Nickel-plated aluminum powder was prepared by a double reduction system of sodium hypophosphite and hydrazine. The effects of different amounts of nickel coating on the morphology, phase, compaction resistivity and electromagnetic parameters of nickel-plated aluminum powder coating were studied. The results of XRD and SEM clearly show that the nickel-plated aluminum powder was prepared successfully in a dual reduction system. In addition, the nickel-plated aluminum powder also has good absorbing properties in the X-band. The results show that when the nickel coating amount is 50 w/ % and the impedance matching thickness is 2.6 mm, the reflection loss value is less than –10 dB in the range 8.49–12.40 GHz. At the same time, when the impedance-matching thickness is 2.4 mm and the frequency is 10.45 GHz, the reflection-loss value reaches its best value of –25.88 dB. The composite material presents excellent corrosion resistance and electromagnetic shielding properties, which provides a new strategy for the development of electroless plating composite materials.