This work aims at solving the problems of difficult dispersion, easy oxidation and high cost of nano carbon during application, carbon/magnesium aluminate spinel (C/MgAl2O4) composite powders were prepared using MgC2O4·2H2O, MgO2, Al2O3 powder, and Al powder as raw materials by combustion synthesis. The results indicate that with the maximum MgC2O4·2H2O addition of 33.34 mass%, the prepared powder contains 1.17 mass% of carbon and carbon distributes among spinel grains. The MgAl2O4 spinel shows both granular and rod-like morphologies. The granular MgAl2O4 spinel is generated from mutual diffusion between MgO and Al2O3; while the rod-like MgAl2O4 spinel is mainly formed by the vapor-solid growth mechanism from Mg vapor and Al2O3.