorption coefficient of
a compound if the concentration of compound is accurately determined.
where A is the measured absorbance, ε is molar attenuation coefficient of the
compound, c is the amount concentration of the compound, l is the path
length of light through material sample.

 Quantification of compounds: If the molar absorption coefficient at a

wavelength is known for the compound, the concentration can easily be
estimated using Beer-Lambert law.
 Energy band gap: UV-Vis spectroscopy helps us to determine the energy
band gap of the material using the formula:
 (αhv)2 = Eg -hv (4)
where, α is the absorption coefficient of the material and v is the frequency
of incident radiation.
 Quality control: A given organic compound such as a drug can be studied
for its purity. Comparison of spectrum with the standard drug will detect the
impurities, if any. UV/Visible absorption is often used to detect the nucleic
acid contamination in the protein preparations.

4.3 Fourier Transform Infrared Spectroscopy:

Fourier-transform infrared spectroscopy (FTIR) is a technique used to obtain

an infrared spectrum of absorption or emission of a solid, liquid or gas. An FTIR
spectrometer simultaneously collects high-spectral-resolution data over a wide
spectral range. This confers a significant advantage over a dispersive spectrometer,
which measures intensity over a narrow range of wavelengths at a time.

The term Fourier-transform infrared spectroscopy originates from the fact that
a Fourier transform (a mathematical process) is required to convert the raw data
into the actual spectrum.

4.3.1 Components:
IR sources:

FTIR spectrometers are mostly used for measurements in the mid and near IR
regions. For the mid-IR region, 2−25 µm (5000–400 cm−1), the most common
source is a silicon carbide element heated to about 1200 K. The output is similar to
a blackbody. Shorter wavelengths of the near-IR, 1−2.5 µm (10000–4000 cm−1),
require a higher temperature source, typically a tungsten-halogen lamp. The long
wavelength output of these is limited to about 5 µm (2000 cm−1) by the absorption
of the quartz envelope. For the far-IR, especially at wavelengths beyond 50 µm
(200 cm−1) a mercury discharge lamp gives higher output than a thermal source.

Detectors:

Mid-IR spectrometers commonly use pyroelectric detectors that respond to

changes in temperature as the intensity of IR radiation falling on them varies. The
sensitive elements in these detectors are either deuterated triglycine sulfate
(DTGS) or lithium tantalate (LiTaO3). These detectors operate at ambient
temperatures and provide adequate sensitivity for most routine applications. To
achieve the best sensitivity the time for a scan is typically a few seconds. Cooled
photoelectric detectors are employed for situations requiring higher sensitivity or
faster response. Liquid nitrogen cooled mercury cadmium telluride (MCT)
detectors are the most widely used in the mid-IR. With these detectors an
interferogram can be measured in as little as 10 milliseconds. Uncooled indium
gallium arsenide photodiodes or DTGS are the usual choices in near-IR systems.
Very sensitive liquid-helium-cooled silicon or germanium bolometers are used in
the far-IR where both sources and beamsplitters are inefficient.

Beam splitter:

Simple interferometer with a beam-splitter and compensator plate. An ideal beam-

splitter transmits and reflects 50% of the incident radiation. However, as any
material has a limited range of optical transmittance, several beam-splitters may be
used interchangeably to cover a wide spectral range. For the mid-IR region, the
beamsplitter is usually made of KBr with a germanium-based coating that makes it
semi-reflective. KBr absorbs strongly at wavelengths beyond 25 μm (400 cm−1) so
CsI is sometimes used to extend the range to about 50 μm (200 cm−1).

ZnSe is an alternative where moisture vapor can be a problem but is limited to

about 20μm (500 cm−1).
CaF2 is the usual material for the near-IR, being both harder and less sensitive to
moisture than KBr but cannot be used beyond about 8 μm (1200 cm−1). In a simple
Michelson interferometer one beam passes twice through the beamsplitter but the
other passes through only once. To correct for this an additional compensator plate
of equal thickness is incorporated. Far-IR beamsplitters are mostly based on
polymer films and cover a limited wavelength range.

Attenuated total reflectance (ATR):

ATR is one accessory of FTIR spectrophotometer to measure surface properties of

solid or thin film samples rather than their bulk properties. Generally, ATR has a
penetration depth of around 1 or 2 micrometers depending on your sample
conditions.

Fourier transform

The interferogram in practice consists of a set of intensities measured for discrete

values of retardation. The difference between successive retardation values is
constant. Thus, a discrete Fourier transform is needed. The fast Fourier
transform (FFT) algorithm is used.

4.3.2 Applications:
FTIR can be used in all applications where a dispersive spectrometer was used in
the past. In addition, the improved sensitivity and speed have opened up new areas
of application. Spectra can be measured in situations where very little energy
reaches the detector and scan rates can exceed 50 spectra a second. Fourier
transform infrared spectroscopy is used in geology, chemistry, materials and
biology research fields.

Following are the few applications of Fourier Transform Infrared Spectroscopy-

  Biological materials

FTIR is used to investigate proteins in hydrophobic membrane environments.

Studies show the ability of FTIR to directly determine the polarity at a given site
along the backbone of a trans-membrane protein.

 Microscopy and imaging

An infrared microscope allows samples to be observed and spectra measured from

regions as small as 5 microns across. Images can be generated by combining a
microscope with linear or 2-D array detectors. The spatial resolution can approach
5 microns with tens of thousands of pixels. The images contain a spectrum for each
pixel and can be viewed as maps showing the intensity at any wavelength or
combination of wavelengths. This allows the distribution of different chemical
species within the sample to be seen. Typical studies include analysing tissue
sections as an alternative to conventional histopathology and examining the
homogeneity of pharmaceutical tablets.

 Nanoscale and spectroscopy below the diffraction limit

The spatial resolution of FTIR can be further improved below the micrometer scale
by integrating it into scanning near-field optical microscopy platform. The
corresponding technique is called nano-FTIR and allows for performing broadband
spectroscopy on materials in ultra-small quantities (single viruses and protein
complexes) and with 10 to 20 nm spatial resolution.

 FTIR as detector in chromatography

The speed of FTIR allows spectra to be obtained from compounds as they are
separated by a gas chromatograph. However, this technique is little used compared
to GC-MS (gas chromatography-mass spectrometry) which is more sensitive. The
GC-IR method is particularly useful for identifying isomers, which by their nature
have identical masses. Liquid chromatography fractions are more difficult because
of the solvent present. One notable exception is to measure chain branching as a
function of molecular size in polyethylene using gel permeation chromatography,
which is possible using chlorinated solvents that have no absorption in the area in
question.

 TG-IR (thermo gravimetric analysis-infrared spectrometry)

Measuring the gas evolved as a material is heated allows qualitative identification

of the species to complement the purely quantitative information provided by
measuring the weight loss.

5. EXPERIMENTAL WORK:
5.1. Synthesis of Magnetite Fe3O4 Nanoparticles by Sol-Gel
Technique
5.1.1: Iron oxide nanoparticles:

Iron oxide nanoparticles are composed of iron oxide particles of size 1–100 mm.
The two primary biocompatible forms of iron oxide are magnetite (Fe3O4) and the
oxide form maghemite (γ-Fe3O4). Magnetic fluids, data storage, catalysis, and
biomedical applications are some of the key applications. In biomedical
research, magnetic nanoparticles are applied in magnetic bio-separation, biological
detection, detoxification, immunoassays, hyperthermia, medical diagnosis, tissue
repair, tumor therapy, and targeted drug delivery. Iron oxide nanoparticles are
known to improve imaging contrast in magnetic resonance imaging (MRI).

Iron oxide nanoparticles tend to aggregate due to their large surface to volume ratio
exhibiting strong super-paramagnetic properties. Physiochemical properties such
as the particle size, distribution, and concentration are invaluable for adjusting the
optical and magnetic properties. Combinatorial therapies assisted by iron oxide
nanoparticles are indicated in cancer therapy. Fe3O4 nanoparticles can
provide targeted drug delivery and enhance imaging and therapeutic through high
localization at the target site under magnetic field. Synergistically these
nanoparticles also cause tumor cell death via localized hyperthermia under
alternating magnetic fields and/or photon application (with therapeutic agents) that
generates heat.

Multiple techniques are applied for the synthesis of magnetic nanoparticles.

Although coprecipitation of iron salts is the most common method, desired
sizerange and nonuniform distribution of the particle are some of the drawbacks .
Sonolysis, electrospray-synthesis, flow injection synthesis, polyol method, sol–
gel reaction, hydrothermal synthesis, and micro emulsions are just a few of
these techniques.

5.1.2 Synthesis using sol-gel technique:

4.8372 g of Ferric Nitrate was dissolved in 100 ml of distilled water to create 0.2M
solution. Also 0.79994 g (0.1M) of sodium hydroxide was dissolved in 100 ml of
distilled water. Then the ferric nitrate solution was added to sodium hydroxide
solution with vigorous stirring. The stirring was done on a magnetic stirrer for 5-6
hours until thick precipitate was formed. The precipitates were filtered and dried in
oven. The brown colored precipitates were then crushed into fine powder.
Calcination of magnetite particles was first done at 500℃ and then at 800℃.

5.2 Synthesis of PVA-Magnetite Nanocomposite

5.2.1 PVA: Polyvinyl alcohol (PVA) has attracted the attention of many
researchers due to its superior characteristics such as hydrophilicity,
biodegradability, biocompatibility, and non-toxicity. It is a nontoxic water soluble
polymer which has been used widely in different research areas including
membrane, biomedical, and drug delivery systems. It could be blended with
different polymers due to its high hydrophilicity and processability. PVA films
exhibit high tensile strength, abrasion resistance, and oxygen barrier properties
which are superior as compared to other polymers

5.2.2 Synthesis of PVA-Magnetite Nanocomposite

0.081 g of PVA was dissolved in 20 ml of distilled water. Then the magnetite

nanoparticles prepared were poured into the PVA solution and the resulting
solution was sonicated for about 2 hours. A homogeneous brown colored PVA-
Magnetite Nanocomposite solution was synthesized.

6. RESULTS AND DISCUSSION

 XRD of Magnetite Fe3O4 Nanoparticles

Figure 6 X ray spectra of the synthesized iron oxide particles

Figure 6 shows the X-Ray diffraction spectra of synthesized iron oxide
nanoparticles: magnetite (Fe2O3). The XRD pattern shows that the nanoparticles
are Fe2O3 magnetite nanoparticles having size 4.9 nm found with the help of
Scherrer’s formula (2) with observed peaks at the defined positions: 35.5⁰, 53.95⁰,
57.42⁰, 57.47⁰ and 63.8⁰ corresponding to (311), (422), (511), (511), (440)
crystalline planes of magnetite phase with corresponding inter planar distances 2.5
A⁰, 1.7 A⁰, 1.6 A⁰, 1.6 A⁰ and 1.4 A⁰.

 UV-Vis of Magnetite-Fe3O4 Nanoparticles

Figure 7 UV-Vis absorption spectra of magnetite-Fe3O4 nanoparticles

Figure 7 shows the absorbance curves of the magnetite nanoparticles. It displays

the onset of absorption maxima at 439 nm in the visible range between 400 nm to
600 nm.
 XRD of PVA-Magnetite Nanocomposite

Figure 8 X-Ray diffraction pattern of PVA-Magnetite Nanocomposite

 UV-Vis of PVA

Figure 9 UV-Vis absorption spectra of PVA

Figure 8 shows the X-Ray Spectra of PVA-Magnetite Nanocomposite with peaks
at 23.32⁰, 32.26⁰, 34.58⁰, 48.46⁰ and 53.1⁰. The peaks at 34.58⁰ and 53.1⁰
correspond to Fe3O4 nanoparticles while the peak at 23.32⁰ is that of PVA. So, the
resulting XRD pattern is a PVA-Magnetite Nanocomposite.

Figure 9 shows the UV-visible absorption spectra of PVA. The peak at 277 nm
belongs to the carbonyl groups. In addition, there is no observed peak in the 350-
600 nm range.

 UV-Vis of PVA-Magnetite Nanocomposite

Figure 10 UV-Vis absorption spectra of PVA-Magnetite Nanocomposite

Figure 10 shows the UV-Vis spectra of PVA-Magnetite Nanocomposite which

shows both the peaks of magnetite nanoparticles with the onset of absorption
maxima at 449 nm in the visible range between 400 nm to 600 nm and PVA at 272
nm indicating the presence of carbonyl groups and thereby confirming the
synthesis of the nanocomposite.
 FTIR of PVA
RC SAIF PU, Chandigarh

99.8

2153.2
838.2
95

1429.8
1713.8 1377.2 1093.9
90 2945.3 1264.2

1643.0

85

%T

80

75

70

3350.5
67.0
4000.0 3600 3200 2800 2400 2000 1800 1600 1400 1200 1000 800 650.0
cm-1
Navjot CNSNT-8.sp - 4/26/2019 - PVA
Figure 11 FTIR spectrum of PVA

 FTIR of PVA-Magnetite Nanocomposite

RC SAIF PU, Chandigarh

93.4
92
917.0
90
2153.9 846.9

88
1712.5
86 1376.4
1416.9 1262.8
84 1641.2 1092.3

2941.7
82

80
%T
78

76

74

72

70

68 3326.0
67.0
4000.0 3600 3200 2800 2400 2000 1800 1600 1400 1200 1000 800 650.0
cm-1

Navjot CNSNT-9.sp - 4/26/2019 - Nano

Figure 12 FTIR spectrum of PVA-Magnetite Nanocomposite
In Figure 11, all major peaks related to hydroxyl and acetate groups are shown in
the FTIR spectrum of PVA. More specifically, the broad band observed between
3550 and 3200 cm−1 is associated with the O-H stretch from the intermolecular and
intramolecular hydrogen bonds. The vibrational band observed between 2840 and
3000 cm−1 is the result of the C-H stretch from alkyl groups and the peaks between
1713 and 1643 cm−1 are due to the C=O and C-O stretches from the remaining
acetate groups in PVA

Figure 12 shows the FTIR spectrum of PVA-Magnetite Nanocomposite. The

peaks correspond to that of PVA and there is one small additional peak at 917 cm-1.
The peaks at 3326 cm-1 1641 cm-1 of Magnetite Nanoparticles coincides with the
peaks of PVA which indicate OH stretching mode.

7. CONCLUSION:
Iron Oxide (Fe3O4) nanoparticles have been synthesized and confirmed by XRD
and UV-Vis Results which gave well defined peaks and absorption maxima
respectively. Crystallite size was calculated from the most prominent diffraction
line and it came out to be 4.9 nm. Then the Magnetite-PVA nanocomposite was
synthesized whose XRD, UV-Vis, FTIR was done and its UV-Vis and FTIR
results were compared with that of pure PVA. XRD of the magnetite-PVA
nanocomposite contains both the peaks of magnetite and PVA. The peaks at 34.58⁰
and 53.1⁰ correspond to Fe3O4 nanoparticles while the peak at 23.32⁰ is that of
PVA. UV-Vis spectra of the synthesized nanocomposite incorporate the
absorption maxima of PVA at 277cm-1 and the absorption maxima of Magnetite
nanoparticles at 439 nm in the visible range between 400 nm to 600 nm. An FTIR
spectrum of the nanocomposite is similar to that of PVA with an additional peak at
917 cm-1. The peaks at 3326 cm-1 1641cm-1 of Magnetite Nanoparticles coincides
with the peaks of PVA which indicate OH stretching mode.
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