This paper presents the analysis of the mean crystallite size and microstress in thin titanium silicide films based on the broadening of x‐ray diffraction profiles. The titanium silicide specimens were obtained by rapid thermal annealing of thin titanium films deposited on single‐crystal silicon substrate. The experimental results have shown either the face centered orthorhombicC54 type TiSi2structure with mean crystallite size of 50 nm or the base centered orthorhombicC49 type TiSi2structure with 20 nm mean crystallite size, depending on annealing conditions. A decrease in the microstress has been observed with increasing annealing times at 800 °C, without significant variations of the mean crystallite size.