Temperature stable MO-ZrO2-Ta2O5 ceramics (M = Co, Ni) were prepared by solid state route. Crystal structure was determined by X-ray diffraction and Raman spectrum. Single-phase MZrTa2O8 was formed through the reaction between intermediate MTa2O6 and residual ZrO2. Quantitative phase analysis verified that changing temperature considerably adjusted the chemical compositions of ceramics. In the case of CoZrTa2O8, the optimum dielectric properties were er∼24.3, Q × f∼95,300 GHz (Q∼11,305 at 8.43 GHz), and τf ∼ -30.50 ppm/°C. The NiZrTa2O8 ceramic had er = 23.5, Q × f = 86,404 GHz (Q∼10,774 at 8.02 GHz), and τf = −20.20 ppm/°C. Their large τf values were compensated since MZrTa2O8 and MTa2O6 had opposite τf. Particularly, near zero τf of −2.67 and 0.22 ppm/°C were obtained for M = Co, Ni at 1150 and 1175 °C, respectively.