Project Report On Synthesis and Characterisation of Fe O - Pva Nanocomposite
Project Report On Synthesis and Characterisation of Fe O - Pva Nanocomposite
Project Report On Synthesis and Characterisation of Fe O - Pva Nanocomposite
AND CHARACTERISATION OF
Fe3O4-PVA NANOCOMPOSITE
SHREYA SHARMA
CONTENTS
1. Introduction
2. Nanoparticles
3. Nanocomposites
4. Characterization Techniques
5. Experimental Work
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.
2. NANOPARTICLES:
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 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.
2. Electrical conductivity
4. Thermal stability
5. Chemical resistance
6. Surface appearance
7. Optical clarity
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.
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:
Figure 2
4. CHARACTERISATION TECHNIQUES:
X-Ray source
Goniometer: the platform that holds and move the sample
Sample holder
Detector : to detect the scattered X-rays
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
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:
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):
4.2.2 Applications:
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:
Beam splitter:
Fourier transform
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.
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.
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.
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.
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℃.
5.2.1 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
UV-Vis of PVA
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.
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
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
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.
8.REFERENCES
[1] Ling Li, Maohong Fan, Robert C. Brown, and J. (Hans) Van Leeuwen;
Synthesis, Properties, and Environmental Applications of nanoscale IronBased
Materials: A Review (2006)
[2] Wei Wu, Zhaohui Wu, Taekyung Yu, Changzhong Jiang and Woo-Wik Kim;
Recent progress on magnetic iron oxide nanoparticles: synthesis, surface functional
strategies and biomedical applications (2015)
[4] Eunice Aparecida Campos, Denise Villela Barcza Stockler Pinto, Jose Irineu
Sampaio de Diveira, Elizabeth da Costa Mattos, Rita de Cassia Lazzarini Dutra;
Synthesis, Characterization and Applications of Iron Oxide Nanoparticles – a Short
Review
[15] Gupta AK and Gupta M. Synthesis and surface engineering of iron oxide
nanoparticles for biomedical applications. Biomaterials. 26(18) (2005)3995-4021
.