Laser-Assisted Low Temperature Processing of PZT Thin Films

1997 ◽  
Vol 493 ◽  
Author(s):  
Yongfei Zhu ◽  
Jinsong Zhu ◽  
Y. J. Song ◽  
S. B. Desu

ABSTRACTA novel method for lowering processing temperature of ferroelectric Pb(Zr1−xTix)O3 (PZT) thin films was developed utilizing a laser-assisted two-step process. In the first step, perovskite phase was initiated in the PZT films by subjecting the films to a fornace anneal at low temperatures in the range of 470 °C to 550 °C depending on the Zr/Ti ratio. Later, the films were laser-annealed (using krF excimer laser) at room temperature to grow the perovskite phase, and to improve microstructure and ferroelectric properties. It was found that this two-step process was very effective in producing excellent quality ferroelectric PZT films at low temperatures. It should be noted that although laser annealing of amorphous and/or pyrochlore films directly (one-step process) produces perovskite phase, the ferroelectric properties of these films, irrespective of the composition, were rather unattractive. Some possible reasons for the ineffectiveness of the one-step process were discussed.

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.


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.


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.


1996 ◽  
Vol 433 ◽  
Author(s):  
Hiromitsu Kurogi ◽  
Yukihiko Yamagata ◽  
Tomoaki Ikegami ◽  
Kenji Ebihara ◽  
Bok Yin Tong

AbstractPb(ZrxTi1−x)O3(PZT) thin films have excellent ferroelectric, optical, piezoelectric and pyroelectric properties. We prepared PZT thin films using the excimer laser ablation technique. A pulsed KrF excimer laser was used to ablate PZT bulk targets. We have studied optimum preparation conditions such as an oxygen pressure, a laser energy fluence and a substrate temperature.In this paper, we investigated the composition, crystallization and ferroelectric properties of the PZT films prepared under various deposition conditions.The X-ray diffraction (XRD) patterns showed that the PZT films prepared on MgO(100) substrates at 600°C and with a laser fluence of 2J/cm2 had a perovskite - pyrochlore mixed structure. The condition of 100 mTorr oxygen pressure provided high quality perovskite films. It is found that the stoichiometric composition of the deposited films is obtained in ambient oxygen of 100˜400 mTorr. The ferroelectric properties of the Pt/PZT/Pt/MgO structure were studied. The capacitance-voltage characteristics and the corresponding hysteresis loop of the dielectric-electric field curve were discussed.We also studied optical emission of the PZT plasma plume to understand quantitative relation between the PZT film quality and the ablation plume plasma. We identified spectral lines originated in Pb, Pb+, Zr, Zr+, Ti, Ti+, PbO and TiO. These spectral intensities have remarkable dependence on the ambient O2 pressure.


1999 ◽  
Vol 596 ◽  
Author(s):  
Tingkai Li ◽  
Sheng Teng Hsu ◽  
Yufei Gao ◽  
Mark Engelhard

AbstractThree kinds of oriented electrodes of Pt, Ir and Pt/Ir electrodes were prepared using electron beam evaporation techniques for deposition of PZT thin films. An oxide MOCVD reactor with liquid delivery system was used for the growth of PZT thin films. [Pb(thd)2], Zr(TMHD)4 and Ti(IPO)4 were dissolved in a mixed solvent of tetrahydrofuran or butyl ether, isopropanol and tetraglyme to form a precursor source. The deposition temperature and pressure were 500 - 650°C and 5 - 10 Torr, respectively. The experimental results showed PZT thin film deposited on various electrodes had different phase formation, microstructure and ferroelectric property. The X-ray patterns showed the perovskite phase of PZT was formed on both Ir and Pt/Ir electrodes at 550°C. The grain size of the PZT thin film increases after a further, higher temperature annealing. The as-deposited PZT thin film on Pt electrode exhibits pyrochlore phase at 550°C. The phase is transformed to perovskite phase after 650°C annealing. The experimental results also indicated that the MOCVD PZT thin film on Pt/Ir exhibits better ferroelectric and electrical properties compared to those deposited on Pt and Ir electrodes. A 300 nm thick PZT thin film on Pt/Ir electrode has a square, well saturated, and symmetrical hysteresis loop with 2Pr value of 40 μC/cm2 and 2Ec of 73 kV/cm at an applied voltage of 5 V. The hysteresis loop of the PZT thin film is almost saturated at 2 V. The leakage current of the film is 6.16 × 10−7 A/cm2 at 100 KV/cm. The electrode effects on ferroelectric properties of PZT thin films also have been investigated.


2012 ◽  
Vol 1397 ◽  
Author(s):  
Dirk Kaden ◽  
Hans-Joachim Quenzer ◽  
Martin Kratzer ◽  
Lorenzo Castaldi ◽  
Bernhard Wagner ◽  
...  

ABSTRACTIn this work high quality ferroelectric PZT films have been prepared in-situ by hot RF magnetron sputtering. 200 mm wafer were coated with PZT films of 1 μm and 2 μm thickness at sputter rates of 45 nm/min in a high volume production sputtering tool. The films were grown on oxidized Si substrates prepared either with sputtered Ti/TiO2/Pt, sputtered Ti/TiO2/Pt/TiO2 or evaporated Ti/Pt bottom electrodes at substrate holder temperatures in the range from 550 °C to 700 °C. At these temperatures, the material nucleates in the requisite piezoelectric perovskite phase without need of an additional post annealing treatment.The films were investigated with respect to their chemical composition and their crystallographic, piezoelectric and dielectric properties. At an intermediate chuck temperature of 600 °C the PZT thin films were characterized by a minimum volume fraction of secondary nonpiezoelectric phases. A Zr/(Zr+Ti) ratio of 0.53 has been achieved matching the morphotropic phase boundary. By improving the deposition process and poling procedure, a notable high e31,f coefficient of -17.3 C/m2 has been obtained. The corresponding longitudinal piezoelectric constant was determined to have an effective longitudinal piezoelectric coefficient d33,f of 160 pm/V.


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.


1999 ◽  
Vol 596 ◽  
Author(s):  
Jang-Sik Lee ◽  
Eung-Chul Park ◽  
Jung-Ho Park ◽  
Byung-Il Lee ◽  
Seung-Ki Joo

AbstractSelective nucleation and lateral growing method have been developed for high quality ferroelectric PZT(65/35) thin films using perovskite-phase PZT island seed. The PZT films on PZT seed island were transformed into the perovskite phase at temperatures as low as 540°C, which is 150°C lower than compared to that of PZT thin films deposited on Pt films. The temperature difference enables lateral growth without undesirable random nucleation. Maximum grain sizes of the perovskite-phase PZT films were determined by the annealing temperature. The PZT thin films show a leakage current density of 8×10−8 A/cm2, breakdown field of 1240 kV/cm, saturation polarization of 42 μC/cm2, and remanent polarization of 30 μC/cm2, whose values were maintained up to 2×1011 cycles. In this study, we show that when there was no grain boundary in the area measured, degradation such as fatigue and retention was not observed even with Pt electrodes. So the main source of degradation is the grain boundary in the PZT thin films.


2009 ◽  
Vol 08 (03) ◽  
pp. 299-303 ◽  
Author(s):  
SAJJAD DEHGHANI ◽  
ABDOLGHAFAR BARZEGAR ◽  
MOHAMMAD HOSSEIN SHEIKHI

Ferroelectric PbZr 1-x Ti x O 3 (PZT) thin films have been extensively investigated because of their excellent piezoelectric, pyroelectric, ferroelectric, and dielectric properties. Sol–gel synthesis and spin-coating are popular routes to the formation of high quality, dense, and crack-free thin films. In this work, high quality, crack-free PZT thin films have been prepared by sol–gel method via spin-coating on Pt/Ti/SiO2/Si substrate by different temperature processings. The crystallographic and morphological properties of the films have been analyzed by X-ray diffraction and scanning electron microscopy. The electrical properties of thin films including the permittivity, loss tangent, and polarization–voltage hysteresis loop were measured and compared for different films. Finally, by optimizing temperature processing, highly textured and high quality films of PZT with perovskite phase were obtained on Pt/Ti/SiO2/Si substrates.


2021 ◽  
Author(s):  
jie jiang ◽  
Lei Liu ◽  
Kuo Ouyang ◽  
Zhouyu Chen ◽  
Shengtao Mo ◽  
...  

Abstract With its excellent ferroelectric properties such as large dielectric constant and large remanent polarization, PZT thin films are extensively used in micro-sensors and other devices. In this study, the sol-gel process was used to fabricate Pb(Zr0.52Ti0.48)O3 thin films with Pb(ZrxTi1−x)O3 seed islands. The experimental consequences demonstrate that all the Pb(Zr0.52Ti0.48)O3 thin films with Pb(ZrxTi1−x)O3 seeds show pure perovskite phase with no other impurity phases, and the electrical properties of Pb(Zr0.52Ti0.48)O3 thin films modified by Pb(ZrxTi1−x)O3 seed islands with different Zr/Ti ratios are improved, such as remanent polarization increased, dielectric properties increased, coercive electric field decreased, leakage current density decreased, etc. In particular, the electrical properties of the Pb(Zr0.52Ti0.48)O3 thin films with Pb(ZrxTi1−x)O3 seed islands are the most optimal when the x is 0.52. This paper provides a new technique for optimizing the electrical properties of PZT thin films, which is of great significance for breaking through the bottleneck of the development of ferroelectric memory.


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