Densification mechanisms during reactive spark plasma sintering of Titanium diboride and Zirconium diboride

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.