Herein, Mg1−x
Ni
x
ZrTa2O8 (x = 0, 0.1, 0.3, 0.5, 0.8, 1) ceramics are synthesized using a solid‐phase reaction method. Ni2+ replacing Mg2+ improves the drawback of high sintering temperature and poor temperature stability. The samples have the relative density above 95% at the optimal sintering temperature. The sintering temperature of Mg1−x
Ni
x
ZrTa2O8 reduces from 1475 °C to 1400 °C. And single‐phase Mg1−x
Ni
x
ZrTa2O8 ceramics with monoclinic wolframite structure are analyzed. According to the Rietveld refinement results, with the doping of Ni2+, the transformation of unit cell volume leads to the shift of the main peak in the XRD pattern to a higher angle in 0 ≤ x ≤ 0.3 and a lower angle in 0.5 ≤ x ≤ 1. The εr of Mg1−x
Ni
x
ZrTa2O8 is comparable to MgZrTa2O8. At 1400 °C, the Q×f is increased from 10,598 GHz in the undoped sample to 43,041 GHz in Mg0.9Ni0.1ZrTa2O8 ceramic. The absolute values of τf of ceramic samples decrease with the excessive Ni2+. The desirable dielectric properties (εr = 20.79, Q×f = 43,041 GHz, τf = −33.04 ppm/°C) are obtained at 1400 °C. Ni substitution is effective for MgZrTa2O8 ceramic to optimize densification temperature and retain the high Q×f value.This article is protected by copyright. All rights reserved.