Formation of metastable c-AlN and its effect on the mechanical properties of AlN/(Ti,Al)N nanoscale multilayersA 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 (MoSi 2.2 N 2.5 ) and SiC were deposited by magnetron sputtering from planar MoSi 2 and SiC targets onto single crystal silicon wafers. The relative amount of both components was varied ͑12.5-50 vol. % of SiC͒ while keeping the bilayer thickness constant ͑12 nm͒, or the bilayer thickness was varied ͑6-24 nm͒ with constant Mo-Si-N to SiC ratio ͑25 vol. % of SiC͒. Mechanical properties were measured by nanoindentation on as-deposited films and films annealed in vacuum at 500 and 900°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°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°C in vacuum. The potential of Mo-Si-N as a barrier layer against intermixing between nanolayered MoSi 2 and SiC at 900°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.