Aging characteristics of a hybrid sol-gel Pb(Zr, Ti)O 3 precursor solution
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Aging characteristics of a hybrid sol-gel Pb(Zr, Ti)O3 precursor solution Timothy J. Boylea) Advanced Materials Laboratory, Sandia National Laboratories, 1001 University Boulevard, SE, Albuquerque, New Mexico 87106
Duane Dimos Sandia National Laboratories, 1515 Eubank NE, Mail Stop 1405, Albuquerque, New Mexico 87715
Robert W. Schwartz Advanced Materials Laboratory, Sandia National Laboratories, 1001 University Boulevard, SE, Albuquerque, New Mexico 87106
Todd M. Alam and Michael B. Sinclair Sandia National Laboratories, 1515 Eubank NE, Mail Stop 1405, Albuquerque, New Mexico 87115
Catherine D. Buchheit Advanced Materials Laboratory, Sandia National Laboratories, 1001 University Boulevard, SE, Albuquerque, New Mexico 87106 (Received 30 August 1996; accepted 9 December 1996)
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 1 H 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.
I. INTRODUCTION
There are a wide variety of chemical solution deposition methodologies (i.e., sol-gel, metallo-organic deposition, or hybrids) that have been reported for the fabrication of lead zirconate titanate (PZT) thin films.1–8 Generally, these precursor solutions incorporate commercially available materials in the form of metal carboxylates and/or metal alkoxides. Typically, solution processes modify these starting materials either by (i) dissolving them in a solvent (i.e., neodecanoate carboxylic acids3,6 or 2-methoxyethanol2 ) at reflux temperatures (ultimately generating solventligand exchanged species), (ii) combining various metal carboxylates/acetylacetonates without heating (i.e., Haertling process),4 or (iii) mixing metal alkoxides and carboxylates with heating, such as the Sequential a)
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J. Mater. Res., Vol. 12, No. 4, Apr 1997
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Precursor Addition (SPA)1 or the Inverted Mixing Order (IMO) process.5,7 The IMO process, which is a hybrid approach, has been shown to
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