Synthesis and Characterization of CdS Nanomaterial

Dissertation submitted in partial fulfilment

of the requirements for the degree of

Bachelor of Science
in
Electronic Science
by

Miss Priyanka Sarmah

B.Sc 6th semester
Roll No.:-16ELT2315
Dept. of Electronics
Jagannath Barooah College (Autonomous)
Jorhat-785001, Assam

Under the supervision of

Dr Pronob Jyoti Saikia

Department of Electronics
Jagannath Barooah College (Autonomous)
Jorhat-785001, Assam, India

1
 Jagannath Barooah College (Autonomous)
Dept. of Electronics
Jorhat-785001,Assam

Dr Pronob Jyoti Saikia

HoD of Electronics

CERTIFICATE OF THE SUPERVISOR

This is to certify that Miss Priyanka Sarmah, a 6 th semester

student of B.Sc, Dept. of Electronics from Jagannath Barooah
College (Autonomous), Jorhat has completed her dissertation on
“Synthesis and Characterization of CdS Nanomaterial”.
During her dissertation period she has displayed very sincere and
consensus attitude towards her work. Her performance during
this work was found satisfactory.

I wish her success in all her future endeavours.

Date: (Pronob Jyoti Saikia)

Place: Supervisor

2
 ACKNOWLEDGEMENT

I express my sincere gratitude to the Principal, J.B.College

(Autonomous) for giving us the opportunity to be a part of this
dissertation paper.
I render my heartfelt gratitude to my supervisor Dr Pronob Jyoti
Saikia, HoD of Electronics, J.B.College (Autonomous) for guiding us
throughout the period and enlightening us with the knowledge.
I am thankful to Dr Bhupen kr Baruah sir, Assistant Professor,
Chemistry, J.B.College (Autonomous),Mr Ankuraj Boruah Sir,Mr
Bhaskar Borah for his initiatives, kind guidance without which it
would not be possible to complete the project.
It is our pleasure that we finished our project in CSIR-NEIST. I would
also like to render my thanks to the Head, HRD, NEIST and special
thanks to Dr. Lakshi Saikia sir , Mr. Paran Jyoti Kalita Sir (Material
Science Division) and Mr. Jugal Bori .

I am indebted to my loving parents and my near and dear ones for

their inspiration, support and love. Finally, thanks are due to all my
friends and well wishers for their support throughout my course and
project work.
Ultimately, the entire period was a successful one and we got to learn
a lot. All credits go to the excellent facilities, the availabilities of
modern technologies and the knowledgeable yet helping stuff of the
institute.
PRIYANKA SARMAH
B.Sc 6th semester
Roll No.:-16ELT2315
Dept. of Electronics
Jagannath Barooah College
(Autonomous)
Jorhat-785001, Assam

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 DECLARATION

I hereby declare that the dissertation entitled “Synthesis and

Characterization of CdS Nanomaterial” is submitted by Priyanka
Sarmah, Roll no.: 16ELT2315 is an original work done and
submitted by me in partial fulfilment for the Degree of Bachelor of
Science in Electronics , J.B. College ( Autonomous), Jorhat. This is a
record work done by me under the guidance of Dr. Pronob Jyoti
Saikia, Head of the Department (HoD) of Department of Electronics,
J.B.College (Autonomous).

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 Abstract

Nanomaterials are the leading edge to the rapidly developing

nanotechnology. For the synthesis of nanomaterials over a wide range
of chemical composition, the development of reliable and efficient
methods is a challenging issue in nanotechnology.
CdS nanoparticles (NPs) are widely used in applications such as
photodegradation of organic molecules, photocatalysis of water
splitting, and as building blocks of photovoltaic devices.
Cadmium sulphide nanoparticles by using precipitation method is
simple, fast and can developed at room temperature. The obtained
particles were characterized using XRD (X-ray diffraction study),
SEM(scanning electron microscopy) UV-Visible spectrophotometer.
Cadmium sulphide nanoparticles are good adsorbent. When CdS
nanoparticles were dispersed in the solution as single entities, showed
very good resistance against oxidation for months, according to their
polymer shell.

5
CONTENT PAGE NO

1. Chapter -1
a) Introduction...............................................................9-14
b) Review of literature.................................................12-13
2. Chapter -2
a) Materials and method.....................................................14
b) Experimental details....................................................15-20
3. Chapter -3
a) Result and Discussion..............................................21
i. Scanning Electron Microscopy (SEM).......21-22
ii. X-Ray Diffraction (XRD)..............................23
iii. UV Visible Microscopy...............................24-25
4.Chapter -4
b) Conclusion.............................................................26
c) Future work............................................................27
Reference...................................................................................28

6
List of Figures

7
List of table

8
 Chapter-1

Introduction

The present era of science and the implementation of it in the society

is a very important factor for the new works that has been done in the
laboratory in research work done by the students and researchers. The
synthesis and characterization of nanoparticles and to check the
improvement of its property by synthesizing it via different routes
available in the laboratory.
Nanoscience and nanotechnology have been an interesting field of
research and gained much importance from last two decades. In
layman terms “The study of properties of materials at nanoscale is
termed as nanoscience, whereas the fabrication and application of the
nanostructures are termed as nanotechnology”. Nanoparticles are the
smallest of the microscopic particles or ultrafine particles which is
having size in the range of 1-100nm.[1]

Among various nanoparticles a great interest has been shown towards

cadmium sulphide (CdS) nanoparticles because of availability of
discrete energy levels, size dependent optical properties, tunable
bandgap and a well-developed synthetic protocol, easy preparation
technique with good chemical stability.[1]

Due to its very high photosensitivity it has usage in detection of

visible radiations, in light emitting diodes, solar cells, photochemical
catalysis, gas sensors, various luminescence devices, optoelectronic
devices and a range of biological application.[1]

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Semiconducting optoelectronic materials play an important role in a
variety of application due to their unique optical, electrical, magnetic
and piezoelectric properties. Modification of these properties of
semiconductor materials depends upon the size, shape, morphology
and dimensions of material.[1]

Cadmium sulphide (CdS) semiconductor is an excellent visible light

detector among other semiconductors.

Properties of Cadmium Sulphide (CdS):-

Property Value
Physical state and appearance Solid. (Solid powder.)
Molecular Weight 144.46 g/mole
Color Yellow or brown
Density 4.826 g/cm3
Melting Point Sublimes. (1750°C or 3180°F)
Boiling Point 980°C or 1800°F
Specific Gravity 4.82 g/cm3
Solubility Insoluble in hot and cold water
but soluble in acid

10
Different methods for nanoparticles synthesis:

There are various physical, chemical and biological methods for

synthesizing CdS nanoparticles (fig.1). In laboratory CdS
nanoparticles can be synthesized by chemical methods and biological
methods. Biosynthesis of CdS nanoparticles using various plant
products and microorganisms had gained much more importance than
the other methods as it is less expensive and more environment-
friendly.[1]

Fungi
Plant Products
Yeast
Biological method
Bacteria

Nanoparticles
synthesis

Thermal
Plasma Condensation
Physical method Chemical
Pyrolsis method Reduction

Evaporation
Explosion Sol-Gel method Precipitation

Fig 1: Different methods for nanoparticles synthesis

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The parameters of the synthesis, which can be fixed and optimized for
the synthesis are listed below. However, there are some additional
parameters in the synthesis of each size which have to be identified
and tuned in order to get a particular size of interest.
These are:
1. Volume of the reactants
2. Stirring speed
3. Rate of addition of CdCl2
4. Time of stirring after CdCl2 addition
5. Temperature
6. PH-value

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 Defence &
Security
Metallurgy
Energy & Materials
storage

Agriculture
Applications of Electronics
& Food nanotechnology

Cosmetics Textile
And Paints

Biotechnology

Fig 2: Different applications of nanotechnology

13
Cadmium is one of the toxic heavy metal found in the effluents of
industries. Cadmium ions are not biodegradable and they accumulate
in living organisms at a higher concentration and cause various health
hazards. There are various techniques which are most commonly used
to remove the heavy metals like cadmium from water bodies are
ultrafiltration, lime precipitation, ion exchange and reverse osmosis,
electrochemical treatment, oxidation-reduction
But the use of these techniques have certain limitations like
incomplete precipitation, high operating cost and generation of a large
amount of metal bearing toxic sludge

14
 Review of literature

A theory of size confinement in semiconductor nanoparticles is well

described in text books and reported partly in some previous doctoral
theses.[6]

Determination of the nanoparticle size

What is the real size of the nanoparticle ? This is a fundamental

question specially for the nanoparticles synthesized with organic
capping molecules. Importantly no size determination technique
allows an exact size determination. The difficulty arises mainly
because of the limitations of the available methods and also because
of the influence of the capping molecules attached to the particle
surface. The methods used conventionally to determine particle sizes
are listed below.[6]

1) UV-VIS absorption
2) X-Ray Diffraction (XRD)
3) Transmission Electron Microscopy (TEM)
4) Scanning tunnelling Microscopy (STM)
5) Atomic Force Microscopy (AFM)
6) Small angle X-ray Scattering (SAXS)

UV-VIS absorption is a very first characterization method for the

nanoparticles because the absorption features give information about
the nanoparticle formation, the band gap and the size distribution of
the nanoparticles. However, it is an indirect method for determining
the particle size.[6]

15
X-ray powder diffraction was used for structure and size
determination by many groups. The particle size can be obtained
either by direct computer simulation of the X-ray diffraction pattern
or from the full width at half maximum (FWHM) of the diffraction
peaks using the Debye-Scherrer formula.[6]
Furthermore, the validity of Scherrer’s equation, the effect
of defects, shapes and size distributions on the X-ray diffraction
patterns has to be examined. This is possible with a direct computer
simulation approach[6].

Electron microscopy is widely used to determine the size of particles.

TEM allows the imaging of individual particles and to some extent to
evaluate the statistical distribution of sizes and shapes of the particles
in sample. High magnification imaging with lattice contrast allows
imaging of individual crystallite morphologies.[6]

16
 Chapter-2

Materials and Method

Apparatus Required:
1. Digital balance
2. Glass Beaker
3. Graduated cylinder
4. Glass stir rod
5. Hot Plate
6. Funnel
7. Convection Oven(with different environment)
8. Watch glass
9. Mortar pestle(crusher)
Chemical Required:

1. Cadmium Chloride (CdCl2)

2. Sodium Hydroxide (NaOH)
3. Hydrogen Sulphide (H2S)
4. Methanol
5. Acetone

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 Experimental Details

 The sample of CdS material was prepared by using Cadmium

Chloride, Sodium Hydroxide and Hydrogen Sulphide by
precipitation method.
 Aqueous solution of 0.1 M CdCl2 (20ml) and 0.1 M of Sodium
Hydroxide (20ml) were separately prepared in this method.
 Hydrogen Sulphide was passed into the solution and Sodium
Hydroxide was slowly added to methanol.
 CdCl2 solution was added after stirring the previously prepared
solution for one hour.
 Acetone was used as a non solvent for selective precipitation
after three hours of constant stirring (till the yellow solution was
formed).
 CdS nanoparticles were obtained in orange powder form when
precipitate formed was allowed to evaporate at room
temperature.

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 Flow Chart

Aqueous solution of 20 Aqueous solution of 20ml Sodium

ml CdCl2 was prepared Hydroxide was prepared

X ml of methanol was added

H2S gas passes through it

Stirring

Yellow solution was obtained

Add acetone as a non-solvent

Evaporate at room temperature

Orange powder formed

19
 Experimental Setup:

Fig.3:- Sample and chemicals used

20
Fig.4:-Hot Plate with the sample

Fig.5:- Filtering solution

21
Fig.6:Dry precipitate part

22
 Fig.7:-Grinding Solution

Chapter-3

Results and Discussion

The structural and morphological properties were determined by

diffraction studies (using X-Ray Diffraction (XRD) Spectroscopy)
and microscopic studies using Scanning Electron Microscopy (SEM).

23
Scanning Electron Microscope(SEM):

SEM image size for CdS= 2 μm

Shape of CdS = Needle Shape

24
Fig.8: SEM images of CdS material size 7.332μm

25
Division:- Biological Science and Technology Division (Bhatnagar
Building),CSIR-NEIST, Jorhat

26
27
X-Ray Diffractometry(XRD):

XRD analysis of the CdS nanoparticles was carried out to study the
crystallinity and purity of the material. The XRD pattern of CdS (Fig.
2) exhibited six peaks corresponding to (002) for 2theta value 26.640,
(110) for 2theta value 44.020, (112) for 2theta value 52.020 and (114)
for 2theta value 72.880 faces in the crystal system. This confirmed the
hexagonal crystal structure of the material.

XRD data further helped to estimate the size of the nanoparticles.

Fig.9: XRD of CdS

28
 UV visible

Fig.10 UV-VIS absorption spectrum of CdS nanoparticles

UV visible absorbtion spectra of CdS is shown in fig.10 The energy

band gap determination of CdS is shown in fig.11.

29
 900

800

700

600
(αhν)2

500

400

300

200

100

0
1 1.5 2 2.5 3 3.5 4 4.5 5 5.5 6 6.5 7

hν (eV)

Fig.11 Energy band gap determination of CdS

Bandgap for CdS nanomaterials is 3.25 eV

256.25nm wavelength corresponding to energy 4.8390244 eV.

30
 Chapter-4

Conclusion

The present study indicates that the precipitation method can be

successfully employed for the preparation of CdS material. In
conclusion, Cadmium sulphide nanoparticles were synthesized by
precipitation method. The synthesized nanoparticles were
characterized by various spectroscopic, XRD (X-ray diffraction
analysis), SEM (scanning electron microscopy), and UV Visible
spectroscopy.

31
 Future Work

In the present work, CdS nanoparticles were synthesized and

characterized.

 These CdS nanoparticles can be used for toxicity test in other

cell lines.
 The toxicity of these synthesized CdS nanoparticles can be
further minimized by surface modification with a class of
compounds namely, flavonoids. This class of compounds,
display important biological activities, including antimalaria,
anticancer, anti - inflammatory, analgesic, antioxidant,
cytotoxic, etc.
 Cytotoxicity studies based on size and shape of the
nanoparticles can be performed
 The synthesized CdS quantum dots could be tagged with
biomolecules for bio - imaging applications.

32
 References

1) Kalpana Doloi, “Synthesis and characterization of Cadmium

Sulphide Nanoparticles and its utilization in removal of
Cadmium from aqueous solution”(2014).

2) K Manickathai, S Kasi Viswanathan & M Alagar, “Synthesis

and characterization of CdO and CdS nanoparticles”,(2008)

3) Nayereh Soltani,Elias Saion, “Visible Light –Induced

Degradation of Methylene Blue in the presence of Photo
catalytic ZnS and CdS Nanoparticle” (2012)

4) Preeti Sahare, “Synthesis and Characterization of CdS

Nanoparticles”.

5) El-Bially A.B.,Seoudi R., EisaW., “Preparation,Characterization

and Physical Properties of CdS Nanoparticles with Different
Sizes”.

6) Sanjeev Joshi, “Preparation and characterization of CdS

nanoparticles”(2004)

33