Abstract: | BiB3O6 (BIBO) single crystals with sizes of 44 mm × 24 mm × 10 mm and weight of 24.7 g have been successfully grown by the top-seeded method. In this note, the preparation of seed, the growth of crystal and some problems encountered are reported. The lattice parameters of BIBO are a =7.1203(7)Å, b = 4.9948(7)Å, c = 6.5077(7)Å, β = 105.586(8)″, V=222.93(5)Å3, which were determined by BRUKER-P4 four-circle diffractometer. BIBO is biaxial crystal and the relative orientation of (X, Y, Z) with regard to (a, b, c) is: X // b, (Y, c) =47.2°, (Z, a) = 31.6°, determined by the X-ray analysis combined with polarized microscopy. The second-harmonic-generation (SHG) conversion efficiency of the sample for 1.064 mm light is up to 67.7%. We have also obtained the third harmonic generation (THG) of 1.064 mm, namely, 1.064 mm + 0.532 mm →0.355 mm. BIBO crystal is free of moisture and hygroscopy |