Black solid precursors obtained from reactions between MCl 5 (M = Nb, Ta) and alkyllithiums, n-butyllithium ( n BuLi) 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 (LiNbO 3 ) and lithium tantalate (LiTaO 3 ). 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 LiNbO 3 and LiTaO 3 precursors.

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