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SYNTHESIS AND CHARACTERIZATION OF
CADMIUM SULPHIDE NANOPARTICLES
BY –ANJNEYA VERMA
Introduction:
Wayne Shenton, Dietmar Pum, Uwe B. Sleytr and Stephen Mann were the first to
synthesis cadmium sulphide nanoparticles by biological method.
The cadmium sulfide is an important II-IV group element semiconductor
(Eg=2.42eV (515nm) at room temperature) with many excellent physical and
chemical properties.
This has promising application in multiple technical fields including
photochemical catalysis, gas sensor, detectors for laser and infrared
Cadmium sulfide is a solid hexagonal or cubic crystal.
Cadmium sulfide is an important n-type semiconductor with a direct band gap
2.42eV., the photoconduction and electroluminescent properties of cadmium
sulfide have been applied in manufacturing a verity of consumer goods.
Green synthesis of CdS Nanoparticles using bacteria:
Bacterial strains of Enterobacteriaceae is used as a potential producer for green synthesis of
CdS nanoparticles.
Bacterial strains were inoculated in BHI broth under sterile conditions and incubated at 37ºC.
The strains vaccinate in Nutrient Agar, EMB Agar and Endo Mediums.
Bacterial suspension was used for this method.
Suspension was vaccinated in Nutrient broth and incubated at 37ºC for 24h for growing of
bacteria.
Then, the suspension were centrifuged at 5000 rpm for 15 min at room temperature and
resulting supernatants were extracted for further processing.
The obtained supernatants were washed with phosphate buffer saline (pH7.0) for 3 times.
1mM solution of CdCl2 (for E. coli) or CdSO4 (for K. pneumoniae) was prepared using deionized
water. 35 ml of the solution was added to supernatants and resulting solution was kept for
incubation in a shaker at 220 rpm and room temperature for 30 min.
Then, 35 ml of 1mM Na2S solution was slowly added to the solution.
The samples were then incubated at room temperature with end over en rotation for 10 min.
Effect of pH and Temperature on nanoparticles synthesis : To find the conditions
under which maximum amount of nanoparticles were synthesized, 1mM
concentration of CdCl2 or CdSO4 and Na2S were added to the solution containing
biomass and incubated in different pH conditions (5–11) and different
temperatures.
The pH of the incubation mixtures was adjusted using 1M HCl and 1M NaOH
solutions.
It was concluded that the optimum condition for synthesis of nanoparticles is
temperature of 30ºC and pH of 9.
Effect of CdCl2 or CdSo4 and Na2S on the nanoparticles synthesis :
The study was carried out by adding different concentrations to the solution
ranging from 1 to 10mM at pH 9.0 and temperature 30ºC.
Synthesis of CdS nanoparticles at various growth phases and time period .
To find the effect of growth phase of the organism on CdS nanoparticles
production, Enterobacteriaceae was inoculated into nutrient broth of 4 different
flasks.
The flasks were allowed to grow at various growth stages (lag phase, log phase,
late log phase and stationary phase). After that the biomass was incubated with
cadmium chloride or cadmium sulfate and sodium sulfide solution. The effect of
time over the growth was evaluated by collecting the samples at every 1 h up to
120 h.
Maximum amount of nanoparticles synthesized by bacterial strains was achieved
in stationary phase.
Results:
UV-Visible spectrophotometer :
Samples were washed twice with 50mM phosphate buffered saline (pH 7.0).
Then, ultrasonic disruption of cells was performed using an ultrasonic processor
over 3 -45 S periods with 10 s intervals between periods. The sonicated samples
were then filtered using a 0.22µm filter to eliminate cell debris and other
pollutants.
The filtered solutions were then used for characterization of CdS nanoparticles.
The dried particles were dispersed in deionized water and were measured using a
UV–Visible spectrophotometer .
The maximum absorption was at 400-450 nm in UV-Visible spectroscopy.
FT-IR and XRD analysis Purification of CdS nanoparticles was carried out according
to the method previously described.
For FT-IR and XRD analysis, samples were dried.
Freezing-drying method was used for this step.
The samples were frozen at -20ºC for 24 h and then dried at -37ºC temperature for
10h with Freezedrier system.
The obtained dried sample was subjected to FT-IR spectrum using Fourier Trans-
form IR spectrophotometer.
The phase formation and purity of CdS nanoparticles were checked by recording
the powder XRD patterns
Conclusion from XRD:
Amino groups bound to particles account for the stability of NPs.
Also FTIR studies established the existence of protein as the stabilizing and
capping agent
EDS ( Energy Dispersive Spectroscopy)
In order to determine the elemental composition of the synthesized nanoparticles,
EDS spectrum was recorded.
In this EDS spectrum, strong signals showed the presence of Cd and S.
This confirms that the nanoparticles are made of CdS alone. EDS spectrum was
recorded based on the micrographs measurements focusing on clusters of the
nanoparticles.
Resulting EDS spectrum from purified and dried CdS nanoparticle .The figure also
shows the signals from Cd and S elements from other metals. In the analysis of CdS
nanoparticles by energy dispersive spectroscopy the presence of elemental CdS
signal was confirmed.
The CdS nanocrystallites display an optical absorption band peaking at 3-4 keV,
which is the typical absorption of metallic CdS nanocrystallites due to the surface
plasmon resonance.
Scanning Electron Microscopy (SEM) Electron micrographs of crystal morphologies
and exteracellular organization of CdS nanoparticles found in Enterobacteriaceae.
For scanning electron microscopy (SEM) analysis, samples of the biologically
synthesized nanoparticles were prepared on gold-coated SEM grids.
In order to confirm the synthesis of nanoparticles, images were recorded using
SEM.
These images showed that the synthesized nanoparticles were spherical in shape
and had uniform morphology.
The size of the particles ranged between 5 and 200nm and the shape of the
particles were found to be almost spherical.
In this study, the ability of Enterobacteriaceae in synthesizing Cadmium sulfide
nanoparticles has been investigated.
It was found out that the exposure of bacterial cells to Cadmium Sulfide ions,
results in formation of Cadmium Sulfide nanoparticles either intracellulary or
extracellulary.
The synthesized nanoparticles were characterized and the effect of various
conditions on the synthesis were analyzed.
The synthesized Cadmium Sulfide nanoparticles were characterized using UV–
Visible spectroscopy, scanning electron microscopy (SEM), XRD and FTIR analysis
and energy-dispersive spectroscopy (EDS).
CdS Nanoparticles

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CdS Nanoparticles

  • 1. SYNTHESIS AND CHARACTERIZATION OF CADMIUM SULPHIDE NANOPARTICLES BY –ANJNEYA VERMA
  • 2. Introduction: Wayne Shenton, Dietmar Pum, Uwe B. Sleytr and Stephen Mann were the first to synthesis cadmium sulphide nanoparticles by biological method. The cadmium sulfide is an important II-IV group element semiconductor (Eg=2.42eV (515nm) at room temperature) with many excellent physical and chemical properties. This has promising application in multiple technical fields including photochemical catalysis, gas sensor, detectors for laser and infrared Cadmium sulfide is a solid hexagonal or cubic crystal. Cadmium sulfide is an important n-type semiconductor with a direct band gap 2.42eV., the photoconduction and electroluminescent properties of cadmium sulfide have been applied in manufacturing a verity of consumer goods.
  • 3. Green synthesis of CdS Nanoparticles using bacteria: Bacterial strains of Enterobacteriaceae is used as a potential producer for green synthesis of CdS nanoparticles. Bacterial strains were inoculated in BHI broth under sterile conditions and incubated at 37ºC. The strains vaccinate in Nutrient Agar, EMB Agar and Endo Mediums. Bacterial suspension was used for this method. Suspension was vaccinated in Nutrient broth and incubated at 37ºC for 24h for growing of bacteria. Then, the suspension were centrifuged at 5000 rpm for 15 min at room temperature and resulting supernatants were extracted for further processing. The obtained supernatants were washed with phosphate buffer saline (pH7.0) for 3 times. 1mM solution of CdCl2 (for E. coli) or CdSO4 (for K. pneumoniae) was prepared using deionized water. 35 ml of the solution was added to supernatants and resulting solution was kept for incubation in a shaker at 220 rpm and room temperature for 30 min. Then, 35 ml of 1mM Na2S solution was slowly added to the solution. The samples were then incubated at room temperature with end over en rotation for 10 min.
  • 4. Effect of pH and Temperature on nanoparticles synthesis : To find the conditions under which maximum amount of nanoparticles were synthesized, 1mM concentration of CdCl2 or CdSO4 and Na2S were added to the solution containing biomass and incubated in different pH conditions (5–11) and different temperatures. The pH of the incubation mixtures was adjusted using 1M HCl and 1M NaOH solutions. It was concluded that the optimum condition for synthesis of nanoparticles is temperature of 30ºC and pH of 9.
  • 5. Effect of CdCl2 or CdSo4 and Na2S on the nanoparticles synthesis : The study was carried out by adding different concentrations to the solution ranging from 1 to 10mM at pH 9.0 and temperature 30ºC. Synthesis of CdS nanoparticles at various growth phases and time period . To find the effect of growth phase of the organism on CdS nanoparticles production, Enterobacteriaceae was inoculated into nutrient broth of 4 different flasks. The flasks were allowed to grow at various growth stages (lag phase, log phase, late log phase and stationary phase). After that the biomass was incubated with cadmium chloride or cadmium sulfate and sodium sulfide solution. The effect of time over the growth was evaluated by collecting the samples at every 1 h up to 120 h. Maximum amount of nanoparticles synthesized by bacterial strains was achieved in stationary phase.
  • 6. Results: UV-Visible spectrophotometer : Samples were washed twice with 50mM phosphate buffered saline (pH 7.0). Then, ultrasonic disruption of cells was performed using an ultrasonic processor over 3 -45 S periods with 10 s intervals between periods. The sonicated samples were then filtered using a 0.22µm filter to eliminate cell debris and other pollutants. The filtered solutions were then used for characterization of CdS nanoparticles. The dried particles were dispersed in deionized water and were measured using a UV–Visible spectrophotometer . The maximum absorption was at 400-450 nm in UV-Visible spectroscopy.
  • 7.
  • 8. FT-IR and XRD analysis Purification of CdS nanoparticles was carried out according to the method previously described. For FT-IR and XRD analysis, samples were dried. Freezing-drying method was used for this step. The samples were frozen at -20ºC for 24 h and then dried at -37ºC temperature for 10h with Freezedrier system. The obtained dried sample was subjected to FT-IR spectrum using Fourier Trans- form IR spectrophotometer. The phase formation and purity of CdS nanoparticles were checked by recording the powder XRD patterns
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  • 11. Conclusion from XRD: Amino groups bound to particles account for the stability of NPs. Also FTIR studies established the existence of protein as the stabilizing and capping agent
  • 12.
  • 13. EDS ( Energy Dispersive Spectroscopy) In order to determine the elemental composition of the synthesized nanoparticles, EDS spectrum was recorded. In this EDS spectrum, strong signals showed the presence of Cd and S. This confirms that the nanoparticles are made of CdS alone. EDS spectrum was recorded based on the micrographs measurements focusing on clusters of the nanoparticles. Resulting EDS spectrum from purified and dried CdS nanoparticle .The figure also shows the signals from Cd and S elements from other metals. In the analysis of CdS nanoparticles by energy dispersive spectroscopy the presence of elemental CdS signal was confirmed. The CdS nanocrystallites display an optical absorption band peaking at 3-4 keV, which is the typical absorption of metallic CdS nanocrystallites due to the surface plasmon resonance.
  • 14. Scanning Electron Microscopy (SEM) Electron micrographs of crystal morphologies and exteracellular organization of CdS nanoparticles found in Enterobacteriaceae. For scanning electron microscopy (SEM) analysis, samples of the biologically synthesized nanoparticles were prepared on gold-coated SEM grids. In order to confirm the synthesis of nanoparticles, images were recorded using SEM. These images showed that the synthesized nanoparticles were spherical in shape and had uniform morphology. The size of the particles ranged between 5 and 200nm and the shape of the particles were found to be almost spherical.
  • 15.
  • 16. In this study, the ability of Enterobacteriaceae in synthesizing Cadmium sulfide nanoparticles has been investigated. It was found out that the exposure of bacterial cells to Cadmium Sulfide ions, results in formation of Cadmium Sulfide nanoparticles either intracellulary or extracellulary. The synthesized nanoparticles were characterized and the effect of various conditions on the synthesis were analyzed. The synthesized Cadmium Sulfide nanoparticles were characterized using UV– Visible spectroscopy, scanning electron microscopy (SEM), XRD and FTIR analysis and energy-dispersive spectroscopy (EDS).