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Surface Sol – Gel synthesis of Cadmium Sulfide fine particles in silica matrix

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 Journal of Research in Nanobiotechnology
Journal of Research in Nanobiotechnology
An International Online Open Access
Original Research Publication group

Surface Sol – Gel synthesis of Cadmium Sulfide fine

particles in silica matrix

Authors: ABSTRACT:
Yesu Thangam Y and
Anitha R. A simple and novel method was proposed for the preparation of CdS
semiconductor nanoparticles with controllable size and stability in silica matrix using
sol-gel method at room temperature. Cadmium sulfide nanoparticles have been
synthesized using respective metal precursors and Tetraethylorthosilicate (TEOS) as a
Institution:
Department of Chemistry, source of silica matrix. Formations of nanoparticles were characterized using UV-Vis
Jayaraj Annapackiam Spectrophotometer, Fourier-Transform Infrared Spectroscopy (FTIR), X-ray Diffraction
College for Women (XRD) and Scanning Electron Microscopy (SEM). The UV absorption analysis of the
(Autonomous), Periyakulam, sample showed the optical absorption edge that exhibited a blue shift with respect to
Tamil Nadu. that of bulk samples. Determination of size and composition observed from X-ray
diffraction pattern have shown that nanoparticle size is 4nm approximately and the
estimated band gap was calculated as 2.82 eV whereas the band gap for bulk CdS is
2.42 eV. Scanning electron microscopy was used for characterization of microstructure
and surface properties of synthesized CdS particles. This method would be utilized for
Corresponding author: the preparation of various nanoparticles because of its simplicity and low cost as well
Yesu Thangam Y. as the better quality of production.

Email: Keywords:
[email protected] Silica matrix, sol-gel method, TEOS, FTIR, band gap, CdS nanoparticles.

Web Address: Article Citation:

http://jresearchbiology.com/ Yesu Thangam Y and Anitha R.
documents/NB0003.pdf. Surface Sol – Gel synthesis of Cadmium Sulfide fine particles in silica matrix.
Journal of Research in Nanobiotechnology (2012) 1(1): 014-018

Dates:
Received: 21 Jun 2012 Accepted: 28 Jun 2012 Published: 11 Jul 2012

© Ficus Publishers.
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 Thangam and Anitha, 2012

INTRODUCTION nonlinear optical, photo electrochemical cells and

Semiconductor nanoparticles have been heterogeneous photo catalysis (Hu et al., 1998).
investigated over the past years due to their specific CdS (with Eg = 2.42 eV at room temperature) has
optical, electronic and catalytic properties. These promising applications in multiple fields including
properties emerge from the high surface-to-volume ratio mechanical, optoelectronic, photo degradation of water
present in nanoparticles (Martinez-Castanon et al., pollutants and hydrogen generation by visible light
2005). It has been appreciated that size dependent (Lakshmikvamar and Rastogi 1994). Cadmium sulphide
properties in semiconductor materials are possible as the (CdS) has excellent visible light detecting
particle size approaches the Bohr radius of exciton. properties among the others semiconductors
This requirement is basically attributed to the (El- Bially AB et al., 2012). Therefore preparation of
confinement of charged particles within the CdS nanoparticles has been a very popular research area
small volume of the particle and is known in recent years. In this paper, we report a low
as the quantum confinement effect (QCE) or temperature, cost effective and simple route to obtain
quantum size effect (QSE) (Alivisatos, 1996). larger quantity of CdS nanoparticles loaded
The semiconductor nanoparticles within the dimension in silica matrix.
of Bohr radius exhibit strong size dependent properties.
Such particles may lead to quantum dot lasers, single Particle Size 2.88nm
electron transistors and also have biological applications
Absorbance

(Yin et al., 1998 and Chan and Nie, 1998).

The nanomaterials of size below 100 nm show
unique electrical and chemical properties because of a
large surface area per unit mass and potentially high
surface reactivity making them highly desirable for
industrial applications (Bhaben Tanti et al., 2012).
It is essential to synthesize semiconductor nanoparticles Wavelength nm
not only with a narrow size distribution but also with Figure 1 UV-Vis Spectrum of Cadmium Sulfide
good thermal stability. In many cases semiconductor Nanoparticle.
nanoparticles are synthesized in polymers, using the
chemical capping method or by embedding them in an 35

inert matrix. Such a matrix is useful in avoiding the

30
coalescence of the nanoparticles (Vogel et al., 1997).
Transmittance
Transmittance

939.33
Chemical capping of organic molecules provided
25
chemical stability up to ~300°C. However, beyond this
623.03
temperature the particle coalesce (Vogel et al., 2000). 20
1001.05 1323.16

Therefore CdS nanoparticles in a silica matrix have been 651.93

synthesized using a simple and inexpensive procedure. 15

1400.32
CdS is an important II-IV semiconductor owing 600 800 1000 1200 1400
to its unique electronic and optical properties, and its Wavenumber
Wavenumber cmcm-1
-1

potential applications in solar energy conversion, Figure 2 FTIR Spectrum of CdS Nanoparticle.
015 Journal of Research in Nanobiotechnology (2012) 1(1): 014-018
Thangam and Anitha, 2012

Na2S of required molarity was added and the solution

120
(111) was vigorously stirred for approximately ninety minutes.
The solution was then transferred to the glass vials for
100
gelation. Gelation occurred within an hour. Samples
Intensity(arb.units)

80 were left in glass vials at room temperature for drying.

(220)
(311) The gels were completely dried in seven days and
60
opaque samples of cadmium sulfide embedded in a silica
40
matrix were obtained. The samples without Cadmium

20
Sulfide were transparent but transparency reduced with
increasing Cadmium Sulfide content. The samples were
0
10 20 30 40 50 60 70 quite hard and handleable (Hebalkar et al., 2001).
2 Theta (Degrees) Characterization
The UV-Vis spectra of synthesized CdS
Figure 3 XRD Analysis of CdS Nanoparticle.
samples were recorded by using UV-1800 Shimadzu
EXPERIMENTAL automatic recording double beam spectrophotometer in
Chemicals the range of 200 - 800 nm. Samples for FTIR analysis
Tetraethyl orthosilicate (TEOS), Ethanol, were prepared in the form of pellets. Powder samples of
H2O, HCl, Cadmium acetate and Sodium sulfide. nanoparticles were mixed with KBr powder and pellets
Synthesis were formed. Shimadzu Fourier Transform Infrared
CdS nanoparticles were synthesized by sol–gel Spectrometer (IR Affinity-1) was used to record the
method as follows. Hydrolysis of tetraethylortho silicate spectra. Powder X - ray diffraction patterns of the CdS
(TEOS) was carried out by adding, TEOS: Ethanol: samples were taken using Rigaku miniflex (II) desktop
H2O: HCl in 1: 4: 4: 0 .068 molar ratios.The solution was X-ray diffractometer using a Cu Kα radiation (λ=1.5405
stirred thoroughly for thirty minutes at room Ǻ) source, with Ni filter. The surface morphology of the
temperature. Cadmium acetate of required molarity was CdS particles was obtained using a JEOL model 6390
then added and the solution was stirred again. Finally Scanning Electron Microscope.

Figure 4 (a) SEM image of CdS Nanoparticle in low Figure 4 (b) SEM image of CdS Nanoparticle in high
magnification. magnification.

Journal of Research in Nanobiotechnology (2012) 1(1): 014-018 016

 Thangam and Anitha, 2012

RESULTS AND DISCUSSION of the CdS nanoparticle is calculated as 4nm and the
UV spectrometric analysis showed that as band gap as 2.82eV.
particle size reduces below the Bohr size of exciton, the The surface morphology of the Cadmium Sulfide
energy gap increases and can be observed as shift in the was studied by using SEM images. Inset of
absorption edge (Bangal et al., 2005). The optical figure 4 (a and b) shows the surface morphology of
absorption edge exhibited a blue shift with respect to that CdS nanoparticles at low and high magnification
of bulk samples. The blue shift with the decrease in respectively. The nanosized CdS particles form globular
crystalline size was attributed to the quantum size effects aggregates of microdimensions. These aggregates are
(Xu et al., 1998). From figure 1, the absorption spectrum almost similar throughout indicating uniform particle
was found to be well shifted from their bulk value of dimension (shape and size). However, in high
4.03eV. CdS was prepared using TEOS, the particle size magnification, some smooth rod like structures are
was only 2.88nm. The absorption peak for CdS was observed due to very close packing of the
observed at 308nm. It is noticed that with increasing CdS nanoparticles.
loading, the position of the excitonic peak does not shift.
This implies that the particles do not coalesce as the CONCLUSION
CdS loading increases. This is because all the particles Highly stable nanoparticles of CdS in silica have
are covered with silica and retain their small sizes. been synthesized. It was possible to load the silica with
The FT-IR spectral studies shows that the various amounts of CdS without changing the particle
stretching frequencies for cadmium sulfide appeared at size. The stability of CdS in this matrix is good.
-1
623.03 cm matched the reported values The FT-IR and UV-spectrometric results confirmed that
(Aneeqa Sabah et al., 2010). The stretching frequencies the particles were nanometric in size. X-ray diffraction
corresponds to TEOS was 1000-1500 cm-1. The FT-IR pattern (XRD) reveals cubic phase structure and
spectrum is given in figure 2 Scanning electron microscopy (SEM) showed the rod
The XRD patterns of the synthesized shaped morphology of prepared CdS nanoparticles.
CdS nanoparticles were shown in figure 3. The three This method is an easy low cost synthetic route to
peaks with 2Ө values of 26.514°, 43.762° and 52.0° synthesis CdS nanoparticles at room temperature. This
corresponds to the three crystalline planes of (111), (220) method is also applicable to synthesize other
and (311) of cubic-phase β-CdS. The broadness of semiconductor materials.
the peaks indicates that the dimensions of the
CdS nanoparticles are very small. XRD analysis of the REFERENCES
samples shows that silica has an amorphous network and Alivisatos AP. 1996. Nanoparticles, Journal of
the crystallanity of the CdS-Silica composites is phys.chem, 100:13226.
apparent. The average size of grains has been
Aneeqa Sabah, Saadat Anwar Siddiqi, Salamat Ali.
obtained from the X - ray diffraction pattern using the
2010. Fabrication and Characterization of CdS
Scherrer’s formula
Nanoparticles Annealed by using different Radiations,
D = Kλ/β cos Ө
World Academy of Science, Engineering and
Where, D is the grain size, K is a constant taken
Technology, 69:82-89.
to be 0.94, β is the full width at half maximum (FWHM)
and λ is the wave length of the x-rays. The particle size

017 Journal of Research in Nanobiotechnology (2012) 1(1): 014-018

 Thangam and Anitha, 2012

Bangal M, Ashtaputre S, Marathe S, Ethiraj AS. Vogel W, Urban J, Kundu M. 1997. Surface Chemistry
2005. Semiconductor Nanoparticles, Hyperfine controls crystallinity of ZnS nanoparticles, Langumuir,
Interactions, 160:81-94. 13:827.

Bhaben Tanti, Ajoy Kumar Das, Hemen Kakati and Xu J, Ji FW, Lin JY, Tang SH. 1998. Preparation of
Devasish Chowdhury. 2012. Cytotoxic effect of ZnS Nanoparticles by ultrasonic radiation method,
silver-nanoparticles on root meristem of Allium sativum Applied Physics, A66(6):639-641.
L. Journal of Research in Nanobiotechnology,
Yin Y, Ling X, Ge X, Xia C and Zhang Z. 1998.
1:001-008.
Synthesis of cadmium sulfide nanoparticles in situ using
Chan WCW and Nie SM. 1998. Quantum dot γ-radiation, Chem. Commun, 16:1641.
bioconjugates for ultrasensitive nonisotopic detection.
Science, 281: 2016.

El- Bially AB, Seoudi R, Eisa W, Shabaka AA,

Soliman SI, Abd El-Hamid RK and Ramadan RA.
2012. Preparation, Characterization and Physical
Properties of CdS Nanoparticles with different
Sizes,Journal of Applied Sciences Research,
8(2):676-685.

Hebalkar N, Lobo A, Kulkarni SK. 2001. Properties of

zinc sulphide nanoparticles stabilized in silica, Journal of
Material Science, 36:4377-4384.

Hu, Brust M, Bard AJ. 1998. Photoelectrochemical

Cell and Its Applications in Optoelectronics, Chem.
Mater, 10:1160.

Lakshmikvamar ST, Rastogi AC. 1994. Simple and

Low Temperature Preparation and Characterization of
CdS Nanoparticles as a Highly Efficient Photocatalyst in
Presence of a Low-Cost Ionic Liquid Sol.Energy Mater.,
Sol. Cells, 32:7. Submit your articles online at Ficuspublishers.com
Advantages
Martinez-Castanon GA, Sanchez-Loredo MG, Easy online submission
Azojomo. 2005. Synthesis of CdS Nanoparticles: a Complete Peer review
Affordable Charges
Simple Method in Aqueous Media The Azo Journal of Quick processing
Materials Online, 1:2-7. Extensive indexing
Open Access and Quick spreading
Vogel W, Borse PH, Deshmukh N. 2000. Properties of You retains your copyright
zinc sulphide nanoparticles stabilized in silica, ibid, [email protected]
www.ficuspublishers.com/submit1.php.
16:2032.

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