The mechanical properties of brittle coating structures were characterized by various indentation techniques. The adhesion properties of the coatings were evaluated by in situ scratch and sphere indentation method. Physical vapor deposited TiN coatings on transparent substrates, sapphire, were scratched by diamond cone indenter and in situ observed through the transparent substrate. In situ scratch results reveal that the failure of coating is originated from the damage of the substrate and the plastic deformation of substrate is a primary factor for determining the adhesion breakage. The unique characterization technique for the strength measurement of brittle thin coating has been developed. The strength of the thin coating was evaluated by the sphere indentation on the trilayer structure. The CVD SiC coatings on graphite were characterized by the technique. It is concluded that the microstructure of SiC coatings influences the strength. In this paper, the various indentation technique were applied to evaluate the mechanical properties of TiN and SiC coatings and the effect of microstructure on the reliability of the brittle coating system was discussed.