World Journal of Pharmaceutical Research
Maruthamuthu et al.
World Journal of Pharmaceutical
Research
SJIF Impact Factor 5.045
Volume 4, Issue 01, 710-720.
Research Article
ISSN 2277– 7105
MICROWAVE SYNTHESIS, CHARACTERIZATION AND
BIOLOGICAL ACTIVITIES OF CuS AND CdS NANO PARTICLES
S. Priscilla Prabhavathi, Ranjith, Shameela Rajam,*Maruthamuthu, Johnson.T
PG & Research Department of Chemistry, Bishop Heber College (Autonomous),
Tiruchirapalli,-620 017, Tamilnadu, India.
Article Received on
17 October 2014,
Revised on 11 Nov 2014,
Accepted on 05 Dec 2014
ABSTRACT
The emerging need of CuS and Transition metal sulfides have
numerous applications in various fields made its synthesis needful and
meaning full. In recent years there is increasing interest in
*Correspondence for
semiconductor nano crystals due to their novel physical and chemical
Author
properties. Most of these sulfides are crystalline and exhibit high
Maruthamuthu
lubricities. These features make these sulfides a far better photo-
PG & Research
Department of
luminescent material as compared to oxides. Many sulfides exhibit
Chemistry, Bishop Heber
semi-metallic behavior with respect to the ability to form multiple
College (Autonomous),
oxidation states, thus they are applicable in microelectronics as
Tiruchirapalli,-620 017,
semiconductor materials.The emerging need of Cd and CdS
Tamilnadu, India.
nanoparticles in the medicine and many other fields made its synthesis
needful and meaning full. For example CdS is an important semiconductor and has many
optoelectronic applications including Solar cells, photodiodes, light emitting diodes,
nonlinear optics and heterogeneous photo catalysis. In the present study we have synthesized
CdS nanoparticles of chemical precipitation technique. CdS is an important inorganic
material for light-emitting applications. The literature survey showed that there are numerous
methods to prepare Cadmium Sulfide (CdS) nanoparticles. To our knowledge, there is no
report of synthesis of Cadmium sulfide nanoparticles by using SLS as a capping agent. So we
have planned to synthesis the CdS nanoparticles by using SLS as a capping agent and to
characterize the product by various analytical methods. Such The particles are characterized
using FTIR, XRD, SEM, and Antimicrobial activity.
KEYWORDS: Sulfides, Microwave, FT-IR, XRD, SEM, Anti-microbial activity.
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INTRODUCTION
Recently, much attention has been paid to one-dimensional inorganic (1D) nano structures
due to their unique optical. [1] electric and magnetic properties [2] and potential applications in
nano devices. Many methods have been used to prepare nanorods, nanowires, and nanofibers,
such as vapour liquid solid.
[3]
microwave route.
[4]
Particularly, low-molecular-weight
gelators as the template for fabrication of such nanomaterial’s (nanorods, nanowires, and
nanofibers) have attracted increasing interest since the most organogelations or hydrogel
could self-assemble into different nanoscale super structures, such as fibers, nanotubes,
ribbons, through weak non-covalent interactions (H-bonding, π-π interaction, coordination)
[5]with
controlled size, shape, organization and porosity, have been generated template by the
organogels.
[6]
It was well known that inorganic metal salts were the most convenient and
economic inorganic precursors in the mineralization, but it was difficult to introduce metal
salts into organogels system due to their poor solubility in most organic solvents, such as
chloroform, benzene, and cyclohexane, in which it was easy to form gels for
organogelators.[7] Therefore, it promoted us to use hydrogels instead of organogels as
template to mineralize the metal ions. Up to date, few inorganic nanostructures such as
semiconductor nanomaterials have been prepared based on microwaves synthesis. [8] FT-IR
spectra revealed that H-bonding was the main driving forces for the formation of the
hydrogel. Meanwhile, the CuS nano ribbons were firstly fabricated directed by the
microwaves synthesis.
[9]
CdS is an n-type semiconductor with band gap energy of 2.4 eV.
Among the II–VI semiconductors, CdS is of special interest because it has great potential
applications in photocatalys is and optoelectronic devices because of its high photosensitivity
coupled with the ability to tune the emission in the visible light range with different crystal
structures, sizes and shapes.
[10]
Cadmium sulfide (CdS) has the thermodynamic potential to
drive water splitting in to hydrogen and oxygen with visible light illumination. The bulkphase hexagonal CdS when compared to bulk-phase cubic CdS suspensions. In this way, it is
important to develop synthesis methods that are capable to obtain CdS in pure hexagonal
phase with sizes and shapes suitable for photo catalytic proposals. There are different
methods used to synthesize CdS, such as solvothermal synthesis.
[11]
hydrothermal process
microwave irradiation, sonochemistry process and sonochemistry-assisted microwave.
[12]
In
general, cubic-phase CdS has been obtained by the method that uses low temperatures and, in
these cases, it is possible to obtain quantum-sized particles. In contrast, hexagonal-phase
CdS. However, microwave methods usually yield CdS in hexagonal phase, probably due to
the high temperatures and pressures produced bubbles. Microwave uses high power ultrawww.wjpr.net
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sonic waves (20W to 900W) to promote chemical reactions.
[13]
and has been successfully
applied in the synthesis of new materials, since they provide smaller particle size and higher
surface area than reported by other methods. The advantages of microwave methods are high
intensity of waves, controllable reaction conditions, capacity to form uniform shapes, narrow
distributions of particle size and high purity. Ghowsetal. Applied a microwave method to
prepare hexagonal and/or cubic CdS and concluded that the crystal structure is governed by
the kind of cadmium salt solution used in the preparation of the sample, besides the
microwaves intensity and kind of solvent. In the present work, we used a microwave method
to prepare CdS using CdCl2 and Na2S2O3 as the precursors for preparing nanoparticles of CdS
in unique hexagonal phase with high morphological homogeneity. Besides, we evaluated the
influence of different CdS ratios in the quality and size of the nanoparticles and the
possibility of tuning the emission of visible light with the different synthesis conditions.The
chemistry and pharmacology of sulfide nanoparticles have been of great interest to medicinal
chemistry because its sulfide nanoparticles possessed various biological activitiessuch as
anticancer antihypertensive antimicrobial anti-HIV.
[14]
etc. In the presentStudy is it planned
to synthesize sulfide nanoparticles and characterize these compounds by IR, SEM, and XRD
spectral analysis. Since these compounds contain highly biological active nucleussulfide
nanoparticles, it is also aimed at carrying out anti-microbial activity.
MATERIALS AND METHODS
All melting points were taken in open capillaries and are uncorrected.IR spectra were
recorded in KBr on Shimadzu spectrometer. The microorganisms for anti-microbial activity
were obtained from National Chemical Laboratory, Pune.
COMPOUND-1 (CuS)
Synthesis of Copper sulfide nanoparticles using SLS
All chemicals used in this work were analytical reagent grade from commercial
marketwithout further purification 1.52g(0.02mol)Thiourea and 0.06g SLS (Sodium lauryl
sulfate) in 25ml solution 0.5M cupric chloride were dissolved under vigorous stirring and
heat to 333K for 15 min. The result suspension was put in a domestic microwave device for 3
min with power 450 W. After cooling to room temperature naturally, and centrifuged, the
precipitate was washed with distilled water and ethanol and then dried at 800 C for 4 hours.
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COMPOUND-2 (CdS)
Synthesis of Cadmium Sulfide nanoparticles using SLS
1.52g (0.02mol) Thiourea and 0.06g SLS (Sodium Lauryl Sulfate) in 25ml solution. 0.5M
Cadmium Carbonate were dissolve under vigorous stirring and heat to 333K for 15min. The
result suspension was put in a domestic microwave device for 3 min with power 450W. After
cooling to room temperature naturally, and centrifuged, the precipitate was washed with
distilled water and ethanol and then dried at 800 C for 4hours.
IR SPECTRAL DATA
The FT-IR spectrum of our compound is shown in Spectrum CdS & CuS. The FT-IR
spectrum of our compound also confirmed the formation of these nanoparticles.
Spectrum CdS& CuS
Analyzing the FTIR spectra of CdS nanoparticles, prepared for different molarities and
environment were almost similar there is negligible shifting in absorption peaks of all spectra.
Hence only one FTIR spectra is shown in Fig 3. One can observe many absorption bands,
which are given in Table I.
The very weak absorption bands at 3383.14 cm-1 is assigned to O-H stretching vibration of
water molecules, due to presence of moisture in the sample. CdS particles showed two
stretching bands, asymmetric and symmetric, around 2926.01 cm-1 and 2854.65 cm-1 are
associated with C-H stretching (Tang et al 2005). There are medium to strong absorption
bands at 613 cm-1 and 723 cm-1(closely related to band positions 669.0 cm-1 and 718.9 cm1have been assigned to Cd-S stretching by Periasamy et al1997), possibly due to Cd-S
stretching.
Table.1 CdS
S. No.
1
2
3
Positions (Cm-1)
3000-3600
1600-1400
700-500
Intensities
Medium
Weak
Medium
Assignments
Stretching
Bending
Stretching
Hence the existences of above mentioned bands identify the presence of CdS and alsothe
impurities that the samples consisted of water molecules or hydroxide ions. The IR spectrum
present one large band which is characteristic CuS and absorption peak of OH located at
3483.44cm-1. This shape of spectrum showed that there are no impurities. Which could be
detected in the sample. This results indicates the interaction between –OH group and CdS &
CuS nanoparticles.
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Table.2 CuS
S. No
1
2
3
Positions (Cm-1)
3300-3500
1080-1360
1600
Intensities
Medium
Medium-weak
Medium
Assignments
Stretching
Stretching
Bending
RESULT AND DISCUSSION
CdS, CuS Nanoparticles are prepared from CdCO3, CuCl2. Ethanol as a solvent and SLS as a
capping agent. Our reaction yielded yellow and black colored solid product. We carried out
basic analytical methods like FT-IR to identify our product. Powder XRD and SEM
analytical methods are used to identify particle size and morphology. [15]
Powder XRD Analysis of CdS
Structural studies were carried by Powder X-ray diffraction.Thepowder XRD patterns were
recorded in a Rigaku Powder X-ray diffractometer.The size of the nanoparticle is determined
from XRDpatterns by using Debye - Scherer formula, According to this equation:
D =Kλ/βcosθ
Where, λ is the wavelength of Cu Kα radiation (λ=1.5406), β the full width at half maximum
intensity, θ is the diffraction angle of the considered diffraction peak and K is a Scherer
constant taken as 0.90 for the almost spherical particles.
Spectrum IIIA
The recorded powder XRD spectrum of our CdS nanoparticles is shown in Spectrum. The
calculated average sizes of CdSnanoparticles are in the range from 24 to 54nm. The sizes are
given against each pattern in figure. The three peaks with 2θ values of 25.12, 43.80, 52.01
and particle range respectively 54.26, 53.5, 44.19 and 24.35nm for samples correspond tothe
XRD patterns of the CdS sample can be exhibit a single sphalerite crystal structure.
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Fig 1: XRD pattern of CdS nanoparticle.
Fig.2SEM images of CdS.
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Spectrum IIIB
The recorded powder XRD spectrum of our CdS nanoparticles is shown in Spectrum IIIA.
The calculated average sizes of CdSnanoparticles are in the range from 13 to 101nm. The
sizes are given against each pattern in figure. The three peaks with 2θ values of 10.3, 23.8,
0.3 and its range respectively 79.77, 30.07, 101.57, 13.07nm for sample correspond tothe
XRD patterns of the CdS sample can be exhibit a single sphalerite crystal structure.
5.0e+003
Intensity (cps)
4.0e+003
3.0e+003
2.0e+003
Integrated Intensity (cps deg)
1.0e+003
0.0e+000
20
40
60
80
20
40
60
80
6.0e+003
4.0e+003
2.0e+003
0.0e+000
2-theta (deg)
Fig.3 XRD pattern of CuS nanoparticle.
Fig.4XRD pattern of CuS nanoparticle.
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Fig.5 SEM images of CuS.
Antimicrobial study
The purified compounds A, &B, were tested for their antimicrobial activity against,
Escherichia coli, Enterobacter, Proteus & klebsiella.
Fig. 6 Anti Microbial Activty Images of Cds.
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Fig.7: Anti Microbial Activty Images of Cus.
Table 3: Anti-microbial activity of different chemical compound preparation against
pathogenic.
Ref No: BHC-BT-CTS03/2014/TJCdS& CuS
Name of the bacteria
E.coli
Proteus
Enterobacter
Klebsiella
Mean zone of
Sample 1
(CdS)
13.00
10.00
12.00
12.00
inhibition in mm
Sample 2
(CuS)
15.00
13.00
12.00
14.00
The Antimicrobial activity of the given SAMPLE against the above Microorganisms has been
recorded as per the zone of inhibition formation. The results indicates that the sample 1 is
more Effective forE.coli when compare with other organisms such as Enterobacter, Proteus
& klebsiella.
CONCLUSION
CdS and CuS Nanoparticles are prepared by using CuCl2 and CdCO3 and sodium Louryl
sulphate as a capping agent in ethanol medium, respectively. The shifting values of N-H
stretching, N-H Bending and C-H Bending in FT-IR Spectrum of compound-1 CuS conforms
the capping of SLS. The size of the nanoparticles of compound-1 is measured by the powder
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XRD analysis.The shifting values of N-H stretching and bending, C-H bending in FT-IR
Spectrum of compound-2 conforms the capping of SLS. The size of the nanoparticles of
compound-2 is measured by powder XRD analysis, which is in range between 25nm. SEM
analysis of the compound-2 also confirms to the formation of CdS nanoparticles.The test
organisms used in the study were E.coli, Proteus, Enterobacter & Klebsiella the entire test
cultures were obtained. The cultures were maintained at 4°c on Nutrient agar.The
antibacterial of the selected sample preparations were performed by agar well diffusion
method. 20ml of sterile Muller Hinton agar (Hi Media) was poured in sterile Petri dishes. The
plates was allowed to solidify and used. 10ml of sterile, Muller Hinton agar medium (seed
agar) was seeded with organism (about 0.2ml according to 0.5 McFarland’s standard), in
semi hot conditions and was poured uniformly on the base agar. 8mm bores were made each
equal distant from one another on the medium using sterile borer and 100µl of the different
urine preparation were added to respective bore. The plates were incubated at 37°C for 24 hrs
and zone of inhibition was measured. A reference standard of streptomycin (100µg/ml) was
also used to compare with the obtained results in the study. For each test, three replicates
were performed.
ACKNOWLEDGEMENT
The authors thank the Principal, Management and PG & Research Department of Chemistry,
Bishop Heber College, for the facilities provided to carry out this work.
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