Int. Journal of Applied Sciences and Engineering Research, Vol. 1, Issue 3, 2012
© 2012 by the authors – Licensee IJASER- Under Creative Commons License 3.0
Research article
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ISSN 2277 – 9442
Synthesis and characterization of Lead (II) hydroxide
Nanoparticles
1
1
R.Hepzi Pramila Devamani, 2M.Alagar
Post Graduate Department of Physics, V.V.Vanniaperumal College, Virudhunagar.
2
Centre for Research and Post Graduate Department of Physics,
Ayya Nadar Janaki Ammal College, Sivakasi.
doi: 10.6088/ijaser.0020101049
Abstract: Nano particles of lead (II) hydroxide have been prepared by chemical co-precipitation method.
The particle size and crystal structure of lead (II) hydroxide nano powders are characterized by X-ray
diffraction (XRD).The surface morphology of the ample is studied from SEM images. The FTIR spectrum is
used to study the stretching and bending frequencies of molecular groups in the sample. The absorption
spectra of the sample are recorded in the UV range. From the analysis of absorption spectra, lead (II)
hydroxide is found to have a direct band gap of 5.41eV.
Key words: XRD, SEM, FTIR, UV, Nanoparticles.
1. Introduction
Optical properties of semiconductor nano particle enhances when compared to that of its bulk size
(Navaneethan, 2009), (Jamie, 2006)(Hines,2003),(Yang,2006). In the semiconductor nano particles, optical
property enhancement has been attributed to the modification of surface morphology (navaneethan, 2009),
(Jamie, 2006). When size of the nano particles are below Bohr radius it leads to the quantum confinement
effect (Navaneethan, 2009), (Soo, 1994). Lead hydroxide is used in making porous glass; in
electrical-insulating paper; in electrolytes in sealed nickel-cadmium batteries; in recovery of uranium from
sea water and as a catalyst for oxidation of cyclododecanol.
2. Materials and methods
Nano particles of Lead (II) hydroxide was prepared by chemical precipitation method, adding Lead
(II) nitrate and sodium hydroxide. Precise amount of the reagents taking into account their purity were
weighed and dissolved separately in distilled water into 0.1 M concentration. After obtaining a
homogeneous solution, the reagents were mixed using magnetic stirring. The precipitate was separated
from the reaction mixture and washed several times with distilled water. The wet precipitate is dried and
thoroughly ground using an agate mortar to obtain the samples in the form of fine powder.
3. Tests conducted
X-ray diffraction is an ideal technique for the determination of crystallite size of the powder samples.
The basic principle for such a determination involves precise quantification of the broadening of the peaks.
XRD line broadening method of particle size estimation was chosen in this investigation for determining
the crystallite size of the powder sample. XRD and the morphology of the powder samples were carried
out by scanning electron microscope (SEM) at Centre for Electro Chemical Research Institute, Karaikudi.
The infra red spectroscopic (IR) studies of Lead (II) hydroxide nano particles were made by using
‘SHIMADZU’ FTIR 8400S model spectrometer through KBr method. The UV spectrum was taken in the
483
*Corresponding author (e-mail: [email protected])
Received on May 16, 2012; Accepted on June 20, 2012; Published on July. 1, 2012
Synthesis and characterization of Lead (II) hydroxide Nanoparticles
absorbance mode in the wavelength range from 200 to 800 nm.
4 Results and discussion
4.1. XRD Studies
The XRD patterns of the prepared samples of lead (II) hydroxide are shown in fig.1. XRD studies
reveal that the samples are nano sized and crystalline. The fine particle nature of the samples is reflected in
the X-ray line broadening. The size of the synthesized nano particles are calculated using Scherrer equation.
The average grain size of the particles is found to be 60.17nm.
Counts
pboh2leadIIhydroxide
3600
1600
400
0
10
20
30
40
50
60
70
Position[°2Theta]
Figure 1: XRD pattern of Lead (II) hydroxide
4.2 SEM Studies
To identify the morphology of nano particles, the synthesized sample Lead (II) hydroxide was
subjected to SEM studies. From the SEM studies, the morphology of the particles is identified. The
morphology of most of the particles in SEM was observed to be spherical .The fig.2 and fig.3 show the
SEM images of the Lead (II) hydroxide sample.
R.Hepzi Pramila Devamani1, M.Alagar
Int. Journal of Applied Sciences and Engineering Research, Vol. 1, Issue 3, 2012
484
Synthesis and characterization of Lead (II) hydroxide Nanoparticles
.
Figure 2: SEM image of Lead (II) hydroxide at 3.00 kx
Figure 3: SEM image of Lead (II) hydroxide at 5.00 kx
4.3 FTIR Studies
The FTIR spectrum of the Lead (II) hydroxide sample is shown in the fig.4. The FTIR spectrum for
Lead II hydroxide shows a strong peak at 3506.35cm-1 and 3197.76cm-1 corresponding to the O-H
stretching(6). Another strong and sharp peak with a maximum of 1672.17cm-1 due to H-OH stretching. The
spectrum also shows peak at 1271cm-1 indicating asymmetric stretching and the peak at 1193.85cm-1
R.Hepzi Pramila Devamani1, M.Alagar
Int. Journal of Applied Sciences and Engineering Research, Vol. 1, Issue 3, 2012
485
Synthesis and characterization of Lead (II) hydroxide Nanoparticles
indicates the presence of Lead (6), (Gautam, 2010) and the peak at 721.33cm-1 is due to the plane bending.
Figure 4: The FTIR spectrum for Lead (II) hydroxide
4.4 UV Studies
The band gap of the prepared sample Lead (II) hydroxide was determined by using UV visible
studies. It has been noticed that the optical band gap of Lead (II) hydroxide is 5.41ev. Fig.5 shows the
graph to find the band gap of Lead (II) hydroxide.
uv for Pb(oH)2
1.00E-36
ahu*ahu
8.00E-37
6.00E-37
4.00E-37
2.00E-37
2.47E-43
3.11E+00
4.11E+00
5.11E+00
E ev
6.11E+00
Figure 5: Band gap of Lead (II) hydroxide
R.Hepzi Pramila Devamani1, M.Alagar
Int. Journal of Applied Sciences and Engineering Research, Vol. 1, Issue 3, 2012
486
Synthesis and characterization of Lead (II) hydroxide Nanoparticles
5 Conclusions
The Lead (II) hydroxide nanoparticle has been prepared by chemical co-precipitation method. XRD
analysis and SEM suggest that the average particle size is in the nano range. The SEM picture reveals the
morphology of the particles. From the FTIR spectrum, the stretching and bending frequencies of the
molecular functional groups in the sample are studied. From the UV spectra, the band gap was found.
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R.Hepzi Pramila Devamani1, M.Alagar
Int. Journal of Applied Sciences and Engineering Research, Vol. 1, Issue 3, 2012
487