Time-resolved x-ray diffraction (TRXRD) was performed during Ti5Si3 synthesis by the self-propagating high-temperature synthesis mode for different Ti size fractions. It was determined that the time for product formation (ca. 15 s) was independent of Ti particle size. However, the formation of Ti5Si4 phase occurred when relatively large titanium particles were used. A simultaneous measurement of the temperature and TRXRD allowed us to attribute the shifting of XRD peaks at high temperature to thermal expansion of the Ti5Si3 product. The thermal expansion coefficients differ for different crystal planes, and their numerical values compare well with those reported previously in the literature.
Time resolved X-ray diffraction of organic polymers around the glass transition