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Dense fully-002-textured polycrystalline TiN layers, 110 nm thick with a N/Ti ratio of 1.02±0.03, were grown on SiO2 by ultrahigh vacuum magnetically unbalanced magnetron sputter deposition at Ts=450 °C in pure N2 utilizing high N2+/Ti flux ratios and low energy (EN2+=20 eV) ion irradiation of the growing film. Al overlayers, 160 nm thick and possessing a strong 002 texture inherited from the underlying TiN, were then deposited at Ts=100 °C without breaking vacuum. Synchrotron x-ray diffraction was used to follow interfacial reaction paths and kinetics during postdeposition annealing as a function of time (ta=200–1200 s) and temperature (Ta=500–580 °C). Changes in bilayer microstructure and microchemistry were investigated using transmission electron microscopy (TEM) and scanning TEM to obtain compositional maps of cross-sectional and plan-view specimens by energy dispersive x-ray analysis. The initial bilayer reaction step during annealing involves the formation of a continuous AlN interfacial layer whic...