PROPERTIES OF NANO MATERIALS

 The properties of Nano Materials are very much different

from those at a larger scale.
 Two principal factors cause the properties of Nano
Materials to differ significantly from other materials.

1.Increased relative surface area.

2.Quantum confinement effect.

 These factors can charge or enhance properties such as

reactivity , strength and electrical characteristics
 Copper nanoparticles received much attention due to
its high electrical conductivity, high melting point, low
electrochemical migration behavior and low cost
Two Different Approaches to Nanofabrication

 Top ⇨ Down:

• Start with the bulk material and

“cut away material” to make the
what you want

 Bottom ⇨ Up:
• Building what you want by
assembling it from building blocks
( such as atoms and molecules).

• Atom-by-atom, molecule-by-
molecule, or cluster-by-cluster
INTRODUCTION

Non crystalline solid obtained by

freezing super cooled liquids.
The most common kind of glass is prepared from molten
SiO2 with various amounts of dissolved metal oxides.
Glass contains chains and rings involving Si-O bonds; the
structure is disordered and irregular; liquids that are very
viscous tend to form glasses when cooled rapidly.
The high viscosity makes it hard for the molecules to become
ordered into a crystalline solid
 THE SOL-GEL TECHNOLOGY

Transition of a system from a liquid “sol” (mostly colloidal) into a solid “gel”
phase.
 The technology incorporation of organic and inorganic additives during
the process of formation of the glassy network at room temperature. The sol
gel process involves chemical synthesis of oxides.
Possible to fabricate ceramic or glass materials in a wide variety of forms:
ultra fine or spherical shaped powders, thin film coating, ceramic fibers, micro
porous inorganic membranes, monolithic ceramics and glasses or extremely
porous aerogel materials.
SOL GEL
PROCESSING STEPS

Figure1.3 Processing steps of sol-gel processing

 ADVANTAGES OF SOL-GEL PROCESSING
Can easily shape materials into complex geometries in gel state

Can have low temperature sintering capability

Can produce high purity products

Can provide a simple, economic and effective method to

produce high quality materials.

Allows higher doping levels for rare-earth ions, transition metals

etc without the common clustering effect found in other glass
making techniques.
 EXPERIMENTAL
MATERIALS
 TEOS (tetraethyl orthosilicate)(Si(OC2H5)4
 Ethanol (C2H5OH)
 Copper nitrate tri hydrate (Cu(NO3)2.3H2O )
 Distilled water
 Nitric acid
Samples prepared by sol gel method
We prepared four types of sample with the following
compositions.
1.Sample 1. SiO2 (Matrix)
2.Sample 2.SiO2 + Cu (0.25wt%)
3.Sample 3.SiO2 + Cu (0.50wt%)
4.Sample 4.SiO2 + Cu (1wt%)

Sample photograph
 COPPER NANO : SiO2 GLASS SAMPLE
PREPARATION
TEOS ETOH

Stirring

Mixing with water

Stirring

Sol

Cast into polypropylene containers

and sealed using Parafilms

Drying Aging

Xerogel

800 0C Heating

SiO2 glass

Characterizations
 What is FTIR

 Fourier-transform infrared spectroscopy is a vibrational

spectroscopic technique, meaning it takes advantage of
asymmetric molecular stretching, vibration, and rotation
of chemical bonds as they are exposed to designated
wavelengths of light.
 Fourier transform is to transform the signal from the time
domain to its representation in the frequency domain
 CHARACTERISATIONS
ABSORPTION

Absorption Spectrum of copper nanoparticle doped SiO2

 PLASMONIC ABSORPTION

o The surface Plasmon peak has been observed in absorption spectra of

copper nanoparticle.

o Strong absorption peak observed around 320nm.

o The broad absorption peak observed is due to the collective oscillation of

all free electrons in the copper nanoparticles resulting from the interaction
with the electromagnetic radiation
 FOURIER TRANSFORM INFRARED SPECTROSCOPY
(FTIR)
FTIR spectrum of copper nanoparticle : SiO2 Matrix

• From the FTIR spectrum peaks have been observed at

3755.02cmˉˡ , 2297.18cmˉˡ ,1739.32cmˉˡ, 1368.36
cmˉˡ,1205.95 cmˉˡ,1076.43cmˉˡ, 1019.40
cmˉˡ,796.89cmˉˡ and 458.02cmˉˡ.
 FTIR ANALYSIS
The peaks at 3755.02 cmˉˡ due to the isolated free Si-O-H
(Silanol) stretching.
The observed peak at 1368.36 cmˉˡ corresponds to the H-C-
H bending.
The spectrum shows the presence of Si-O-Si asymmetric
stretching since the peak is observed at 1076.43 cmˉˡ.
The peak observed at 458.02 cmˉˡ corresponds to the Si-O-Si
symmetric stretching.
confirmed the presence of SiO2 bond formation, Si-O-Si
stretching and the formation of the glass.
Since the doped amount of copper nanoparticles is small
compared to SiO2, it is difficult to detect the stretching of
 Introduction
Motivation:
• X-ray diffraction is used to obtain structural
information about crystalline solids.
• Useful in biochemistry to solve the 3D structures of
complex biomolecules.
• Bridge the gaps between physics, chemistry, and
biology.

X-ray diffraction is important for:

• Solid-state physics
• Biophysics
• Medical physics
• Chemistry and Biochemistry

X-ray Diffractometer
 How Diffraction Works: Schematic

NaCl

http://mrsec.wisc.edu/edetc/modules/xray/X-raystm.pdf
X-RAY DIFFRACTION
(XRD)
XRD Analysis

In the diffraction

pattern, there is a broad
peak centered at 2Ɵ~23˚
which is characteristic
peak of amorphous SiO2
 A small characteristic
peak at 43˚ peak is due to
crystalline nature of
copper nanoparticles
 May be due to high
scanning speed the
copper crystalline peaks
are not seen clearly in the
XRD. So it is difficult to
calculate the FWHM
values. So for more
confirmation of copper
 TEM ANALYSIS

figure 1 shows the TEM image of Copper nanoparticles with a scale of 10 nm

 Figure 2 shows the HRTEM copper nanopartcile clearly seen the crystalline
planes of Copper nanoparticle with a scale of 2 nm
 The average size calculated fro TEM measureemnts ~ 15 nm
 Figure 3 shows the SEAD pattern. The circular pattern in the TEM image
confirmed the crystalline nature of the copper nanoparticle.
NANO SIZE CALCUALTION OF IMAGE J
PROGRAM

Using Image J program the size calculated ~ 15 nm