Cerium Oxalate Morphotypes: Synthesis and Conversion into Nanocrystalline Oxide

Inorg Chem. 2019 Aug 5;58(15):10111-10118. doi: 10.1021/acs.inorgchem.9b01250. Epub 2019 Jul 26.

Abstract

Cerium dioxide is a scientifically and technologically important material with a wide range of potential applications, particularly in solid oxide fuel cells and catalysis. Herein, we report a study focusing on the synthesis of nanocrystalline cerium dioxide via thermal decomposition of the oxalate salt. Simply by changing reaction conditions (temperature, concentration, acidity, strike) during the precipitation of the cerium solution with oxalic acid, we were able to obtain different morphologies. The main reaction parameters were mapped and linked to the morphology of the final products. Additionally, it was proved that oxalate precipitation is a robust reaction proceeding at relatively extreme contitions. Moreover, the conversion of cerium oxalate to nanocrystalline oxide was followed to monitor the progress of the reaction, the texture evolution, and the grain growth. The results showed that, for unvaried heating cycle, the grain size of converted material is linked to morphology. The thinner was the original microcrystal the smaller were the CeO2 nanocrystals after calcination. In addition, the grains were found smaller near the edges of the ex-oxalate microcrystals. In both cases, this behavior results from asymmetrical limitations of diffusion during grain growth.