A reliable and optimized process to grow carbon nanotubes (CNTs) in templated pores of polymer derived ceramic (PDC) matrixwas developed. It is realized through the pyrolysis of a preceramic polymer,i.e., poly (methyl-phenyl-silsesquioxane) (denoted as PMPS), in argon atmosphere at 1000°Ctogether with nickel-catalyst-coatedpoly-methyl-methacrylate (PMMA) microbeads (denoted as PMMA-Ni). PMPS served as both a precursor for the ceramic matrix and a carbon source for the CNT growth. PMMA microbeads were used as sacrificial pore formers and coated with nickel via an electroless plating method, which provides much betteran improved control of particle size of the catalyst and its distribution in the material. The influence of PMMA-Ni loading on the in situ growth of CNTs and the properties of CNTs/SiOCnanocomposites were studied through thermogravimetric analysis (TGA), scanning electron microscopy (SEM), X-ray diffraction (XRD), Raman spectroscopy, and density/porosity measurements. Under optimized conditions, uniform distribution of in situ grown CNTs was observed within the templated pores of the SiOC matrix.The optimized process leads to reproducible high yield of CNTs in the pores.The development of such novelCNT/cellular ceramicnanocomposite materials is of significant interest for a variety of sensor applications.