This study covers composite production and characterization of powders obtained by applying the electroless Ni coating technique to Fe–Co powders by microwave sintering technique. The physical, mechanical, and electrical properties of electroless Ni-coated Fe and Co composites samples produced in different compositions by sintering magnetic materials in a microwave oven at 1,100°C were characterized. With the electroless coating technique, a uniform nickel deposit on the Fe–Co particles was coated before sintering with the precipitation procedure. A composite consisting of metallic phase, Fe–Co, and triple additions in a Ni matrix was prepared in an argon atmosphere and sintered by microwave technique. X-ray diffraction, scanning electron microscope, and impedance phase analyzer were used to obtain structural data in the temperature range of 25–40°C and to determine magnetic and electrical properties such as dielectric and conductivity. The ferromagnetic resonance was varied between 10 Hz and 1 GHz, and measurements were made to characterize the properties of the samples. Numerical findings obtained for 25% Ni composition at 1,100°C (Fe–37.5% Co) suggest that the best conductivity and hardness are obtained by adding 25Ni at 1,100°C sintering temperature.