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ZrWMoO8 powders with different morphologies were obtained using ammonium ttmgstate, molybdate tung-state and zirconium tungstate as the starting materials by dehydrating the precursor ZrWMoO7(OH)2(H20)2. The pre-cursor was studied by thermo-gravimetric and differential scanning calorimetry (TG-DSC). The influence of the gelling agents (HCI, HCIO4, HNO3, H2SO4 and H3PO4) on the crystal-lization process and crystal morphology of the products pre-pared was investigated by X-ray powder diffraction (XRD),scanning electron micrograph (SEM) and X-ray fluorescence spectrometer (XRF). Results showed that the morphology of the ZrWMoO8 particles can be simply adjusted by changing the gelling agents, and the thermal expansion coefficients of cubic ZrWMoO8 prepared in HCI solution are -3.84 ×10-6 K-1 from 100℃ to 700℃.