Journal
ACTA MATERIALIA
Volume 55, Issue 8, Pages 2907-2917Publisher
PERGAMON-ELSEVIER SCIENCE LTD
DOI: 10.1016/j.actamat.2006.12.039
Keywords
EFTEM; HRTEM; grain boundary segregation; sintering; ceramics
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The microstructure and chemistry of 2 mol.% and 5 mol.% cobalt-oxide-doped Ce0.8Gd0.2O1.9 sintered at different temperatures were examined by a combination of electron energy-loss spectroscopy and energy-filtering and high-resolution transmission electron microscopy. Co grain boundary excess was evaluated. It is found that Co solubility in Ce0.8Gd0.2O1.9 is low at temperatures between 800 and 1150 OC, resulting in a large number of Co precipitates at grain boundaries. With increasing sintering temperature, precipitates grow, influencing the Co redistribution and further altering the segregation amount in the grain boundary. The Co grain boundary concentration is shown to increase with the increase of sintering temperature from 890 to 1050 degrees C, which is suggested to be due to grain growth. It is found that Co grain boundary segregation induces a detectable variation in the ELNES of Ce-M-4,M-5 and O-K absorption edges, indicating a reduction of Ce atoms in the grain boundary region. The phase of the precipitates was identified as COO at temperatures between 890 degrees C and 1150 degrees C. HRTEM reveals that grain boundaries are less disordered after prolonged sintering time at higher temperature. At a dopant level of 5 mol.% Co oxide in Ce0.8Gd0.2O1.9, the grain boundaries become more disordered, and exhibit a high amount of Co segregation. (C) 2007 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.
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