Bi2Al4O9 powders were prepared by sol-gel process. The precursors were heated at 500-800°C for 2h to obtain Bi2Al4O9 powder and X-ray diffraction (XRD), Differential thermal analysis (DTA), thermogravimetric analysis (TG), field emission scanning electron microscope (SEM), Fourier transform infrared spectroscopy (FT-IR) techniques were used to characterize precursor and derived oxide powders. XRD analysis show that the powder is still amorphous after calcined at 500°C. The peaks of Bi2Al4O9 become sharp after calcined at 575°C though still existing some amorphous phase. After calcining at 675-800°C, the powder has fully turned into pure Bi2Al4O9 phase. The crystallization process can also be confirmed by DTA-TG and IR. Calcining the precursor at 575°C, the absorption bands at 527 cm-1, 738 cm-1, 777 cm-1, and 919 cm-1are observed, which are assigned to Bi2Al4O9 and becoming stronger and sharper with the increase of temperature.