Modelling of relation between synthesis parameters and average crystallitesize of Yb2O3 nanoparticles using Box-Behnken design

Abstract

A straightforward wet chemical method has been applied for the fabrication of Yb2O3nanoparticles (NPs) fromytterbium nitrate solution by using ammonium carbonate as precipitation agent. Effects of precursor molarity(0.1, 0.15 and 0.2 M), calcination temperature (800, 900 and 1000 °C) and time (2, 4 and 6 h) on averagecrystallite size (CS) of the NPs were statistically investigated by using Box-Behnken design. A simple and ef-fective quadratic model was proposed for controlling the CS. The CS values were calculated by using WilliamsonHall method (W-H) from X-Ray Diffraction (XRD) broadening data and found to be ranging between 13 and26 nm. Agglomerated NPs morphologies and particle sizes were revealed by Field Emission Gun-ScanningElectron Microscopy (FEG-SEM). Fourier Transform Infrared (FTIR) spectrophotometry confirmed that as-re-ceived Yb2(CO3)3xH2O powders were successfully transformed into Yb2O3NPs with calcination. High-ResolutionTransmission Electron Microscopy (HRTEM) results verified the average CS values. ANOVA analyses revealedthat linear and squared terms of the production parameters were significantly related to the CS whereas in-teraction terms were insignificant with the confidence level of 95% (R2= 92.67%, R2-adj = 87.17%). Thecalcination temperature had the highest impact on the average CS followed by the time and precursor molarity.Increasing calcination parameters resulted in bigger crystallites whereas increasing precursor molarity exhibiteda critical supersaturation value (0.15 M) from which the average CS was decreased