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(Hf 1-x Zr x)B 2 solid solution powders were synthesized by two methods. First, solution-based processing of HfCl 4 , ZrCl 4 , sucrose, and H 3 BO 3 was conducted followed by heat treatment in Argon to carry out the carbothermal reduction (CTR) reaction to form the diboride powders. Alternatively, in the so-called borohydride reduction (BHR) method, HfCl 4 , ZrCl 4 and NaBH 4 were mixed in an Argon glove box followed by heat treatment in Argon at 700−1500 °C. The synthesized powders were characterized by XRD, SEM, TEM, EDS, and TGA, and the influence of different parameters such as starting composition, heat treatment temperature and time on products characteristics were revealed. Both CTR and BHR solid solution powders were then consolidated within ∼5 min in a homemade flash sintering (FS) setup. The composition, microstructure, hardness, and thermal-oxidation properties of flash sintered ceramics were characterized, and the implication of this study and directions for future research were discussed. [ABSTRACT FROM AUTHOR]

In this research, near fully dense single phase bulk multicomponent transition metal nitride (Nb1/3Ta1/3Ti1/3)N1−δ has been successfully synthesized from mixed commercial powders of NbN, TaN and TiN via reaction flash sintering technique. This was performed with an applied pressure of ~ 35 MPa at 25°C under a constant DC electric field (~24‐32 V/cm). The flash event, which is the abrupt increase in current (up to ~ 25.2 A/mm2) and temperature, occurred without preheating. The threshold power dissipation on the sample right before the flash is ~ 0.7 W/mm3. The formation of single phase (Nb1/3Ta1/3Ti1/3)N1−δ random solid solution and its compositional uniformity were confirmed by XRD and EDS, respectively. The effects of ball milling duration and limiting current density on phase formation were studied. Simulation based on Joule heating provides an estimate of the ultimate sample temperature of ~ 1850°C. Vickers hardness of the obtained (Nb1/3Ta1/3Ti1/3)N1−δ is 17.6 ± 0.6 GPa, which is comparable to similarly flash sintered ingredient binary nitrides of TaN and NbN. TGA in air shows that the oxidation resistance of (Nb1/3Ta1/3Ti1/3)N1−δ is better than that of TaN and NbN but inferior to TiN. The study demonstrates that reaction flash sintering can be a highly efficient technique for synthesizing bulk multicomponent ceramics for both material fundamental investigations and application development. [ABSTRACT FROM AUTHOR]