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Growth of Er3+‐doped 100‐nm thick LiNbO3(LN) films on Z‐cut LiTaO3(LT) single‐crystal by e‐beam evaporation and in‐situ anneal at 600–800°C was studied. Crystalline phase, crystallographic orientation, Er3+ spectroscopic properties, constituent element valence states, defects, Er3+ concentration and stoichiometry of the films were characterized. The results show that the films are in LN single‐crystal state and orient along with c crystallographic axis. Constituent elements Li, O and Er are present in their respective single valence states Li+, O2−, Er3+, while the Nb is in two valence states Nb5+ and Nb4+. The films have Li2O‐contents around congruent point. Antisite(NbLi4+) is the major defect. Its concentration decreases, while Li2O‐content, crystallinity degree, and fluorescence intensity increase with increased growth temperature. The presence of Er3+ in the grown films is in the form of LN crystalline phase. Its concentration is considerably lower than that in initial target material because of lower e‐beam evaporation efficiency of heavy Er3+. [ABSTRACT FROM AUTHOR]