KOH-Based Hydrothermal Synthesis of Iron-Rich Titanate Nanosheets Assembled into 3D Hierarchical Architectures from Natural Ilmenite Mineral Sands

The synthesis of titanate nanostructures from low-cost mineral precursors is a topic of continuous interest, considering not only their fundamental aspects but also the benefits of incorporating such nanomaterials in a wide variety of applications. In this work, iron-rich titanate nanosheets were synthesized from Ecuadorian ilmenite sands (ilmenite–hematite solid solution-IHSS) through an alkaline hydrothermal treatment (AHT) using potassium hydroxide (KOH). The effect of the duration of the KOH-AHT was assessed at 180 °C for 24, 48, 72, and 96 h. The morphology evolution over time and the plausible formation mechanisms of titanate nanostructures were discussed. The most significant morphological transformation was observed after 72 h. At this time interval, the titanate nanostructures were assembled into well-defined 3D hierarchical architectures such as book-block-like arrangements with open channels. Based on X-ray powder diffraction (XRPD), transmission electron microscopy (TEM), selected area electron diffraction (SAED), and scanning electron microscopy coupled with energy-dispersive X-ray spectroscopy (SEM-EDS) analyses, it was determined that these nanostructures correspond to iron-rich layered titanates (Fe/Ti mass ratio of 7.1). Moreover, it was evidenced that the conversion of the precursor into layered nanostructures was not complete, since for all the tested reaction times the presence of remaining IHSS was identified. Our experiments demonstrated that the Ecuadorian ilmenite sands are relatively stable in KOH medium.