Abstract
The impacts of co-precipitation reaction temperature and duration, as well as calcination temperature and duration, on the particle morphology and properties of gadolinia (Gd2O3) nanopowders were investigated. Thermogravimetric curve of thermally treated gadolinium oxalate (Gd2(C2O4)3) showed that pure stable cubic phase Gd2O3 nanopowders could be obtained by calcining at 640 °C and higher. This finding was also supported by results obtained from Fourier Transform Infrared Spectrometry (FTIR) and Raman spectrometry. This study also shows that uniform spherules of Gd2O3 nanopowders could be obtained under controlled synthesis conditions. However, with an increase in both the co-precipitation reaction temperature and duration, the extent of agglomeration of Gd2O3 nanopowders increased, as observed under a Field Emission Scanning Electron Microscope (FESEM). The FESEM images and X-ray Diffraction (XRD) patterns also revealed accelerated grain growth and increased average crystallite size at high calcination temperatures and holding times. It was determined that the most favourable Gd2O3 particle morphology was achieved when Gd2(C2O4)3 was co-precipitated at 40 °C, then thermally degraded at 650 °C, for 1 h and 4 h, respectively. Estimated Scherrer's average crystallite size of the resulting Gd2O3 nanopowders was 16.54 nm, which was further affirmed with the transmission electron microscope (TEM) image, where crystallite sizes of 3–27.5 nm were observed in the Gd2O3 sample. This specimen also demonstrated a considerably large specific surface area of 9.16 m2/g, as measured using a Brunauer–Emmett–Teller (BET) analyser.