本研究以反應燒結法製備(1-x)ZnNb2O6-xTiO2與NiNb2O6-yTiO2微波介電陶瓷。x=0.5，y=1時直接燒結混合原料即可以獲得單一相的Zn0.5Ti0.5NbO4(ZTN)與Ni0.5Ti0.5NbO4(NTN)陶瓷，且密度皆可達理論密度之99%以上。ZTN燒結在1200℃持溫2小時有較佳微波介電特性：Q×f=35000GHz，εr =32.6和τf =-48.38 ppm/℃。NTN燒結在1170℃持溫6小時有較佳微波介電特性：Q×f=3568GHz，εr =53.8和τf =+103.68 ppm/℃。在ZnNb2O6與NiNb2O6陶瓷中分別加入適當量之TiO2可使τf值接近0 ppm/℃，x=0.6時可得較佳微波介電特性：Q×f=19000GHz，εr =49.9和τf =0 ppm/℃，y=0.1時可得Q×f=18700GHz，εr =29.3和τf =-0.05 ppm/℃。添加0.5wt%CuO於ZTN與NTN可以成平飢C燒結溫度，分別於在1070℃/4 h與1130℃/4 h可獲得較佳微波介電特性：Q×f=32000GHz，εr =31.5和τf =-40.89 ppm/℃與Q×f=3579GHz，εr =53.2和τf =+93.81 ppm/℃。 (1-x)ZnNb2O6-xTiO2 and NiNb2O6-yTiO2 ceramics produced using a reaction-sintering process were investigated. Without any calcination involved, pure Zn0.5Ti0.5NbO4 (ZTN) and Ni0.5Ti0.5NbO4 (NTN) phases could be obtained successfully after sintering the pellets with x=0.5, y=1. Pellets with >99% of theoretical density could be obtained. Microwave dielectric properties Q×f=35000GHz, εr =32.6, and τf=-48.38 ppm/oC in ZTN sintered at 1200oC for 2 h and Q×f=35000GHz, εr =32.6, and τf=-48.38 ppm/oC in NTN sintered at 1170oC for 6 h were found. As TiO2 was added into ZnNb2O6 and NiNb2O6 τf values approach 0 ppm/oC could be found. Microwave dielectric properties Q×f=19000GHz, εr =49.9, and τf =0 ppm/oC in pellets with x=0.6 and Q×f=18700GHz, εr =29.3, and τf =-0.05 ppm/oC in pellets with y=0.1 were obtained. With CuO addition, the sintering temperature was lowered to 1070oC for ZTN and 1130oC for NTN. The microwave dielectric properties Q×f=32000GHz, εr =31.5 and τf =-40.89 ppm/oC for ZTN were found. Q×f=3579GHz, εr =53.2 and τf =+93.81 ppm/oC for NTN were found.