Composites of TiC and TiB 2 were prepared by self-propagating high-temperature synthesis (SHS). Two routes were attempted; from the elements and from a mixture of anatase, boron oxide, graphite and magnesium. The reactions were monitored in situ by synchrotron X-ray diffraction (λ=0.26102 Å). The powder mixtures were compacted as cylindrical pellets and upon ignition diffraction patterns were collected every 65 ms with a CCD camera. TiC was the first phase to form, followed by TiB 2 . The reactions take place in time scales of 0.1 s. The temperature profile for the first route was established from the peak position and the known thermal expansion coefficients. The microstructure of the final products was different: particles of 10 μm for the first and submicron for the second. The viability of the second route to produce ceramic powders in a cheaper way was confirmed.