Abstract
In this study, dense fine-grained ZrB2 and TiB2 were fabricated using reactive spark plasma sintering (RSPS) of ball-milled Zr/B and Ti/B mixtures. Systematic investigations were carried out to understand the mechanisms of reactive sintering. Two densification mechanisms were found to be operating during RSPS. The first stage of densification was due to self-propagating high temperature synthesis reaction leading to formation of ZrB2 and TiB2 compacts having relative density of ~48 and ~65%, respectively. The second stage of densification occurred at temperatures more than 1100 °C and resulted in final relative density of more than 98%. Electron backscatter diffraction and electron microscopy studies on interrupted RSPS samples as well as dense samples showed deformed grains and presence of slip steps while grain orientation spread map and pole figure analysis confirmed plastic flow. Plastic flow-aided pore closure is shown as major mechanism during reactive sintering.
Acknowledgements
Authors thank Dr N. Saibaba of Nuclear Fuel Complex (Hyderabad, India) for providing Zirconium powder. Authors would like to thank Dr V. Subramanya Sarma of Indian Institute of Technology Madras for helpful discussions regarding EBSD measurements.