Bi2O2Se single crystals were prepared via a modified Bridgman method. The stoichiometric high-purity Bi2O3 powder (99.999%), Se powder (99.999%), and Bi powder (99.999%) were weighted into evacuated quartz tube with pressure down to 10−2 Pa. The Bi2O2Se powder was obtained when the temperature was kept at 773 K for 6 hours. As-synthesized Bi2O2Se was grounded into powder, reencapsulated into an evacuated quartz tube, molten at 1223 K for 2 hours, then slowly cooled down to 1123 K for 24 hours, and finally cooled down to room temperature to form a bulk crystal, which is confirmed as tetragonal Bi2O2Se with the space group of I4/mmm (a = b = 3.88 Å, c = 12.16 Å, Z = 2) by XRD.

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