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

Abstract

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 themore » cubic phase, at temperatures ranging from {approximately}400{degree}C to greater than 700{degree}C, depending on the heating rate.« less

Authors:
; ; ;
Publication Date:
Research Org.:
Sandia National Labs., Albuquerque, NM (United States)
Sponsoring Org.:
USDOE, Washington, DC (United States)
OSTI Identifier:
10116785
Report Number(s):
SAND-93-0975C; CONF-931142-5
ON: DE94005573; BR: GB0103012
DOE Contract Number:  
AC04-94AL85000
Resource Type:
Conference
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
Subject:
36 MATERIALS SCIENCE; ZIRCONIUM OXIDES; DENSITY; CRYSTALLIZATION; SOL-GEL PROCESS; THIN FILMS; 360202; STRUCTURE AND PHASE STUDIES

Citation Formats

Schwartz, R W, Voigt, J A, Buchheit, C D, and Boyle, T J. Densification and crystallization of zirconia thin films prepared by sol-gel processing. United States: N. p., 1993. Web.
Schwartz, R W, Voigt, J A, Buchheit, C D, & Boyle, T J. Densification and crystallization of zirconia thin films prepared by sol-gel processing. United States.
Schwartz, R W, Voigt, J A, Buchheit, C D, and Boyle, T J. 1993. "Densification and crystallization of zirconia thin films prepared by sol-gel processing". United States. https://www.osti.gov/servlets/purl/10116785.
@article{osti_10116785,
title = {Densification and crystallization of zirconia thin films prepared by sol-gel processing},
author = {Schwartz, R W and Voigt, J A and Buchheit, C D and Boyle, T J},
abstractNote = {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.},
doi = {},
url = {https://www.osti.gov/biblio/10116785}, journal = {},
number = ,
volume = ,
place = {United States},
year = {Fri Dec 31 00:00:00 EST 1993},
month = {Fri Dec 31 00:00:00 EST 1993}
}

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