JOURNAL OF SEMICONDUCTOR TECHNOLOGY AND SCIENCE, VOL.18, NO.1, FEBRUARY, 2018 ISSN(Print) 1598-1657 https://doi.org/10.5573/JSTS.2018.18.1.091 ISSN(Online) 2233-4866

Manuscript received Jun. 16, 2017; accepted Sep. 4, 2017 1 Department of Physics, University of Mohaghegh Ardabili, P.O. Box 179, Ardabil, Iran 2 Department of Engineering Sciences, Sabalan University of Advanced Technologies (SUAT), Namin, Iran E-mail : azizian@uma.ac.ir, yashar.a.k@gmail.com

Preparation of Lead Oxide Nanostructures in Presence of Polyvinyl Alcohol (PVA) as Capping Agent and

Investigation of Their Structural and Optical Properties

Yashar Azizian-Kalandaragh1,2*

Abstract—In this research, a simple ultrasound-assisted method has been used for the preparation of lead oxide nanostructures in the presence of polyvinyl alcohol (PVA) as a capping agent. Different concentrations of PVA were added to the mixture to control of nanostructure size. The as-prepared lead oxide nanostructures have been investigated by UV-Vis spectroscopy, X-ray diffraction (XRD), Fourier transform infrared (FT-IR) and scanning electron microscopy (SEM). UV-Vis spectroscopy results show a shift in the peaks and broadening with increasing of PVA amount. The XRD pattern indicates the uncapped sample contain mixture phase of lead oxides and PVA-capped samples were high purity and no other peaks were observed. The average crystallite size of nanoparticles was estimated using Debye-Scherrer's formula and the measured sizes reveal clearly the crystallite size decreases with increasing PVA concentration. The SEM results show by increasing in capping agent concentration, the distribution of nanoparticles has been changed. FT-IR Spectroscopy results show by increasing of capping agent concentration the energy between the functional group is changed and some peaks show a slight shift.

Index Terms—Lead oxide, capping agent, nanoparticle size, XRD, UV-Vis spectroscopy

I. INTRODUCTION

The synthesis and characterization of semiconductor nanomaterials have been a drastic field of research due to their potential applications in different branches and technologies [1-3]. Size-controlled preparation of semiconducting nanostructures is a major challenge in nanoscience and nanotechnology because their essential physiochemical properties and applications are forcefully related on the size-dependent quantum size effect. There has been a great attention of interest in developing various techniques for controlling the nanostructures sizes and shapes using organic capping agents [4-7]. Various organic capping materials, with different head groups, hydrophobic chains, and molecular architectures, have been widely employed as capping or inducing agents to control the nucleation, growth, and assembly of metal oxide nanostructures. Poly (vinyl alcohol) (PVA) is a biodegradable, water soluble, semicrystalline, nontoxic, biocompatible, and artificial polymer [8]. Due to these unique properties, PVA is widely utilized in many potential applications like food packaging [9], medicine [10], biosensors [11], electronic devices [12] and so forth. In addition, PVA is a most frequently used for the preparation of metal oxide nanostructures in aqueous solution [13-15]. For example, PVA-capped PbO thin films were prepared by Asogwa by chemical bath deposition method. His optical investigation results showed that such thin film can be used in solar cells [16]. Thottoli et al. synthesized ZnS nanoparticles with PVA as capping agent through wet chemical method. They observed in particular PVA and citrate concentration

92 YASHAR AZIZIAN-KLANDARAGH : PREPARATION OF LEAD OXIDE NANOSTRUCTURES IN PRESENCE OF POLYVINYL …

preparation of hexagonal ZnS nanoparticles is possible at lower temperature [17].

A general way for size control is the use of capping agents that commonly adsorb on the surface of nanostructures, causing a nanoparticle-stabilizer essence which then indicates very stable nanostructures formation [18]. Between different metal oxide materials, lead oxide is a significant semiconductor material which has been used extensively in the area of luminescence materials [19], gas sensors [20], storage devices [21], glass industry [22], pigments [23], nanoscale electronic devices [24], photocatalytic [25] and so on. The lead element has many oxide polymorphs including PbO (α, β and amorphous), Pb2O3, Pb3O4, PbO2 (α, β and amorphous). It is reported that the lead-to-oxygen ratio defines the band gap and, hence, the color of materials. It is also reported that the color of PbO is yellow and the color of Pb3O4 is red [26, 27]. PbO itself has two forms: the first one is yellow β-PbO, which is stable at high temperature and the second one is red α-PbO, which is stable at low temperature. PbO is an indirect bandgap semiconductor material with tetragonal and orthorhombic crystalline phases. The band gap of tetragonal and orthorhombic crystalline structures of PbO semicon- ductors in its bulk form are 1.9-2.2 eV and 2.6 eV, respectively [28, 29].

Many methods such as calcination [30], hydrothermal [31], sol-gel [32], spray pyrolysis [33], sonochemical [34], microwave-assisted method [35], electrochemical method [36], thermal deposition [37] have been reported for the synthesis of lead oxide nanostructures. Recently, PbO nanoparticles have been synthesized by ball milling and solvothermal methods as a highly efficient, simple, cheap, and recyclable catalyst by Tayebee et al [38]. Ranjbar and his coworker prepared PbO nanoparticles by decomposition of nano-sized Pb(II) coordination polymer at 600°C. They reported a study that the coordination polymers may be suitable precursors for the preparation of nanoscale metal oxide materials with different morphologies [39].

Among mentioned synthesis techniques, the ultrasound-assisted method has proven to be the most favorable technique for the preparation of nanostructured materials as the process is relatively simple and the nanoparticle size can be controlled. The ultrasound waves can promote the formation of nanostructures.

According to the researchers, the effects of high-intensity of ultrasound result from acoustic cavitation: The formation, growth and implosive collapse of bubbles in liquids which generate transient temperatures of approximately 5000K, pressures of about 1800 atm and cooling rates of 1010 K/s [40, 41]. In summary, lead oxide nanostructures were prepared by a ultrasound-assisted method in the presence of PVA as a capping agent. In addition, the particle size was tuned by variation of the concentration of capping agent. The band gap energy of the lead oxide nanocrystals varied according to the crystal morphology because of the size effect. The morphology and structural properties of lead oxide nanostructures were analyzed by means of SEM, FT-IR, XRD, and UV-Vis.

II. MATERIALS AND METHODS

1. Preparation of PbO Nanostructures To synthesize lead oxide nanomaterials the chemicals

used were lead acetate (Pb(C2H3O2)2), polyvinyl alcohol (PVA) and sodium hydroxide (NaOH). In a typical procedure, aqueous stock solutions of (0.2M) 1.51 g of Pb(C2H3O2)2, was dissolved in 20 ml distilled water, in another baker 0.16 g, NaOH was dissolved in 20 ml of distilled water. The lead acetate solution was then added to the sodium hydroxide solution and then cooled to room temperature. This solution was irradiated with a high intensity ultrasonic at room temperature for 20 min using Dr. Heilscher ultrasound processor (UP200H Germany, 14 mm diameter Ti horn, 200 W/cm2, 24 kHz). Different amounts of an aqueous solution of PVA (1%, 2%, 3% and 4%) were added to the solution and the effect of addition was characterized. The prepared solution was centrifuged to get the precipitate out and washed four times using double distilled water and ethanol to remove the unreacted reagents and dried in an oven at 300°C for 3h. To convert the as-prepared sample to PbO, the as-prepared powders were annealed at 250°C for 1h in the open air. The Possible chemical reaction for the formation of PbO nanoparticles are as follows:

2NaOH+ Pb(C2H3O2)2 → 2 NaC2H3O2 + Pb(OH)2

Calcinated at 300

ºC Pb(OH)2 PbO+ H2O

JOURNAL OF SEMICONDUCTOR TECHNOLOGY AND SCIENCE, VOL.18, NO.1, FEBRUARY, 2018 93

An illustration scheme of the PVA capped PbO is shown in Scheme 1. According to Abedini et al., studies the effect of PVA as a stabilizer for dissolved metallic salts is through steric and electrostatic stabilization. However, the explanation of full mechanism is complex, due to the existence of hydrogen bonds, between the water molecules and the polarized groups on the polymer [42].

2. Instruments

Surface morphologies were studied using the

LEO1430 VP scanning electron microscope (SEM) with 15 kV accelerating voltage. The X-ray diffraction (XRD) patterns of products were recorded on a Philips X’pert X-ray diffractometer with CuKα radiation (λ=1.54056 A˚) employing a scanning step of 0.02o S-1, in the 2θ range from 10o to 80o. UV-Vis absorption spectra of the samples were obtained using a Shimadzu spectrophoto- meter (Japan, model 1800). Fourier transform-infrared (FT-IR) spectra were obtained using Perkin Elmer Spectrum RXI apparatus. Thermal analyses were done using a thermogravimetric apparatus (model Linseis, STA PT-1000).

II. RESULTS AND DISCUSSION

1. X-ray Diffraction (XRD) Fig. 2(a)-(e) shows the XRD patterns of the uncapped

and capped samples prepared by the ultrasound-assisted method, respectively.

The uncapped sample’s pattern (Fig. 2(a)) indicates diffraction peaks corresponding to mixtures of lead

oxides nanostructures (PbO, PbO2, and Pb3O4). In Fig. 2(b)-(e) all diffraction peaks appeared in this pattern match very well with ICDD data, all diffraction peaks can be indexed to the tetragonal phase of PbO.

The mean crystallite size of PbO nanostructures was calculated using Debye-Scherrer's equation:

D = 0.9 λ/β cosθ (1)

where D is the average crystallite size, λ is the wavelength of CuKα, β is the full width at half maximum of the diffraction peak and θ is the Bragg's angle [43]. The crystallite sizes were calculated to be 42, 32, 30, 27 and 26 nm for samples with 0%, 1%, 2%, 3% and 4% PVA concentration, respectively. The measured sizes reveal clearly that with increasing PVA concentration the crystallite size decreases gradually.

Fig. 1. The schematic illustration of PVA-capped PbO.

Fig. 2. XRD pattern of the uncapped sample (a) and PVA-capped samples, (b) containing 1% PVA, (c) containing 2% PVA, (d) containing 3% PVA, (e) containing 4% PVA.

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2. UV-Vis Analyses To investigate the optical characteristics of as-prepared

PbO nanostructures, the UV-Vis absorption spectrum was recorded in 250-800 nm is shown in Fig. 3.

The optical absorbance edge of PbO samples was blue shifted from that of the bulk tetragonal phase of PbO (564 nm, Eg= 2.2 eV). The broadening of the absorbance spectrum with increasing in capping agent concentration due to the quantum confinement of nanostructures.

Band gap (Eg) of the as-prepared nanostructures can be determined by the following equation:

(αhν)2 = K(hν - Eg) (2) where α is the absorption coefficient, hν is the photon energy (eV), K is a constant, and Eg is the band gap [44].

The corresponding band gaps energy for prepared samples were calculated 2.4, 3, 3.3, 3.42 and 3.5 eV. The shift in the band gaps can be connected with the quantum size effect in PbO nanostructures. Fig. 4 shows the Tauc's plot of (αhν)2 against the photon energy (hν) for as-prepared samples.

The blue-shifted band gap of PbO quantum dots can be explained by the hyperbolic band model (HBM). We use this approximation to calculate the radius of quantum dots (R) and compare it with experimental values obtained from X-ray diffraction. In the HBM, Eg,nano for the quantum dots calculated by:

2 2

1,2 2, , 2

2[ ]g bulk

g nano g bulk

EE E

Rpm

= +h

(3)

where μ, ,g nanoE and ,g bulkE are:

Reduced mass, gap energy in quantum dots and gap energy in bulk form respectively [45, 46]. For the PbO, µ=me

* mh*/ me

*+ mh* where me

*=0.46me, mh* =0.38me

(me is the electron mass equal to 9.1×10-31 kg) [47]. Table 1 shows the results calculated diameter (D=2R)

of quantum dots from HBM approximation and experimental data obtained from XRD analysis.

The calculated diameter by HBM approximation is in good agreement with the size estimated from the XRD results.

3. Scanning Electron Microscopy (SEM)

Fig. 5 shows the scanning electron microscopy analysis

(SEM) for the powders synthesized under ultrasound wave whit different amount of PVA capping agent.

It is obvious from the SEM images that the nanoparticles are formed in nearly spherical structure and there is a difference between the uncapped and PVA-capped samples. In the uncapped sample, the particles cling together and a cluster formed, but in capped

Fig. 3. UV-Vis spectrum of PbO nanostructures (a) without capping agent, (b) containing 1% PVA, (c) containing 2% PVA, (d) containing 3% PVA, (e) containing 4% PVA.

Fig. 4. Tauc plot of PbO samples (a) without capping agent, (b) containing 1% PVA, (c) containing 2% PVA, (d) containing 3% PVA, (e) containing 4% PVA.

Table 1. The calculated diameter (2R) by HBM and comparing them with XRD data

Sam.

App. (a) (b) (c) (d) (e)

HBM 49 nm 35 nm 32 nm 30 nm 29 nm XRD 42 nm 32 nm 30 nm 27 nm 26 nm

JOURNAL OF SEMICONDUCTOR TECHNOLOGY AND SCIENCE, VOL.18, NO.1, FEBRUARY, 2018 95

samples, the distribution of the nanoparticles has been changed.

4. Fourier Transform Infrared (FT-IR)

In the order to further study and determination of

adsorption mechanism of PVA onto the nanoparticle surface, FT-IR analysis of PVA-capped lead oxide was

carried out and the acquired data were compared with uncapped samples. Fig. 6 show the FT-IR spectra of lead oxide.

The absorption band around 3350 cm-1 corresponds to the O-H stretching vibration of adsorbed H2O molecules on the samples [48]. The peak at 2440 cm-1 is related to antisymmetric vibration of C-H and The peak at 1740 cm-1 corresponds to the stretching of C=O vibration.

Fig. 5. SEM images of PbO samples (a) without capping agent, (b) containing 1% PVA, (c) containing 2% PVA, (d) containing 3% PVA, (e) containing 4% PVA.

96 YASHAR AZIZIAN-KLANDARAGH : PREPARATION OF LEAD OXIDE NANOSTRUCTURES IN PRESENCE OF POLYVINYL …

The peak around 1470 cm-1 is attributed to stretching bending vibration of O-H. Another peak appears around 1060 cm-1 is attributed to bending vibration of C-O [49]. The peak around in 830 cm-1 appears which is due to the Pb-O vibrations and peak around 700 cm-1 is related to asymmetric bending vibration of Pb-O-Pb [50]. A comparative analysis shows, with the addition of PVA as a capping agent to lead oxide, the energy between functional groups in changed and some peaks show a slight shift which confirms the formation of the composition of PVA and lead oxide.

IV. CONCLUSION

In summary, lead oxide nanostructures capped with different concentration of PVA have been prepared and their optical and structural characteristics have been investigated using different techniques. Quantum size effect is obvious from the optical absorption spectra, which showed a blue shift in the excitonic specification as compared to the bulk lead oxide. The analyses of SEM, XRD, and absorption edge of the prepared samples showed that the amount of capping agent affects the structural and optical characteristics of nanostructures. Blue shift in UV-Vis peak and appearance of some peaks in FT-IR spectrum confirm the formation of very fine nanostructures and the size of these nanostructures can be controlled by the amount of capping agent material.

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Yashar Azizian-Kalandaragh was born in Namin/Ardabil/Iran in 1978. He received the B.Sc. degree from Mohaghegh Ardabili University, Ardabil, Iran, in 2002, the M.Sc. degree from Guilan University, Rasht, Iran, in 2005, and the Ph.D.

degree from Baku State University, Baku, Azerbaijan, in 2008, all in physics. He is involved in theoretical and experimental consideration of surface physics, biophysics, and fluid dynamics.