Iron-Based Spiky Microspheres Synthesized Using Oxalate via One-Step Hydrothermal Process — Presence of Humboldtine

Abstract

In this study, novel iron-based spiky microparticles (approximately 1–2[Formula: see text][Formula: see text]m in diameter) were synthesized using iron oxalate precursors using a straightforward one-step hydrothermal reaction. The microparticles’ morphological, mineralogical and chemical properties were investigated using scanning electron microscopy (SEM), X-ray diffractometry (XRD), Raman spectroscopy and UV-Vis spectroscopy. The physico-chemical characteristics of spiky microparticles were also compared with cubic iron microparticles synthesized using standalone iron as well as with the addition of glycine. XRD and Raman analyses identified substantial presence of humboldtine, a type of ferrous oxalate dehydrate mineral, in the resultant yellowish solid hydrothermal product. The mechanism involving reactions of species in the hydrothermal process was described herein. The results described in this study afford vital insights into the design of iron oxalate-based microparticles synthesis processes.