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Title: Densification and crystallization of zirconia thin films prepared by sol-gel processing

Conference ·
OSTI ID:28832
; ; ;  [1]
  1. Sandia National Labs., Albuquerque, NM (United States)

We have investigated the effects of precursor nature and heat-treatment schedule on the densification and crystallization behavior of sol-gel derived zirconia thin films. Precursor solutions were prepared from n-propanol, zirconium (IV) n-propoxide, and either acetic acid, or 2,4-pentanedione (acac) and water additions. By controlling the ligand type and ligand-to-metal ratio, we were able to prepare films which displayed significant differences in densification behavior. We attribute the dissimilarity in densification to variations in the nature of the as-deposited films, as influenced by ligand type and concentration. While the acac-derived film was a physical gel, (i.e., a physical aggregation of the oligomeric species), the acetic acid-derived film, which exhibited less consolidation, was a chemical gel that could not be redissolved in the parent solvent. Films prepared with large acac/metal ratios and small water additions exhibited minimal crosslinking at 25{degrees}C, displayed the greatest consolidation ({approximately} 86% shrinkage) and the highest refractive index (n = 2.071) when heat-treated. These results indicate the importance that M-O-M bonds (crosslinks) formed at low temperature can have on densification behavior. We also report on the effects of heat-treatment schedules and ramp rates on densification behavior. All of the films of the present study crystallized into the cubic phase, at temperatures ranging from {approximately} 400{degrees}C to greater than 700{degrees}C, depending on the heating rate.

Research Organization:
Sandia National Laboratories (SNL), Albuquerque, NM, and Livermore, CA (United States)
DOE Contract Number:
AC04-94AL85000
OSTI ID:
28832
Report Number(s):
CONF-931142-; TRN: 94:010156-0015
Resource Relation:
Conference: 1. meeting of the Pacific Rim ceramic societies, Honolulu, HI (United States), 7-10 Nov 1993; Other Information: PBD: 1994; Related Information: Is Part Of Ceramic transactions: Ferroic materials - design, preparation, and characteristics. Volume 43; Bhalla, A.S.; Nair, K.M.; Lloyd, I.K.; Yanagida, H.; Payne, D.A. [eds.]; PB: 438 p.
Country of Publication:
United States
Language:
English