Nanoparticles

Introduction:
"A particle having one or more dimensions of the order of 100nm or less".
In nanotechnology, a particle is defined as a small object that behaves as a whole unit
in terms of its transport and properties. Particles are further classified according to size: in terms
of diameter, fine particles cover a range between 100 and 2500 nanometers. On the other hand,
ultrafine particles are sized between 1 and 100 nanometers. Similar to ultrafine particles,
nanoparticles are sized between 1 and 100 nanometers. Nanoparticles may or may not exhibit
size-related properties that differ significantly from those observed in fine particles or bulk
materials. Although the size of most molecules would fit into the above outline, individual
molecules are usually not referred to as nanoparticles.
Nanoclusters have at least one dimension between 1 and 10 nanometers and a narrow
size distribution. Nanopowders are agglomerates of ultrafine particles, nanoparticles, or
nanoclusters. Nanometer-sized single crystals, or single-domain ultrafine particles, are often
referred to as nanocrystals.
Nanoparticle research is currently an area of intense scientific interest due to a wide
variety of potential applications in biomedical, optical and electronic fields.

Synthesis of nanoparticles:

The synthesis and application of nanoparticles is one of the most interesting fields of
research from a basic and applied point of views. The method employed by our group is a
micellar method that could be easily scaled-up and allows the control of the composition and size
of the nanoparticle.
Many of these nanomaterials are made directly as dry powders, and it is a common
myth that these powders will stay in the same state when stored. In fact, they will rapidly
aggregate through a solid bridging mechanism in as little as a few seconds. Whether these
aggregates are detrimental will depend entirely on the application of the nanomaterial.

If the nanoparticles need to be kept separate, then they must be prepared and stored in
a liquid medium designed to facilitate sufficient interparticle repulsion forces to prevent
aggregation. Different process of synthesis of nanoparticles are as follow:

1. Synthesis of nanoparticles in microemulsion:

The use of water-in-oil microemulsions for the synthesis of nanoparticles is one of the
most promising methods. The application of this technology allows the preparation of the
nanoparticles. The microemulsion technology has been applied for the synthesis of pure metal
nanoparticles (Pt, Pd, Ir, Rh, Rh, Au, Ag, Cu) as well as for the preparation of the bimetallic
nanoparticles (Pt/Pd, Pt/Ru, Pt/Ir, Pt/Rh). The method can also be used for the synthesis of
multimetallic nanoparticles. In the case of bi and multimetallic nanoparticles the atomic
composition can be modified according with the needs.
Moreover, this methodology can be used for the preparation of different types of
nanoparticles such as SiO2, CdS, ZnS, ZrO2, CaCO3, BaCO3, CdSe, TiO2, etc.
The particle size of the nanoparticle ranges between 1-50 nm but is strongly dependent
of the surfactant employed. The main advantage of this method is the different compositions and
sizes that can be obtained.
The catalytic and electrocatalytic properties of the nanoparticles depend on the state
and cleanness of their surface. For that reason is very important to develop some
decontamination procedures able to clean the surface of the nanoparticles without
modifying the initial structure and surface composition of the nanoparticles. This
decontamination will allow the application of the nanoparticles with their complete catalytic or
electrocatalytic properties. In the Chemistry-Physics Department some decontamination
protocols able to obtain these requirements have been developed.

2. Synthesis of nanoparticles in colloidal systems:

The preparation of nanoparticles in colloidal systems is one of the most well known
methods for the synthesis of nanomaterials. Moreover, this methodology allows, in several cases,
synthesize nanoparticles with some preferential orientations/shapes and it is very well-known
that the shape of the nanoparticles influences their optical, electronic, catalytic and

electrocatalytic properties. This fact is specially important when the nanoparticles are going to be
applied in electrocatalytic or catalytic reactions which are sensitive to the structure of the
catalyst. The application of this method to electrocatalysis is a really innovative concept. The
main advantage of using this method is the possibility of controlling the shape of the particles.
The particle size of the nanoparticle ranges between 5-50 nm but again is strongly
dependent of the capping material employed. Thus, different shapes, with different properties,
can be prepared (cubics, tetrahedral, spherical, truncated octahedral).

Layer-by-layer assembly:
The layer-by-layer (LBL) assembly method, combined with the seeded growth
technique, has been used to deposit gold shells on the surface of hematite (-Fe2O3) spindles.
The LBL method yields dense coatings of preformed Au nanoparticles, while AuCl4 ions are
further reduced by a mild reducing agent, thicker, rough nanostructured shells can be grown.

Advantages of synthesis:

Customization of the process of synthesis, test, scale-up and technology transfer to the
company.

Use of decontaminated protocols for the cleaning of some particles.

Techniques appropriated for metallic, bimetallic and multimetallic particles.

Also applyable to other compounds as SiO2, CdS, ZnS, ZrO2, CaCO3, BaCO3, CdSe, TiO2,
etc.

Synthesis of Titanium dioxide Nano particles

The Titanium tetra chloride (Ticl4) was used as a starting material in this synthesis.50 ml of
TiCl4 was slowly added to the 200 ml distilled water in an ice cool bath. The beaker was taken
from the ice bath to Room temperature. The beaker was kept in magnetic stirrer to make a
homogeneous solution for 30 minutes. Bath temperature was raised to 150c and kept in the same
temperature till the process of nano particle was completed.

In another vessel 26 grams of Urea was dissolved in 250 ml of distilled water. From the vessel
150 ml of urea solution was added to beaker under constant stirring, drop by drop touching the
walls of the beaker. The solution turned into white colloid without any precipitation. After the
complete reaction, the solution was allowed to settle and the solution was washed with distilled
water for 5 times.

Characterization of Nanoparticles
Characterization of the nanoparticles was done by three tests such as X-ray Diffraction Method
(XRD) and Fourier Transform Infrared Spectroscopy (FTIR) and transmission electron
microscope.

The crystallinity was determined by XRD using a Bruker D8 Advance X rays

Diffractometer equipped with a Cu K ( =

1.54 A ) source (applied voltage 40 kV, current 40 mA). About 0.5 g of the dried particles were
deposited as a randomly oriented powder onto a Plexiglas sample container, and the XRD
patterns were recorded at angles between 20 and 80, with a scan rate of 1.5/min.
The crystallite domain diameters (D) were obtained from XRD peaks according to the
Scherers equation:
0.89

D =

-------------W Cos

Where is the wavelength of the incident X-ray beam (1.54 A for the Cu K), O is the
Braggs diffraction angle, W the width of the X-ray pattern line at half peak-height in radians.
The chemical composition of the synthesized materials was checked by FTIR spectroscopy with
a Bio-Rad FTS-40 spectrometer. The shape and size of the nano particles were obtained through
TEM, using a Philips EM201C apparatus operating at 80kv. The samples for TEM
measurements were placed on carbon-coated copper grids. The samples for TEM measurements
were prepared from much diluted dispersions of the particles in 2-propanol. Surface area
measurements were determined from BET on a Coulter SA 3100 surface area analyzer, under N2
flow.

Finishing Process
The woven and knitted fabric of 100% cotton and 45/55% polyester/cotton were applied with
Titanium dioxide nano particles by Spraying using spray gun and also Pad-Dry-Cure method.

Procedure
Nano particle were applied on the face side of the fabric with concentration 1%, Material to
liquor ratio1:20, Acrylic binder 1%. The 100% Cotton and 45/55% polyester/ cotton woven and
knitted fabric were cut to the size of 30 x 30 cm. These fabrics were coated with Titanium
dioxide nano particles by using a spray gun. A dispersion of nano particle was filled in the hand
spray gun. The fabric substrate was fixed on a vertical board. The nano particle solution was
evenly sprayed over the fabric by maintaining a constant distance between the fabric and spray
gun nozzle. The excess solution was squeezed using a padding mangle which was running at a
speed of 15 m/min with a pressure of 15 kg/cm2 after padding the fabric was dried naturally and
then cured for 3 minutes at 150C.

Characterization of nano particles using XRD, FTIR and TEM

The results shown in figure 4.1 & 4.2 indicate that the experimental conditions greatly affect the
morphology and size of the articles, prepared with the different condition. In fact, increasing the
reaction temperature, results in a significant lowering of the nanoparticles size and of their
agglomeration number D, calculated as
0.89
D=

-------------W Cos

TEM size distributions were obtained for nano particles, as shown in Figure 4.3. The mean
crystallite size is presented in Table 4.1.

Figure 4.1: X ray diffraction report of Titanium dioxide nano particle

Figure 4.2: Fourier Transform Infrared Spectroscopy of Titanium dioxide nano particle

Figure 4.3: TEM image of Titanium dioxide nano particle

CONCLUSIONS
Tio2 nano particles were synthesized and characterized using XRD, FTIR, TEM and SEM. It is
shown that the nano-Tio2 impregnated onto woven and knitted textiles showed excellent
antibacterial activity against two representative bacteria, Staphylococcus aureus and Klebsiella
pneumoniae. This work provides a simple method for aqueous preparation of Tio2 nano
composites and their application onto 100% cotton & 45/55% polyester/cotton fabrics to impart
antibacterial function.