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The formation of Ti2AlN by solid state reaction between layers of wurtzite-AlN and -Ti was characterized by in situ x-ray scattering. The sequential deposition of these layers by dual magnetron sputtering onto Al2O3(0001) at 200 °C yielded smooth, heteroepitaxial (0001) oriented films, with abrupt AlN/Ti interfaces as shown by x-ray reflectivity and Rutherford backscattering spectroscopy. Annealing at 400 °C led to AlN decomposition and diffusion of released Al and N into the Ti layers, with formation of Ti3AlN. Further annealing at 500 °C resulted in a phase transformation into Ti2AlN(0001) after only 5 min.