Size-controlled synthesis of metal oxide nanoparticles with a flow-through supercritical water method

Hydrothermal synthesis of metal oxide (AlOOH/Al₂O₃, CuO, Fe₂O₃, NiO, ZrO₂) nanoparticles from metal nitrate aqueous solution was carried out at 673 K and pressures ranging from 25 MPa to 37.5 MPa with a flow-through supercritical water method. Size, phase and crystallinity of the obtained particles were characterized by TEM, XRD and TG, respectively. Effect of the difference of the metals in starting materials, pressures and concentrations on particle size and crystallinity was analyzed on the basis of supersaturation, which was evaluated by estimated metal oxide solubility. The result suggests that supersaturation should be set to higher than around 10⁴ in this method to obtain particles under 10 nm in diameter. Further, crystallinity of the obtained particles was evaluated as weight loss through TG analysis. It was found that higher supersaturation decreased the crystallinity. This result can be explained that high supersaturation led to the inclusion of water molecules during the formation of particles.