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In following are presented the characterization results of nanostructured hybrid composites using alumina matrix reinforced with nanostructured particles of Ni, Ti and soot. The soot used in this work is the byproduct from the synthesis of Carbon Nanotubes (CNT) or fullerene and contains traces (>1wt%) of either CNT or fullerene. Ni and Ti are used in this work for their inherent catalytic ability for heterogeneous nucleation of carbon nanostructures (nanotubes, fullerenes). The hybrid composites are produced by a combination of methods including mechanical milling, sonication, and Spark Plasma Sintering (SPS). Mechanical milling is conducted in high energy mills, the milled and as manufactured powders are sonicated to assure their dispersion, homogeneity and promote percolation of the components during sintering. Mechanical milling and SPS have positive effects to promote the synthesis of different carbon nanoparticles. For instance, it is observed that mechanical milling of fullerene soot sponsors the synthesis of nanostructured diamond particles and using SPS can be synthesized diamond too and fullerene. Although, it is important to notice that SPS conditions are critical to the amount and type of synthesized particles. The use of CNT soot sponsors porosity, hence lower density resulting in an ideal material for membrane and porous media applications. The results of characterization (X-Ray diffraction, electron microscopy (scanning and transmission)) and the mechanical properties (Vickers microhardness) are discussed accordingly.