Field-Assisted Sintering/Spark Plasma Sintering of Gadolinium-Doped Ceria with Controlled Re-Oxidation for Crack Prevention

Gadolinium-Doped Ceria (GDC) is a prospective material for application in electrochemical devices. Free sintering in air of GDC powder usually requires temperatures in the range of 1400 to 1600 degrees C and dwell time of several hours. Recently, it was demonstrated that sintering temperature can be significantly decreased, when sintering was performed in reducing atmosphere. Following re-oxidation at elevated temperatures was found to be a helpful measure to avoid sample failure. Sintering temperature and dwell time can be also decreased by use of Spark Plasma Sintering, also known as Field-Assisted Sintering Technique (FAST/SPS). In the present work, we combined for the first time the advantages of FAST/SPS technology and re-oxidation for sintering of GDC parts. However, GDC samples sintered by FAST/SPS were highly sensitive to fragmentation. Therefore, we investigated the factors responsible for this effect. Based on understanding of these factors, a special tool was designed enabling pressureless FAST/SPS sintering in controlled atmosphere. For proof of concept, a commercial GDC powder was sintered in this tool in reducing atmosphere (Ar-2.9%H-2), followed by re-oxidation. The fragmentation of GDC samples was avoided and the number of micro-cracks was reduced to a minimum. Prospects of GDC sintering by FAST/SPS were discussed.