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International Refereed Journal of Engineering and Science (IRJES)
ISSN (Online) 2319-183X, (Print) 2319-1821
Volume 2, Issue 10 (October 2013), PP. 48-50

Preparation and Structural characterization of Pb(Zr0.52Ti0.48)O3
ceramics from solid state reaction method
Nitu Kumari1,2, Arun Singh2 and Jagdhar Mandal1
1

2

Department of Physics, TMB University, Bhagalpur, 812007 India
Advance Electronic and Nano-Materials Laboratory, Department of Physics, Jamia Millia Islamia University,
New
Delhi- 110025, India

Abstract:- This paper presents research results on the electro–mechanical behavior of piezoelectric ceramics for
use in actuator applications. The material being investigated is a lead zirconate titanate piezoelectric ceramic
with the composition Pb (Zr0.52Ti0.48)O3. The X-ray diffraction study shows the formation of tetragonal structure.
The sample is synthesized by the solid-state reaction method and then characterized by XRD, SEM and FT-IR.
Keywords:- Structural, FT-IR, PZT, solid solutions, XRD.

INTRODUCTION
The recent advances in Micro-Electro-Mechanical systems have created a strong interest in the
fabrication of small piezoelectric transducers for various applications in the field of sensors and actuators, where
they already have found industrial applications. Actuators that use direct expansion of piezoelectric materials are
the most usual ones [1,2] but in such a case the displacement is rather small. The displacement is achieved by
the strain induced unidirectional along an applied DC electric field, which makes possible extremely high
accuracy in positioning. Therefore, this investigation was conducted to obtain structural and electrical properties
of Lead Zirconate Titanate as a result of XRD, SEM, FT-IR.

EXPERIMENTAL PROCEDURE
The sample was prepared by the solid-state reaction method of PbO, ZrO2 and TiO2 were pre-calcined
at 800oC for 5 hrs. The mixed powders are pressed hydraulically to form disc shaped pellets 12 mm diameter
and 1.8 mm thick, with 5wt% polyvinyl alcohol (PVA) as a binder. The pellets are stacked in a covered
alumina crucible filled with PZ powders to prevent lead loss. Finally, the sintering is carried out a sintering
temperature at 1250oC for 2hrs to forms Pb(Zr0.52Ti0.48)O3 (PZT).

CHARACTERITION
“3.1Structural”
“3.11 XRD”
Room temperature XRD patterns of the sintered pellets of PZT are shown in Fig.1. The X-ray
diffraction (XRD) spectra of the sintered samples are recorded in the 2θ range of 20° - 70° with step of 0.02° and
scanning rate of 1°/min. These have sharp and single phase of the sample was confirmed by comparing the
pattern with the earlier reported data which indicating better homogeneity and crystallization of the samples. All
the reflection peaks were indexed and lattice parameters of the compounds were calculated using a powder
diffraction refinement computer program (PowderX) [C. Dong, 1999] and the crystal structure is found to be
tetragonal with space group p4mm [3]. The diffraction peaks of PZT were indexed according to previously
reported results [4].
The value of lattice parameters „c‟ of PZT ceramic composition were found to be 4.123 Å where as “a
= b” is 4.008 Å. The estimated value of lattice strain (tetragonality) c/a is 1.029. The values bear a resemblance
to tetragonal unit cell. The volume of the unit cell is found to be 73.441 Å3. The bulk density of the sintered
pellets was measured by Archimedes liquid displacement method and the relative density of the sample is found
to be 94% of the theoretical density

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Preparation and Structural characterization of Pb(Zr0.52Ti0.48)O3 ceramics…

“3.12 Scanning electron microscopy”
Figure 2.shows the scanning electron micrograph (SEM) of sintered PZT ceramics. The micrographs
indicate that the inhomogeneous distribution of polycrystalline grain throughout the surface of material. The
average grain size calculated from the micrograph of PZT is 0.20 µm.

“3.13FT-IR study”
Fourier transform infrared (FT-IR) spectra of polycrystalline Pb(Zr0.52Ti0.48)O3 ceramic compositions
were carried out in the wave number range of 1200 – 400 cm-1, using Perkin Elmer FT-IR spectrometer, the
spectral resolution of the instrument is 0.4cm-1. Before recording the transmission spectra, KBr powder was
heated to evaporate the excess moisture and then thin pellets were made using the specimen powder and space
pure KBr in the ratio 1:20 by weight shown in Fig. 3.There were two distinct absorption bands at 597 cm -1(v2),
536 cm -1(v1) observed. These absorption bands resemble with the reported FTIR observations of PZT
ceramics.25 In the perovskite structures the TiO6 octahedral is responsible for two distinct vibration modes: one
at 563 cm -1 attributed to bending vibration and another at 597 cm -1 due to stretching of octahedral [5,6]. The
absorption bands ν1 represent bending modes while ν2 represent stretching modes in the BO6 (TiO3 and ZrO3)
octahedron in ABO3 structure.

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Preparation and Structural characterization of Pb(Zr0.52Ti0.48)O3 ceramics…

CONCLUSION
In this work, the synthesis of PZT ceramics in the region of the morphotropic Phase Boundary (MPB)
has been investigated. The ceramics exhibited a complete tetragonal phase for this samples PNZT ceramics
prepared by a high-temperature, solid-state reaction technique reveal good homogeneity and formation of a
single-phase compound with tetragonal structure. SEM indicates homogeneous distribution of polycrystalline
grain throughout the surface of material..
Ackonwledgement
The authors are thankful to the DST, Ministry of Science and Technology, Govt. of India for financial
support. One of the authors (A.S.) would like to thank the DST, Ministry of Science and Technology, Govt. of
India for award of Young Scientist.

REFERENCE
[1].

[2].

[3].
[4].
[5].
[6].
[7].
[8].

J.P. Cruz, E. Joanni, P.M. Vilarinho, A.L.Kholkin, “Thickness Effect on the Dielectric, Ferroelectric,
and Piezoelectric Properties of Ferroelectric Lead Zirconate Titanate Thin Films,” J. Appl. Phys. 108,
1141 06 (2010).
Muhtar Ahart, addury Somayazulu, R. E. Cohen, P. Ganesh, Przemyslaw Dera, Ho-kwang Mao,
Russell J. Hemley, Yang Ren, Peter Liermann & Zhigang Wu,“ Origin of Morphotropic Phase
Boundaries in Ferroelectrics,” Nature 451, 545-548. 31 January (2008).
H. Yokata, N. Zhang, A.E. Taylor, P.A. Thoms and A.M. Glazer,“Crystal “Crystal structure of the
rhombohedral phase of PbZr1−xTixO3 ceramics at room temperature”, Phys. Rev. B 80,104109 (2009)..
S.R. Shannigrahi, R.N.P. Choudhari, H.N. Acharya Material Science and Engineering B 56, 3139(1999).
Last J. T, Phys. Rev. 105, 1740 (1957).
R A Nyquist, and R O Kagel, (New York: Academic Presss) p 100 (1971).
J. Suchanicz, D. Sitko, N.-T. H. Kim-Ngan, and A. G. Balogh, ”electric properties of soft PZT
ceramics under combined electric and mechanic fields”, J. Appl. Phy. 104, 094106 (2008).
L.B. Kong , W. Zhu, O.K. Tan, “Preparation and characterization of Pb (Zr0.52 Ti0.48)O3ceramics from
high-energy ball milling powders”, Materials Letters 42 (2000). 232–239.

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International Refereed Journal of Engineering and Science (IRJES)

  • 1. International Refereed Journal of Engineering and Science (IRJES) ISSN (Online) 2319-183X, (Print) 2319-1821 Volume 2, Issue 10 (October 2013), PP. 48-50 Preparation and Structural characterization of Pb(Zr0.52Ti0.48)O3 ceramics from solid state reaction method Nitu Kumari1,2, Arun Singh2 and Jagdhar Mandal1 1 2 Department of Physics, TMB University, Bhagalpur, 812007 India Advance Electronic and Nano-Materials Laboratory, Department of Physics, Jamia Millia Islamia University, New Delhi- 110025, India Abstract:- This paper presents research results on the electro–mechanical behavior of piezoelectric ceramics for use in actuator applications. The material being investigated is a lead zirconate titanate piezoelectric ceramic with the composition Pb (Zr0.52Ti0.48)O3. The X-ray diffraction study shows the formation of tetragonal structure. The sample is synthesized by the solid-state reaction method and then characterized by XRD, SEM and FT-IR. Keywords:- Structural, FT-IR, PZT, solid solutions, XRD. INTRODUCTION The recent advances in Micro-Electro-Mechanical systems have created a strong interest in the fabrication of small piezoelectric transducers for various applications in the field of sensors and actuators, where they already have found industrial applications. Actuators that use direct expansion of piezoelectric materials are the most usual ones [1,2] but in such a case the displacement is rather small. The displacement is achieved by the strain induced unidirectional along an applied DC electric field, which makes possible extremely high accuracy in positioning. Therefore, this investigation was conducted to obtain structural and electrical properties of Lead Zirconate Titanate as a result of XRD, SEM, FT-IR. EXPERIMENTAL PROCEDURE The sample was prepared by the solid-state reaction method of PbO, ZrO2 and TiO2 were pre-calcined at 800oC for 5 hrs. The mixed powders are pressed hydraulically to form disc shaped pellets 12 mm diameter and 1.8 mm thick, with 5wt% polyvinyl alcohol (PVA) as a binder. The pellets are stacked in a covered alumina crucible filled with PZ powders to prevent lead loss. Finally, the sintering is carried out a sintering temperature at 1250oC for 2hrs to forms Pb(Zr0.52Ti0.48)O3 (PZT). CHARACTERITION “3.1Structural” “3.11 XRD” Room temperature XRD patterns of the sintered pellets of PZT are shown in Fig.1. The X-ray diffraction (XRD) spectra of the sintered samples are recorded in the 2θ range of 20° - 70° with step of 0.02° and scanning rate of 1°/min. These have sharp and single phase of the sample was confirmed by comparing the pattern with the earlier reported data which indicating better homogeneity and crystallization of the samples. All the reflection peaks were indexed and lattice parameters of the compounds were calculated using a powder diffraction refinement computer program (PowderX) [C. Dong, 1999] and the crystal structure is found to be tetragonal with space group p4mm [3]. The diffraction peaks of PZT were indexed according to previously reported results [4]. The value of lattice parameters „c‟ of PZT ceramic composition were found to be 4.123 Å where as “a = b” is 4.008 Å. The estimated value of lattice strain (tetragonality) c/a is 1.029. The values bear a resemblance to tetragonal unit cell. The volume of the unit cell is found to be 73.441 Å3. The bulk density of the sintered pellets was measured by Archimedes liquid displacement method and the relative density of the sample is found to be 94% of the theoretical density www.irjes.com 48 | Page
  • 2. Preparation and Structural characterization of Pb(Zr0.52Ti0.48)O3 ceramics… “3.12 Scanning electron microscopy” Figure 2.shows the scanning electron micrograph (SEM) of sintered PZT ceramics. The micrographs indicate that the inhomogeneous distribution of polycrystalline grain throughout the surface of material. The average grain size calculated from the micrograph of PZT is 0.20 µm. “3.13FT-IR study” Fourier transform infrared (FT-IR) spectra of polycrystalline Pb(Zr0.52Ti0.48)O3 ceramic compositions were carried out in the wave number range of 1200 – 400 cm-1, using Perkin Elmer FT-IR spectrometer, the spectral resolution of the instrument is 0.4cm-1. Before recording the transmission spectra, KBr powder was heated to evaporate the excess moisture and then thin pellets were made using the specimen powder and space pure KBr in the ratio 1:20 by weight shown in Fig. 3.There were two distinct absorption bands at 597 cm -1(v2), 536 cm -1(v1) observed. These absorption bands resemble with the reported FTIR observations of PZT ceramics.25 In the perovskite structures the TiO6 octahedral is responsible for two distinct vibration modes: one at 563 cm -1 attributed to bending vibration and another at 597 cm -1 due to stretching of octahedral [5,6]. The absorption bands ν1 represent bending modes while ν2 represent stretching modes in the BO6 (TiO3 and ZrO3) octahedron in ABO3 structure. www.irjes.com 49 | Page
  • 3. Preparation and Structural characterization of Pb(Zr0.52Ti0.48)O3 ceramics… CONCLUSION In this work, the synthesis of PZT ceramics in the region of the morphotropic Phase Boundary (MPB) has been investigated. The ceramics exhibited a complete tetragonal phase for this samples PNZT ceramics prepared by a high-temperature, solid-state reaction technique reveal good homogeneity and formation of a single-phase compound with tetragonal structure. SEM indicates homogeneous distribution of polycrystalline grain throughout the surface of material.. Ackonwledgement The authors are thankful to the DST, Ministry of Science and Technology, Govt. of India for financial support. One of the authors (A.S.) would like to thank the DST, Ministry of Science and Technology, Govt. of India for award of Young Scientist. REFERENCE [1]. [2]. [3]. [4]. [5]. [6]. [7]. [8]. J.P. Cruz, E. Joanni, P.M. Vilarinho, A.L.Kholkin, “Thickness Effect on the Dielectric, Ferroelectric, and Piezoelectric Properties of Ferroelectric Lead Zirconate Titanate Thin Films,” J. Appl. Phys. 108, 1141 06 (2010). Muhtar Ahart, addury Somayazulu, R. E. Cohen, P. Ganesh, Przemyslaw Dera, Ho-kwang Mao, Russell J. Hemley, Yang Ren, Peter Liermann & Zhigang Wu,“ Origin of Morphotropic Phase Boundaries in Ferroelectrics,” Nature 451, 545-548. 31 January (2008). H. Yokata, N. Zhang, A.E. Taylor, P.A. Thoms and A.M. Glazer,“Crystal “Crystal structure of the rhombohedral phase of PbZr1−xTixO3 ceramics at room temperature”, Phys. Rev. B 80,104109 (2009).. S.R. Shannigrahi, R.N.P. Choudhari, H.N. Acharya Material Science and Engineering B 56, 3139(1999). Last J. T, Phys. Rev. 105, 1740 (1957). R A Nyquist, and R O Kagel, (New York: Academic Presss) p 100 (1971). J. Suchanicz, D. Sitko, N.-T. H. Kim-Ngan, and A. G. Balogh, ”electric properties of soft PZT ceramics under combined electric and mechanic fields”, J. Appl. Phy. 104, 094106 (2008). L.B. Kong , W. Zhu, O.K. Tan, “Preparation and characterization of Pb (Zr0.52 Ti0.48)O3ceramics from high-energy ball milling powders”, Materials Letters 42 (2000). 232–239. www.irjes.com 50 | Page