Nickel ferrite/coal-based carbon (NiFe2O4/CBC) composites were synthesized by using microwave irradiation and simple hydrothermal method. The effects of reaction conditions on particle size, morphology, magnetic, and microwave absorption properties of the NiFe2O4/CBC composites were systematically studied. In all NiFe2O4/CBC composites, NiFe2O4 microspheres with different shapes and sizes were anchored on the surface of CBC. By adjusting size of the NiFe2O4 particles, dielectric and magnetic properties of the NiFe2O4/CBC composites could be optimized simultaneously. For the NiFe2O4/CBC sample with the average particle size of NiFe2O4 to be 4.69 nm, when the thickness was 4.42 mm, the minimum reflection loss (RLmin) could reach − 63.15 dB at 9.89 GHz. Meanwhile, the maximum effective absorption bandwidth (EABmax) was 4.91 GHz (6.31–11.22 GHz) at a thickness of 5 mm, which almost covered the whole X-band. The s-shaped hysteresis loop of the sample revealed that it had typical superparamagnetic characteristics. The possible mechanism of microwave absorption was also discussed. Our NiFe2O4/CBC composites could be used as a new and efficient microwave absorption material.