Abstract: | A new beryllium‐free deep‐ultraviolet (DUV) nonlinear optical (NLO) material, β‐Rb2Al2B2O7 (β‐RABO), has been synthesized and characterized. The chiral nonpolar acentric material shows second‐harmonic generation (SHG) activity at both 1064 and 532 nm with efficiencies of 2×KH2PO4 and 0.4×β‐BaB2O4, respectively, and exhibits a short absorption edge below 200 nm. β‐Rb2Al2B2O7 has a three‐dimensional structure of corner‐shared Al(BO3)3O polyhedra. The discovery of β‐RABO shows that through careful synthesis and characterization, replacement of KBe2BO3F2 (KBBF) by a Be‐free DUV NLO material is possible. |