The kinetics of the synthesis of elemental nanoscaled multilayers of Ti and Al in the regime of continuous heating from 300 K up to 973 K was investigated. A series of sputter deposited Ti/Al multilayer thin films with individual layer thickness (d) from 4 nm up to 1000 nm have been used. Differential scanning calorimetry, Friedman-Gupta, Kissinger and Surinach methods of complex kinetic analysis, classical and time resolved X-ray diffraction and scanning electron microscopy have been applied. In the Ti/Al multilayers the sequence of reactions leading to the final product TiAl (and Ti3Al) is determined. The final products as well as the kinetics of their formation depend on the individual layer thickness. Three different kinetic regimes depending on the layer thicknesses have been found. (C) 2008 Elsevier B.V. All rights reserved.