The radiolysis of bulk water results in the formation of hydrogen (H2) generating interest in production for clean energy applications and chemical feedstock. Various metal oxides have been shown to impact H2 formation rate through the oxide-water interface, raising safety concerns for the nuclear energy industry through pressurization, flammable mixtures, and hydrogen cracking. To understand this interfacial radiolysis at a fundamental level, various metal oxides will be used to determine which material parameters impact H2 yields. This report focuses on the development of a controllable synthesis method for spherical yttrium oxide (Y2O3) particles that will be applied to other metal oxides. A hydrothermal hydrolysis reaction using yttrium nitrate (Y(NO3)3) was employed to produce yttrium hydroxide (Y(OH)3) particles that were calcined at 800°C to form the final Y2O3 particles. Through synthesis variations, it was found that a 2-hour, 90°C synthesis with a rapid cooling time was optimal for obtaining spherical particles of 2 consistent morphology. Diffuse reflectance Fourier transform infrared spectroscopy (DRIFTS) studies revealed the prevalence of carbonate on all Y2O3 samples including a high purity commercial product. DRIFTS also highlighted the role of calcination in removing synthesis impurities and facilitating the crystalline transition from hydroxide to oxide. Synthesized, as well as commercially available Y2O3 were exposed to humid air to saturate the surface with water vapor, and flame sealed in an inert atmosphere. Prepared samples were irradiated using a Foss Therapy Model 812 cobalt-60 gamma irradiator to measure the H2 yield from surface water radiolysis. Future work will focus on removing carbonate from the oxide surface to investigate its impact on H2 generation.
