Densification and microstructure of spark plasma sintered TiB2 ceramics with AlN addition

In this research study, the effects of aluminum nitride (AlN) additive on the densification behavior and microstructure development of titanium diboride (TiB2) based ceramic matrix composite were investigated. In this way, a monolithic TiB2 ceramic and a TiB2–5 wt% AlN ultrahigh temperature ceramic composite were fabricated by spark plasma sintering (SPS) process at a temperature of 1900 °C for a dwell time of 7 min under an externally applied pressure of 40 MPa in vacuum conditions. The relative density measurements were carried out using the Archimedes principles for evaluation of bulk density and the rule of mixtures for calculation of theoretical density. Compared to the additive-free monolithic TiB2 ceramic sample with a relative density of ~96%, the addition of AlN as a sintering aid greatly improved the sinterability of TiB2 matrix composite and a near fully dense sample with a relative density of ~100% were obtained by spark plasma sintering process. The removal of harmful oxide impurities of titania (TiO2) and boria (B2O3) from the surfaces of starting TiB2 powder particles and the in-situ formation of new phases such as aluminum diboride (AlB2) and Al2Ti as an intermetallic compound of aluminum and titanium, not only improved the sinterability of the composite ceramic, but also significantly prevented the extreme growth of TiB2 grains.