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

Conference ·
OSTI ID:10116785

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{degree}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{degree}C to greater than 700{degree}C, depending on the heating rate.

Research Organization:
Sandia National Labs., Albuquerque, NM (United States)
Sponsoring Organization:
USDOE, Washington, DC (United States)
DOE Contract Number:
AC04-94AL85000
OSTI ID:
10116785
Report Number(s):
SAND-93-0975C; CONF-931142-5; ON: DE94005573; BR: GB0103012
Resource Relation:
Conference: 1. meeting of the Pacific Rim ceramic societies,Honolulu, HI (United States),7-10 Nov 1993; Other Information: PBD: [1993]
Country of Publication:
United States
Language:
English