doi:10.1016/j.jeurceramsoc.2004.09.004
Copyright © 2004 Elsevier Ltd All rights reserved.
Phase assembly and microstructure of CeO2-doped ZrO2 ceramics prepared by spark plasma sintering
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Tao Xua, Peiling Wanga,
,
, Pingan Fanga, Yanmei Kana, Lidong Chena, Jef Vleugelsb, Omer Van der Biestb and Jef Van Landuytc
aState Key Lab of High Performance Ceramics and Superfine Microstructure, Shanghai Institute of Ceramics, Chinese Academy of Sciences, 200050 Shanghai, China
bDepartment of Metallurgy and Materials Engineering, Katholieke Universiteit Leuven, B-3001 Leuven, Belgium
cEMAT, Universiteit Antwerpen, B-2020 Antwerpen, Belgium
Received 21 April 2004;
revised 23 August 2004;
accepted 27 August 2004.
Available online 17 November 2004.
Abstract
CeO2-doped ZrO2 (8 mol%) starting powder was sintered by means of spark plasma sintering (SPS) at 1300 °C without holding time. The stability of the tetragonal ZrO2 phase in the Ce-ZrO2 ceramic sintered under strongly reducing conditions was investigated. The SPS sample consisted of monoclinic and tetragonal ZrO2 phases with a volume ratio of two to one, as well as a trace amount of a Zr–Ce–O cubic solid solution phase. In contrast, the same powder sintered by hot-pressing in nitrogen at 1300 and 1500 °C for 1 h showed no tetragonal ZrO2. Microstructural observation of the SPS ceramic by SEM and TEM revealed grains with and without twins. The reason for the appearance of the tetragonal phase in the SPS sample sintered under strongly reducing conditions is discussed.
Keywords: Ce-TZP; Spark plasma sintering; Hot-pressing; Phase stability; Microstructure; ZrO2
Fig. 1. XRD patterns of the ceramics sintered under different conditions: (a) hot-pressed at 1300 °C, (b) hot-pressed at 1500 °C, and (c) SPS-ed at 1300 °C. The Si was added as internal marker.
Fig. 2. Phase diagram of the ZrO2–CeO1.5 system.17
Fig. 3. SEM micrograph of the 8 mol% CeO2 stabilized ZrO2 ceramic sintered by SPS.
Fig. 4. TEM micrograph of the 8 mol% CeO2 stabilized ZrO2 ceramic sintered by SPS.
Fig. 5. Detail of a monoclinic grain of the 8 mol% CeO2 stabilized ZrO2 ceramic sintered by SPS.
Fig. 6. TEM micrographs and EDS spectra taken from different grains in the 8 mol% CeO2 stabilized ceramic sintered by SPS. The analysis results of the labelled positions are summarized in Table 2.
Table 1.
Sintering conditions, densities and phase assembly of the sintered samples

aCss: Zr–Ce–O cubic solid solution; t: tetragonal; s: strong; m: medium; w: weak; tr: trace.
Table 2.
EDS results of different point analysis at the locations indicated in Fig. 6

aZr ions are assumed to retain their tetravalent state.

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