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

Author:

Lagos Karina J.12,Marinkovic Bojan A.3ORCID,Dosen Anja4ORCID,Debut Alexis5ORCID,Vizuete Karla5ORCID,Guerrero Victor H.2ORCID,Pardo Emilio1ORCID,Pontón Patricia I.2ORCID

Affiliation:

1. Molecular Science Institute, Coordination Chemistry Group, University of Valencia, 46980 Paterna, Spain

2. Department of Materials, Escuela Politécnica Nacional (EPN), Quito 170525, Ecuador

3. Department of Chemical and Materials Engineering, Pontifical Catholic University of Rio de Janeiro (PUC-Rio), Rio de Janeiro 22453-900, Brazil

4. International Centre for Diffraction Data (ICDD), Newtown Square, PA 19073, USA

5. Centro de Nanociencia y Nanotecnología, Universidad de las Fuerzas Armadas (ESPE), Sangolquí 171103, Ecuador

Abstract

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.

Publisher

MDPI AG

Subject

Geology,Geotechnical Engineering and Engineering Geology

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