Composites of M-2.5 mol. % Fullerene C60 composites (where M= Fe or Al) are prepared by mechanical milling and Spark Plasma Sintering (SPS). The SPS technique has been used to consolidate the resulting powders and preserve the massive nanostructure. Results of X-Ray Diffraction and Raman Spectroscopy show that larger milling balls (9.6 mm in diameter) produce transformation of the fullerene phase during mechanical milling. Alternatively smaller milling balls (4.9 mm in diameter) allow retention of the fullerene phase. SEM shows homogeneous powders with different particle sizes depending on milling times. Sintering produces nanostructured composite materials with different reinforcing phases including C60 fullerenes, diamonds and metal carbides. The presence of each phase depends characteristically on the energy input during milling. Transmission Electron Microscopy (TEM) and Raman Spectroscopy show evidence of the spatial distribution and nature of phases. Diamonds and carbides can be identified for the sintered Fe containing composites with a relatively high volume fraction.