A new series of Dion-Jacobson layered perovskite compounds A’LnNaNb3O10 (A’ = Cs, Rb, H; Ln = Nd, Pr) was synthesized for the first time. Phase and chemical purity of compounds were proved using XRD, SEM, and EDX. Compounds RbNdNaNb3O10, RbPrNaNb3O10, CsNdNaNb3O10 and CsPrNaNb3O10 were synthesized using solid-state reaction, whereas HNdNaNb3O10, HPrNaNb3O10 were obtained by ion-exchange reaction. Crystal structures of solid-state reaction products were refined using the Rietveld method. The plausibility of obtained crystal structures was studied using the bond valence sum (BVS) method. The thermal behavior of compounds was established using DTA. Ion-exchange products were found to be metastable hydrates. The presence of the crystallization water was confirmed by DTA and IR spectroscopy. Optical band gap, electronegativity, valence band (EVB), and conduction band (ECB) potentials of obtained compounds were calculated from diffuse reflectance spectroscopy data. A previously proposed correlation between band gap and structural distortions was confirmed.
