A novel synthesis of FeNbO4 nanorod by hydrothermal process

Abstract

This study reports a facile, gram-scale synthesis of FeNbO4 nanorods via hydrothermal route, using iron nitrate [Fe(NO3)3] and niobium tartarate (Nb tartarate) in presence of potassium peroxosulfate. The formation of single phase, polycrystalline orthorhombic structure of FeNbO4 was confirmed by the careful analysis of the X-ray diffraction (XRD) pattern. The average crystallite size, calculated using a few XRD peaks, was found to be 12.8 nm. As indicated by transmission electron microscopy (TEM) and field emission scanning electron microscopy, the average length and diameter of the rods were found to be only 25 × 7 nm and 47 × 14 nm, respectively. The selected area electron diffraction and high-resolution transmission electron microscopy (HRTEM) data of the single rod implied that FeNbO4 nanorods were polycrystalline in nature and grew up along the c-axis. HRTEM also revealed that the fringes are equidistant with a lattice separation of 0.91 Ǻ, which corresponded to the (111) plane of the FeNbO4 crystal. Elemental composition of the nanorods was confirmed using electron dispersive X-ray spectroscopy analysis while binding state of the surface was intervened through X-ray photoelectron spectroscopy. Mechanistic investigations suggested that potassium peroxosulfate played a crucial role in the unidirectional growth of particles. The synthetic method is simple, amenable to scale up and contributes a new tool box for the development of FeNbO4-based one-dimensional (1D) structures that appears to be more promising for a myriad of applications, compared to their 3D counterparts.