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Rij, Leen Van
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article
Analysis of the preparation of In-doped CaZrO3 using a peroxo-oxalate complexation method
Abstract
The wet chemical synthesis of CaZr<sub>0.9</sub>In<sub>0.1</sub>O<sub>3-α</sub> powders via a peroxo-oxalate complexation method has been studied in detail using different techniques, <i>i.e.</i> TG-DTA, XRD, FT-IR, BET, SEM, EDX, and non-isothermal densification. Using these techniques, the different reaction steps in the calcination process have been clarified. After drying the precipitated complex at 150 °C for 3 h, a mixture of calcium oxalate and an amorphous zirconia phase is found. Between 200 and 450 °C, the calcium oxalate decomposes into calcium carbonate. In the temperature range 450±800 °C, the calcium carbonate decomposes into CaO, while a crystalline zirconia phase appears (CaZr<sub>4</sub>O<sub>9</sub>). In this temperature range, the formation of CaZrO<sub>3</sub> is already observed. Further increasing the calcination temperature to 1000 °C leads to a binary mixture of CaZrO<sub>3</sub> and CaIn<sub>2</sub>O<sub>4</sub>. When the calcination temperature is increased to around 1500 °C, the CaIn<sub>2</sub>O<sub>4</sub> phase dissolves into the calcium zirconate to form the desired CaZr<sub>0.9</sub>In<sub>0.1</sub>O<sub>3-α</sub>. All compacts sintered at 1550 °C for 10 h show single-phase CaZr<sub>0.9</sub>In<sub>0.1</sub>O<sub>3-α</sub>, independent of the calcination temperature. The morphology of the sintered compacts, however, varies with the calcination temperature, due to the presence or absence of a reactive sintering step around 1300 °C. Powders calcined at 1000 °C show a larger grain size in the sintered compact than powders calcined at 1450 or 1550 °C.