Аннотация:Double borate Rb3Tm2B3O9 was newly synthesized by solid-state reaction. The crystal structure of Rb3Tm2B3O9 was refined by Rietveld's method: Pna21, a = 8.6648(1), b = 9.5238(1), c = 12.1722(1) Å, Z = 4. The crystal structure of Rb3Tm2B3O9 consists of -[Tm2O9]∞- chains along the “a” axis. BO3 triangles linked chains in a three-dimensional framework. Rubidium atoms occupied empty ones in channels. The thermal behavior of Rb3Tm2B3O9 was studied in detail in between 25 and 1200 °C by DSC and TG methods. Rb3Tm2B3O9 was congruently melted at 886 °C. The band gap is found as Eg ∼5.14 eV. Nonlinear optical response of Rb3Tm2B3O9 tested via SHG is estimated to be lower than that of KDP. The existence of BO3 groups in Rb3Tm2B3O9 crystal structure has been confirmed by an IR analysis.