A study of the microstructure, thermal stability, nanoindentation mechanical properties, and residual stress evolution of nanolayered Mo-Si-N/SiC thin films as a function of vacuum annealing time and temperature is reported. Multilayers of Mo-Si-N (MoSi2.2N2.5) and SiC were deposited by magnetron sputtering from planar MoSi2 and SiC targets onto single crystal silicon wafers. The relative amount of both components was varied (12.5-50 vol. % of SiC) while keeping the bilayer thickness constant (12 nm), or the bilayer thickness was varied (6-24 nm) with constant Mo-Si-N to SIC ratio (25 vol. LTC Of SiC). Mechanical properties were measured by nanoindentation on as-deposited films and films annealed in vacuum at 500 and 900 degrees C. Microstructure and thermal stability were examined by cross-sectional transmission electron microscopy, glancing angle x-ray diffraction and nuclear resonance broadening. Stress evolution induced by thermal annealing was determined by measuring optically the change in curvature of coated silicon beams. In the as-deposited state, all films exhibited an amorphous microstructure. At 900 degrees C SiC still remained amorphous, but Mo-Si-N had developed a microstructure where nanocrystals of Mo-5-Si-3 were embedded in an amorphous matrix. The interface between Mo-Si-N and SiC was indirectly shown to be stable at least up to 41 h annealing at 1075 degrees C in vacuum. The potential of Mo-Si-N as a barrier layer against intermixing between nanolayered MoSi2 and SiC at 900 degrees C has been demonstrated. Hardness, modulus and residual stress followed the volume fraction rule of mixture of both constituents of the nanolayered Mo-Si-N/SiC structure. Consequently, by optimizing the volume fraction of the constituents, zero residual stress on a silicon substrate is possible after annealing.