Effect of Pb Excess Content on Microstructure and Electrical Properties of Sol Gel Derived PZT Thin Films

1999 ◽  
Vol 596 ◽  
Author(s):  
Zhan-jie Wang ◽  
Ryutaro Maeda ◽  
Kaoru Kikuchi

AbstractLead zirconate titanate (PZT) thin films were fabricated by a three-step heat-treatment process which involves the addition of -10, 0 and 10 mol% excess Pb to the starting solution and spin coating onto Pt/Ti/SiO2/Si substrates. Crystalline phases as well as preferred orientations in PZT films were investigated by X-ray diffraction analysis (XRD). The microstructure and composition of the films were studied by scanning electron microscopy (SEM), transmission electron microscopy (TEM) and electron probe microanalysis (EPMA), respectively. The well-crystallized perovskite phase and the (100) preferred orientation were obtained by adding 10% excess Pb to the starting solution. It was found that PZT films to which 10% excess Pb was added had better electric properties. The remanent polarization and the coercive field of this film were 34.8 μC/cm2 and 41.7 kV/cm, while the dielectric constant and loss values measured at 1 kHz were approximately 1600 and 0.04, respectively. Dielectric and ferroelectric properties were correlated to the microstructure of the films.

2007 ◽  
Vol 14 (02) ◽  
pp. 229-234
Author(s):  
SARAWUT THOUNTOM ◽  
MANOCH NAKSATA ◽  
KENNETH MACKENZIE ◽  
TAWEE TUNKASIRI

Lead zirconate titanate (PZT) films with compositions near the morphotropic phase boundary were fabricated on Pt (111)/ Ti / SiO 2/ Si (100) using the triol sol–gel method. The effect of the pre-heating temperature on the phase transformations, microstructures, electrical properties, and ferroelectric properties of the PZT thin films was investigated. Randomly oriented PZT thin films pre-heated at 400°C for 10 min and annealed at 600°C for 30 min showed well-defined ferroelectric hysteresis loops with a remnant polarization of 26.57 μC/cm2 and a coercive field of 115.42 kV/cm. The dielectric constant and dielectric loss of the PZT films were 621 and 0.0395, respectively. The microstructures of the thin films are dense, crack-free, and homogeneous with fine grains about 15–20 nm in size.


2006 ◽  
Vol 326-328 ◽  
pp. 613-616
Author(s):  
Dae Jin Yang ◽  
Seong Je Cho ◽  
Jong Oh Kim ◽  
Won Youl Choi

Lead zirconate titanate (Pb(Zr0.48Ti0.52)O3 or PZT) films were grown on platinized silicon wafers (Pt/SiO2/Si) by d.c. reactive sputtering method with multi targets. The Pb content of PZT films has been widely recognized as affecting not only the phase formation and microstructure but also the dielectric and ferroelectric properties. Pb content of PZT films was controlled by the variation of Pb target current. The relation between Pb content and Pb target current was expressed as y=0.89x-11.09. The x and y are Pb target current and Pb content, respectively. The pyrochlore phase was transformed to perovskite phase as Pb content was increased. This phase transformation improved the ferroelectric properties of PZT films. In PZT films with perovskite phase, fatigue properties were not improved with excess Pb content. Fatigue properties of PZT films began to be fatigued after 106 switching cycles and coincided with the typical PZT fatigue behavior. Excess Pb content (Pb vacancy) did not affect the fatigue properties of PZT films.


2012 ◽  
Vol 2012 ◽  
pp. 1-9
Author(s):  
B. S. Li

Lead zirconate titanate (PZT) thin films with the morphotropic phase boundary composition (Zr/Ti = 52/48) have been prepared using a modified diol-based sol-gel route by introducing 1–5 mol% barium titanate (BT) nanoseeds into the precursor solution on platinized silicon substrates (Pt/Ti/SiO2/Si). Macroscopic electric properties of PZT film with nanoparticle showed a significant improvement of ferroelectric properties. This work aims at the systematic study of the local switching polarization behavior during fatigue in PZT films with and without nanoparticles by using very recent developed scanning piezoelectric microscopy (SPM). We show that the local fatigue performance, which is characterized by variations of local piezoloop with electric cycles, is significantly improved by adding some nanoseeds. It has been verified by scanning electron microscope (SEM) that the film grain morphology changes from columnar to granular structure with the addition of the nanoseeds. On the other hand, the existence of PtxPb transition phase, which existed in interface at early crystallization stage of pure PZT thin film, deteriorates the property of the interface. These microstructures and the interfaces of these films significantly affect the electrons injection occurred on the interfaces. The domain wall pinning induced by injected electrons and the succeeding penetration into the films is discussed to explain the fatigue performance.


1998 ◽  
Vol 541 ◽  
Author(s):  
Chang Jung Kim ◽  
Tae-Young Kim ◽  
Ilsub Chung ◽  
In Kyung Yoo

AbstractThe PZT thin films were fabricated to investigate the effect of sol-gel processing parameters on the physical and the electrical properties. The films were made with different amount of excess Pb precursors and drying temperatures, and then annealed in various ambients. The physical properties of the films such as crystallinity and microstructure were evaluated using x-ray diffraction, scanning electron microscopy and atomic force microscopy. The ferroelectric properties and current density characteristics of the films were investigated using a standarized feiroelectric test system and pA meter, respectively. It is found that the drying temperature was playing a key role in the formation of the secondary phase on the PZT thin films. In addition, it turned out that the use of nitrogen as an annealing ambient promoted overall ferroelectric properties, when compared to oxygen ambients.


2007 ◽  
Vol 280-283 ◽  
pp. 239-242 ◽  
Author(s):  
Wen Gong ◽  
Xiang Cheng Chu ◽  
Jing Feng Li ◽  
Zhi Lun Gui ◽  
Long Tu Li

Lead zirconate titanate (PZT) thin films with a composition near the morphotropic phase boundary were deposited on silicon wafers by using a modified sol-gel method. Introducing a seeding layer between the interface of PZT film and platinum electrode controlled the texture of PZT films. The lead oxide seeding layer results in highly (001)-textured PZT film, while the titanium dioxide seeding layer results in (111)-textured one. SEM and XRD were used to characterize the PZT thin films. The ferroelectric and piezoelectric properties of the PZT films were evaluated and discussed in association with different preferential orientations.


2000 ◽  
Vol 657 ◽  
Author(s):  
C.F. Knollenberg ◽  
T.D. Sands ◽  
A.S. Nickles ◽  
R.M. White

ABSTRACTSputter-deposited piezoelectric lead zirconate titanate (PZT) thin films with Ti/Pt and polysilicon electrode layers are being investigated for use in Microelectromechanical Systems (MEMS). Existing research shows the nucleation of the perovskite phase of the PZT is linked to the lattice spacing of the underlying Pt electrode and/or seed layers, and is key in obtaining PZT layers with good piezoelectric/ferroelectric properties. Our research with piezoelectric PZT films on Ti/Pt electrode layers aims at employing these films to generate and receive acoustic waves in flexural plate wave devices (FPWs). Our experiments indicate the formation of a random polycrystalline perovskite phase is linked to the emergence of oriented <100> Pt grains within the dominant <111>-oriented crystal structure during rapid thermal annealing in an oxygen environment. Pt films annealed in nitrogen, in contrast, retained their <111> preferential orientation without the formation of Pt <100> grains. PZT films deposited on these electrodes and annealed in nitrogen were strongly oriented in the <111> direction, but exhibited lossy ferroelectric behavior and were prone to delamination. We are also investigating the feasibility of using doped polysilicon electrode layers with PZT thin films. The multiple layers used with the Pt electrode (Pt, Ti, and SiO2 adhesion layer) have significant interactions with one another, and replacing these layers with a single electrode layer should alleviate these complications. A low-temperature PZT deposition process (300°C) and short annealing cycles (30 sec.), coupled with a TiO2 barrier/seed layer should prevent interdiffusion and reactions between the polysilicon and PZT layers. Our experiments show that PZT films deposited and annealed on doped polysilicon layers develop a random polycrystalline perovskite phase, but are subject to tensile cracking. The use of polysilicon as an electrode layer should also facilitate the integration of piezoelectric PZT layers with polysilicon surface micromachined structures using SiGe sacrificial layers.


1993 ◽  
Vol 310 ◽  
Author(s):  
P. H. Ansari ◽  
A. Safari

AbstractFerroelectric lead zirconate titanate (PZT) films with a composition near the morphotropic phase boundary have been deposited by if magnetron sputtering on a Si substrate coated with silicon oxide, titanium, and platinum (Si/SiO2/Ti/Pt). Substrate temperature and oxygen partial pressure were changed during deposition to prepare films with controlled stoichiometry and perovskite structure. The effects of lead titanate (PT) as a buffer layer were investigated. Thin films of PT/PZT have a dielectric constant of 800 with a dissipation factor of 0.04 at 1 kHz. The remnant polarization of 8μC/cm2 and the coercive field of 50 kV/cm were measured. The effect of processing on the formation of perovskite phase and the electrical properties will be discussed.


1997 ◽  
Vol 12 (4) ◽  
pp. 1043-1047 ◽  
Author(s):  
Chang Jung Kim ◽  
Dae Sung Yoon ◽  
Joon Sung Lee ◽  
Chaun Gi Choi ◽  
Kwangsoo No

The lead zirconate titanate (PZT) thin films were fabricated using sol-gel spin coating onto Pt/Ti/glass substrates. Effects of the holding time for pyrolysis and the coating cycle on the preferred orientation of the PZT thin films were studied. The films were fabricated with different coating cycles (3, 5, 7, 9, 11), dried at 330 °C for different holding times (5, 30, 60 min), and then annealed at the same temperature of 650 °C using rapid thermal annealing (RTA). The preferred orientations of the films were investigated using x-ray diffraction and glancing angle x-ray diffraction. The microstructure and the selected area diffraction pattern of the PZT thin films were also investigated using scanning electron microscopy (SEM) and transmission electron microscopy (TEM), respectively.


1995 ◽  
Vol 10 (12) ◽  
pp. 3149-3159 ◽  
Author(s):  
Ellen M. Griswold ◽  
L. Weaver ◽  
M. Sayer ◽  
I.D. Calder

The crystallization kinetics of the pyrochlore to perovskite phase transformation in lead zirconate titanate (PZT) thin films have been analyzed using rapid thermal processing (RTP). Sol-gel PZT thin films, fabricated on platinum electrodes, were annealed at 550 °C to 650 °C with hold times ranging from 1 s to 5 min. Glancing angle x-ray diffraction (XRD) was used for depth profiling to identify the location of phases in the films. Transmission electron microscopy (TEM) provided information on grain structure, nucleation, and growth. The phase information was correlated to the ferroelectric and dielectric properties. The perovskite phase nucleated in the pyrochlore phase throughout the film thickness, and at 650 °C the transformation was complete in 15 s. Fast growing (100) PZT nucleated at the platinum and consumed a small-grained matrix until a columnar structure was obtained. A ramp rate of 100 °C/s was sufficiently fast to prevent transformation during heating and allowed the direct application of an Avrami model for transformation kinetics. An activation energy of 610 kJ/mol was determined.


2012 ◽  
Vol 1427 ◽  
Author(s):  
Kanu priya Sharma ◽  
Thomas Oseroff ◽  
Leda Lunardi

ABSTRACTCrack free lead zirconate titanate (PZT) films for piezoelectric based MEMS devices have been prepared by a multiple coating sol gel process on platinized silicon (100) substrates. Rapid thermal annealing and Conventional furnace annealing were used for densification and crystallization of the amorphous PZT films. Scanning electron microscopy (SEM), Transmission electron microscopy (TEM) and Atomic force microscopy (AFM) were used to observe surface film morphology and grain growth. The phase content of the films was analyzed using X-ray diffraction. The role of intermetallics formed during the heat treatment in the growth of different orientations has also been observed. Film aging critical for device performance has been observed and methods to revert aging effects have been examined and discussed.


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