[en] Samples of BIPBVOX.x (Bi_2V_1_–_xPb_xO_5_._5_–_x_/_2) in the composition range 0.05 ≤ x ≤ 0.20 were prepared by ethylene glycol– citric acid sol–gel synthesis route. Structural investigations were carried out by X–ray diffraction, DTA. The highly conducting γ′– phase was effectively stabilized at room temperature for compositions with x ≥ 0.17. Cyclic voltammetric measurements showed reversible redox reactions of vanadium and irreversible redox reaction of Bi"3"+ in the BIPBVOX system during the first cathodic and anodic sweep. However, a higher stability against the reduction of Bi"3"+ to metallic bismuth was seen for x=0.20.