FERROELECTRIC CHARACTERIZATION OF

RARE EARTH METAL NIOBIUM DOPED

PZT(52/48) NANOCERAMICS FOR SENSOR
APPLICATIONS

Under the guidance of

DR. M. PRABHU
Department Of Nanotechnology
NOORUL ISLAM CENTRE FOR HIGHER EDUCATION
KUMARACOIL, TAMIL NADU-INDIA 629180
 INTRODUCTION
• Ferroelectric PZT powders have attracted a growing practical
interest.

• They have excellent dielectric, piezoelectric and pyroelectric

properties.

• Can be used for actuating and sensing applications.

• Used in FRAM and MEMS.

• The PZT composition with Zr/Ti ratio 52/48 show high

ferroelectric properties.

• Substitution of a higher valence cation niobium (Nb5+ ) results

in high ferroelectric properties.
 LITERATURE REVIEW
• Ferroelectric properties of PNZT having Zr/Ti ratio of 52/48 has been
studied very rarely.

• Klissurska et al. observed that for concentration about 2.0 mol % Nb the
ferroelectric properties were degraded.

• Araujo et al. prepared Nb doped PZT thin films with 5.0 mol % Nb,
obtaining higher values of remanent polarization.

• The effect of Nb doping in PZT bulk ceramics has been studied by Varela et
al. showing 0.5 mol % Nb increases remanent polarization.

• Pereira et al.reported that the Nb oxide is a good sintering aid for PZT
(65/35)-based materials.
 EXPERIMENTAL DETAILS
• PNZT ceramic samples with composition Pb(1-x)Nbx(Zr0.52Ti0.48)O3,
where x = 0, 0.02, 0.05, were prepared by the sol–gel route.

CHEMICAL MATERIALS USED

• Citric acid monohydrate (99.5% AR-Merck)

• Lead (ll) nitrate (99.0%-Avra)
• Zirconium oxychloride (98.0% AR-Thomas Baker)
• Titanium tetraisopropoxide (98% LR-Spectrochem)
• Niobium pentoxide (99.99% AR-Spectrochem)
• Nitric acid (min. 69.0% GR-Merck)
 SOL-GEL SYNTHESIS
• As a first step, citric acid monohydrate was dissolved in 100 ml water and
the solution was stirred well for 10 min continuously.

• After getting a homogeneous solution, niobium pentoxide, zirconium

oxychloride and titanium tetra isopropoxide were added followed by lead
nitrate.

• 5 ml of nitric acid was added to improve the process.

• The complex solution was stirred well for 1 h at room temperature to get a
clean and homogeneous solution.

• Then, the temperature was gradually increased to 80 C.

• Finally, the gel formed was dried at 80 C,the resultant powder was heated
around 850 C for 3 h to obtain the PZT powder.
 THERMAL ANALYSIS
• The thermogravimetric analysis (TGA) and differential thermal analysis
(DTA) of the PNZT powders were carried out with the heating rate of 20
C/min.
• TG curves exhibit two major losses; the first one located between 180 and
246 C (of about 9%) may be due to the elimination of water content from
the prepared sample and the second occurring between 290 and 380 C (of
about 18%) due to the major decomposition reaction of citric acid and
other organic compounds.
• The DTA curves are in conformity with these observations. There are three
exothermic peaks in DTA curve at 156 C, 346 C and 475 C. The first one
may be corresponding to the combustion of most of the organic species
entrapped in PNZT polymerized gel such as citric acid and titanium (lV)
isopropoxide.
• The second with a temperature range of 290 C–380 C is due to the
decomposition of organic compounds, removed nitrates and the
combustion of residual carbon contents.
• At 475 C ,crystallization of PZT begins.
TG/DTA CURVE
 SURFACE MORPHOLOGY
• SEM IMAGES OF PURE PZT
• (a) 10000x (b) 1000x

5 um
 SURFACE MORPHOLOGY
• SEM IMAGES OF NIOBIUM DOPED PZT
• (a) 20000x (b) 50000x
 REMAINING WORK

• DIELECTRIC STUDIES

• FERROELECTRIC MEASUREMENTS
 APPLICATIONS
• MEMS -Microelectromechanical systems

• Sensors -pressure,temperature etc.

• FERAM – Ferroelectric random access memory

• Actuators

• Optoelectronic devices
THANK YOU