Aging Characteristics of a Hybrid Sol-gel Pb(Zr, Ti)O3 Precursor Solution

1997 ◽  
Vol 12 (4) ◽  
pp. 1022-1030 ◽  
Author(s):  
Timothy J. Boyle ◽  
Duane Dimos ◽  
Robert W. Schwartz ◽  
Todd M. Alam ◽  
Michael B. Sinclair ◽  
...  
Keyword(s):  
Lead Zirconate Titanate ◽  
Sol Gel ◽  
Precursor Solution ◽  
Extended Period ◽  
Lead Zirconate ◽  
Film Properties ◽  
Ph Measurements ◽  
Chemical Aging ◽  
H Nmr ◽  
Material Forming

The “aging” characteristics of an acetic acid/methanol solvent-based lead zirconate titanate (PZT) precursor solution, prepared by the Inverted Mixing Order (IMO) process, have been studied for an extended period of time. The changes in film properties were characterized using optical microscopy, optical scattering, and ferroelectric testing. Films generated from the IMO process exhibit an increase in thickness as a function of solution age due to chemical “aging” (esterification) of the precursor solution. This increased thickness results in a decrease in the microstructural uniformity, which affects the electrical and optical properties. In order to understand and eventually control this phenomenon, we have quantified the “aging” of this solution using a variety of analytical methods, including 1H NMR spectroscopy, pH measurements, and Fourier transform infrared (FTIR) spectroscopy. It is of note that we have discovered a method that circumvents this “aging” problem by removal of the volatile material, forming an IMO powder which can be redissolved to produce high quality PZT thin films whenever desired.

scholarly journals Local Fatigue Evaluation in PZT Thin Films with Nanoparticles by Piezoresponse Force Microscopy

2012 ◽  
Vol 2012 ◽  
pp. 1-9
Author(s):  
B. S. Li
Keyword(s):  
Thin Films ◽  
Lead Zirconate Titanate ◽  
Ferroelectric Properties ◽  
Sol Gel ◽  
Precursor Solution ◽  
Grain Morphology ◽  
Piezoresponse Force Microscopy ◽  
Lead Zirconate ◽  
Fatigue Performance ◽  
Pzt Thin Films

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.

scholarly journals Effects of Acetylacetone Additions on PZT Thin Film Processing

1994 ◽  
Vol 361 ◽  
Author(s):  
Robert W. Schwartz ◽  
R.A. Assink ◽  
D. Dimos ◽  
M.B. Sinclair ◽  
T.J. Boyle ◽  
...  
Keyword(s):  
Thin Film ◽  
Lead Zirconate Titanate ◽  
Sol Gel ◽  
Precursor Solution ◽  
Lead Zirconate ◽  
Pzt Thin Film ◽  
Precursor Structure ◽  
Drying Behavior ◽  
Ceramic Microstructure ◽  
Gel Processing

ABSTRACTSol-gel processing methods are frequently used for the fabrication of lead zirconate titanate (PZT) thin films for many electronic applications. Our standard approach for film fabrication utilizes lead acetate and acetic acid modified metal alkoxides of zirconium and titanium in the preparation of our precursor solutions. This report highlights some of our recent results on the effects of the addition of a second chelating ligand, acetylacetone, to this process. We discuss the changes in film drying behavior, densification and ceramic microstructure which accompany acetylacetone additions to the precursor solution and relate the observed variations in processing behavior to differences in chemical precursor structure induced by the acetylacetone ligand. Improvements in thin film microstructure, ferroelectric and optical properties are observed when acetylacetone is added to the precursor solution.

Thickness Dependence of the Electrical Properties of Sol-Gel Derived Lead Zirconate Titanate Thin Films with (111) and (100) Texture

1997 ◽  
Vol 493 ◽  
Author(s):  
F. Chu ◽  
F. Xu ◽  
J. Shepard ◽  
S. Trolier-McKinstry
Keyword(s):  
Dielectric Constant ◽  
Lead Zirconate Titanate ◽  
Remanent Polarization ◽  
Critical Thickness ◽  
Piezoelectric Properties ◽  
Sol Gel ◽  
Precursor Solution ◽  
Lead Zirconate ◽  
Thickness Dependence ◽  
Pzt Films

ABSTRACTCrack-free (111) and (100)-textured Pb(Zr0.52Ti0.48)O3 films with thicknesses ranging from 0.25 to 2.5 μm were prepared using a methoxyethanol-based precursor solution, multiple spin-coating and multiple crystallization steps. The thickness dependence of the dielectric, ferroelectric and piezoelectric properties were investigated on both (111) and (100) oriented PZT films. In both cases, the degree of preferred orientation did not change with thickness. It is found that the dielectric constant, remanent polarization and piezoelectric coefficients (d33 and d31) increase with increasing film thickness. The (100)-textured film showed higher dielectric constant but lower remanent polarization relative to (111) textured film. 1 μm was identified to be a critical thickness that marks the change of dielectric, ferroelectric and piezoelectric behaviors as a function of thickness.

Preparation and Characterization of Pb(Zr0.52Ti0.48)O3 Powders and Thin Films by a Sol-gel Route

2000 ◽  
Vol 15 (6) ◽  
pp. 1336-1341 ◽  
Author(s):  
Dage Liu ◽  
Hongxi Zhang ◽  
Zhong Wang ◽  
Liancheng Zhao
Keyword(s):  
Thin Films ◽  
Lead Zirconate Titanate ◽  
Lead Acetate ◽  
Sol Gel ◽  
Precursor Solution ◽  
Lead Zirconate ◽  
Tetrabutyl Titanate ◽  
Sol Gel Process ◽  
High Fatigue

Lead zirconate titanate [Pb(ZrxTi1−x)O3 (PZT)] powders and ferroelectric thin films with a composition near the morphotropic phase boundary [Pb(Zr0.52Ti0.48)O3] were prepared by a modified sol-gel process using zirconium oxynitrate-2-hydrate as the zirconium source and ethylene glycol as solvent. The precursor solution was prepared from lead acetate-3-hydrate, tetrabutyl titanate, and zirconium oxynitrate-2-hydrate. Perovskite PZT powders were obtained after sintering at 450 °C for 2 h. Films rapid-thermally annealed at 650 °C for 1 min formed well-crystallized perovskite.Microstructures of these films indicated the presence of nano-sized grains (∼50 nm). The remnant polarization was 28.5 μC/cm2, and the coercive field was 39.8 kV/cm. Ferroelectric polarization fatigue test of In/PZT/Pt/Ti/SiO2/Si showed a high fatigue resistance up to 3 × 1010 cycles before Pr decreased by 50%.

Annealing Procedures and Their Effects on PZT/Nanoparticle Thin Films via a Modified Sol-Gel Process

2007 ◽  
Author(s):  
Clayton Easter ◽  
Chad B. O’Neal
Keyword(s):  
Cooling Rate ◽  
Lead Zirconate Titanate ◽  
Sol Gel ◽  
Precursor Solution ◽  
Lead Zirconate ◽  
Base Layer ◽  
Slow Cooling ◽  
Final Annealing ◽  
Free Film ◽  
The Individual

The development of lead zirconate titanate (PZT) films can be a fairly troublesome process when trying to obtain a viable thick crack-free film. Traditional methods for film fabrication via a pure sol-gel solution provide the best results, but still can have many problems. This paper maps out the specific spin-coating and annealing steps used in order to achieve a PZT film with minimal-to-no cracking and/or delamination. A seed layer of PbTiO3 (PT) was used in order to create nucleation sites for the subsequent PZT layers, virtually eliminating any delamination. All layers, including the PT base layer, were spin-coated at 3000 rpm onto a 100-mm silicon wafer (previously sputtered with Ti and Pt for adhesive and conductive purposes, respectively) and soft-baked at 150 °C for 10 min. Initial annealing procedures produced severe cracking, a result of the relatively high cooling rates through the Curie temperature (∼350 °C). The annealing process was refined, for individual layers, to 550°C for 120 s, with a cooling rate of 0.042 °/s between 400 and 300 °C. Final annealing was conducted at 600 °C for 30 min, with a cooling rate of 0.028 °/s between 400 and 300 °C. The resulting PZT layer was virtually crack-free. Platinum was sputtered again subsequent to PZT deposition in order to pole the piezoelectric material. A PZT/nanoparticle powder mixture was also investigated as the piezoelectric layer. PZT nanoparticles were suspended in the sol-gel precursor solution and then spin-coated also at 3000 rpm onto a 100-mm wafer and soft-baked at 150 °C for 10 min. The relatively slow cooling rate was extended between 500 and 100 °C in order to prevent any cracking that might occur along grain boundaries between the individual PZT nanoparticles. The resulting film was crack-free, however displaying areas of agglomerated nanoparticles.

Pb(Zr,Ti)O3 Nanofibers Produced by Electrospinning Process

2008 ◽  
Vol 1129 ◽  
Author(s):  
Ebru Mensur Alkoy ◽  
Canan Dagdeviren ◽  
Melih Papila
Keyword(s):  
Lead Zirconate Titanate ◽  
Perovskite Phase ◽  
Sol Gel ◽  
Precursor Solution ◽  
Lead Zirconate ◽  
Electrospinning Process ◽  
X Ray Diffraction ◽  
Fiber Mats ◽  
Xrd Pattern ◽  
X Ray

AbstractLead zirconate titanate (PZT) nanofibers are obtained by electrospinning a sol-gel based solution and polyvinyl pyrrolidone (PVP) polymer, and subsequent sintering of the electrospun precursor fibers. The PVP content of the precursor solution is critical in the formation of the fully fibrous mats. Scanning electron microscope (SEM) is used to examine the morphology of the precursor fibers and annealed PZT nanofibers. The diameters of the precursor PZT/PVP green fibers have increased with the aging of the precursor solution along with an increase in the viscosity. The viscosity of 500 mPa results in successful fibrous mats, yielding green PZT/PVP fibers with a diameter of 400 nm. The fiber mats are then sintered at 700°C. X-ray diffraction (XRD) pattern of the annealed PZT fibers exhibits no preferred orientation and a pure tetragonal perovskite phase. Preparation of piezocomposites by infusion of epoxy into the nanofiber mat facilitates successful handling of the fragile mats and enables measurements of dielectric properties.

Sol-Gel Derived PZT Thick Films with Nano-Sized Microstructure

2002 ◽  
Vol 748 ◽  
Author(s):  
C. L. Zhao ◽  
Z. H. Wang ◽  
W. Zhu ◽  
O. K. Tan ◽  
H. H. Hng
Keyword(s):  
Lead Zirconate Titanate ◽  
Electromechanical Coupling ◽  
Thick Films ◽  
Sol Gel ◽  
Essential Element ◽  
Processing Parameters ◽  
Lead Zirconate ◽  
Piezoelectric Response ◽  
Coupling Coefficients ◽  
Pzt Films

ABSTRACTLead zirconate titanate (PZT) films are promising for acoustic micro-devices applications because of their extremely high electromechanical coupling coefficients and excellent piezoelectric response. Thicker PZT films are crucial for these acoustic applications. A hybrid sol-gel technology has been developed as a new approach to realize simple and cost-effective fabrication of high quality PZT thick films. In this paper, PZT53/47 thick films with a thickness of 5–50 μm are successfully deposited on Pt-coated silicon wafer by using the hybrid sol-gel technology. The obtained PZT thick films are dense, crack-free, and have a nano-sized microstructure. The processing parameters of this technology have been evaluated. The microstructure of the film has been observed using field-emission scanning electron microscopy and the crystallization process has been monitored by the X-ray diffraction. The thick films thus made are good candidates for fabrication of piezoelectric diaphragm which will be an essential element of microspeaker and microphone arrays.

Early Stages of Crystallization of Sol−Gel-Derived Lead Zirconate Titanate Thin Films

2003 ◽  
Vol 15 (5) ◽  
pp. 1147-1155 ◽  
Author(s):  
A. Wu ◽  
P. M. Vilarinho ◽  
I. Reaney ◽  
I. M. Miranda Salvado
Keyword(s):  
Thin Films ◽  
Lead Zirconate Titanate ◽  
Sol Gel ◽  
Lead Zirconate ◽  
Early Stages ◽  
Zirconate Titanate
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