Chloride flux growth of crystalline strontium niobates and nitridation to perovskite SrNbO2N

Highly crystalline (110) layered perovskite Sr2Nb2O7, (111) layered perovskite Sr5Nb4O15 and complex perovskite Sr4Nb2O9 were prepared by NaCl-KCl flux growth method from SrCO3 and Nb2O5. This flux synthesis achieves single strontium niobate phase in contrast to mixed niobates from the solid state reaction with the same heating parameters. A little excess of Sr source was found to be required for the synthesis of Sr5Nb4O15 and Sr4Nb2O9 at elevated temperature due to slight evaporation. The three strontium niobates were converted to perovskite SrNbO2N via thermal ammonolysis under NH3 flow at 900 °C. Post-wash treatment was performed to remove the byproduct SrO. This makes additional nanopores in SrNbO2N in the cases of Sr5Nb4O15 and Sr4Nb2O9, and results in increasing surface areas of SrNbO2N with Sr:Nb ratios in the precursors (from 9.9 to 19.8 and 35.5 m2/g). On the other hand, the UV-Vis diffusion reflectance spectra reveal decreasing light absorption by defects in SrNbO2N in this order. This suggests fewer low-valent Nb defects in SrNbO2N prepared from precursor with higher Sr:Nb ratio. SrNbO2N prepared from Sr4Nb2O9 would be advantageous for applications that require high surface area and low defect density of the material.