The intercalation reaction of 1,10-phenanthroline with layered compound FePS3

The intercalation reaction of 1,10-phenanthroline with FePS3 in ethanol and in the presence of anilinium chloride has been monitored in detail with th e X-ray powder diffraction (XRD) method to study the reaction mechanism. It is revealed that during the intercalation period there are three phases: t he 001 phase (corresponding to the perpendicular orientation of the 1,10-ph enanthroline ring with the layer of the host FePS3), the 001' phase (standi ng for the parallel orientation of the 1,10-phenanthroline ring with the la yer), and the 001" phase (pristine FePS3), but as the period of the reactio n is prolonged, the 001' and 001" phases diminish gradually and finally dis appear, and the 001 phase is intensified and a complete intercalate is obta ined for Series A, in which excess 1,10-phenanthroline is used. However, fo r Series B in which the optimum amount of 1,10-phenanthroline is used, the 001 and 001" phases diminish gradually, and another intercalate is obtained that exhibits the 001' phase. Moreover, if the amount of phenanthroline us ed in the reaction is more than that in Series B but not in excess, another intercalate containing 001 and 001' phases is obtained. In these intercala tion reactions, the results of IR spectroscopy indicate that anilinium chlo ride serves only as the source of protons for 1,10-phenanthroline, but 1,10 -phenanthroline acts as both the complexing agent of Fe2+ ions removed from FePS3, confirmed by UV spectra of the filtrates, and the inserted guest, s ome of which exists in the form of protonated cation to maintain the charge balance of the intercalates. From the experimental evidence we find that t he arranged orientation of 1,10-phenanthroline between the layers is contro lled by the amount of guest used in the reaction, and a possible intercalat ion mechanism is proposed for the reaction. (C) 2000 Academic Press.