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A simple solid-phase synthetic approach has been exploited for the preparation of Ni-carbon sphere composites using Ni(CH3COO)2•4H2O as nickel source, and vitamin C (L-ascorbic acid) as reductant and carbon source at 500oC for 6 h. The products were characterized by X-ray diffraction analysis (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray energy dispersive spectrometer (EDS), raman spectroscopy and microwave-absorbing measurement. The results show that the products are composed of Ni-carbon sphere particles with average diameters of 1.2 µm. Each sphere particle contains embedded Ni particles with average diameters of 83 nm. The reflection loss (RL) values of the products are lower −10 dB at 2–18 GHz, displaying broad range of microwave absorption. Their minimum RL value is about −33 dB at 4.2 GHz, which exhibit good microwave absorbing properties.