Some structural aspects of neodymium praseodymium oxalate single crystals grown in hydro silica gels

Abstract

The mixed crystals of neodymium praseodymium oxalate are grown by the diffusion of a mixture of aqueous solutions of neodymium nitrate and praseodymium nitrate (as an upper reactant) into the set gel embedded with oxalic acid. By varying the concentration (by volume) of rare earth nitrates in the upper reactant, the incorporation of Nd and Pr in the mixed crystals has been studied. Tabular crystals with the well defined hexagonal basal planes are observed in the mixed crystals of varying concentrations. X-ray diffraction patterns of these powdered samples reveal that these mixed crystals are 'isostructural', while IR and FTIR spectra establish the presence of oxalate groups. TGA and DSC analyses show the correctness of the chemical formula for the mixed crystals, by the release of water molecules (endothermic) and of CO and CO2 (exothermic), with the rare earth oxides as the stable residue. X-ray fluorescence (XRF) and energy dispersive X-ray analyses (EDAX) establish the presence of heavy rare earth elements qualitatively and to a good extent quantitatively. X-ray photoelectron spectroscopic (XPS) studies confirm the presence of rare earth elements (Nd and Pr) as their respective oxides. The findings of these techniques of characterization are in excellent agreement with the proposed empirical structure for the mixed rare earth oxalates. The implications are discussed.