Tetrahydrofuran Activation Assisted Synthesis of Nanosized Lithium Niobate and Lithium Tantalate

Black solid precursors obtained from reactions between MCl₅ (M = Nb, Ta) and alkyllithiums, n‐butyllithium (ⁿBuLi) and ethyllithium (EtLi), in tetrahydrofuran (THF) were heat treated under vacuum at 673–973 K to form nano‐sized particles (20–100 nm in diameter) of lithium niobate (LiNbO₃) and lithium tantalate (LiTaO₃). Stoichiometry of the reactants is critical and affects the phases of the products. Based on the volatile byproducts detected, a reaction pathway involving the activation of THF by alkyllithiums is proposed to be important for the formation of LiNbO₃ and LiTaO₃ precursors.