A series of title compounds as well as their precursors were synthesized by precursor route. Their PXRD patterns were characterized with ZrW2O8 or ZrMo2O8 model by Rietveld method. The thermal contractions of the compounds were determined according to the variable-temperature PXRD data and NTE coefficients were presented. The two-phase mixture of ZrW0.4Mo1.6O8 was also analyzed individually. A series of title compounds as well as their precursors were synthesized by precursor route. Their PXRD patterns were characterized with ZrW2O8 or ZrMo2O8 model by Rietveld method. The thermal contractions of the compounds were determined according to the variable-temperature PXRD data and NTE coefficients were The two-phase mixture of ZrW0.4Mo1.6O8 was also characterized individually.