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The order–disorder temperature (To–d) of Ba[(Co0.6Zn0.4)1/3Nb2/3]O3ceramics was determined viaX-ray diffraction, Raman spectroscopy and differential thermal analysis, respectively. To–dwas determined to be between 1425 and 1450 °C by a quenching method. The endothermic peak in the DTA curve shows the order–disorder transition. B2O3was applied to tune the densification temperature (Ts) and tailor the microwave dielectric properties. The ordering degree and unloaded quality factor (Qf) are improved when Tsis reduced to 1400 °C at B2O3content of 0.25 mol%. Tsis further decreased and the ordering degree and Qfare decreased when B2O3content is increased to 0.5 mol%. The dielectric constant (εr) and temperature coefficient of resonant frequency (τf) decrease slightly with increasing B2O3content. The optimum microwave dielectric properties (i.e., εr = 34.0, Qf = 50,400 GHz, τf = 5.5 × 10−6/°C) are obtained for the Ba[(Co0.6Zn0.4)1/3Nb2/3]O3-0.25 mol% B2O3ceramics sintered at a lower temperature.