Mould casting and sacrificial templating techniques, common in bioceramic technology, were employed to process porous TaCx ultra-high temperature ceramics intended as novel target materials for isotope separation on-line (ISOL) facilities, aiming primarily at the production of medical radioisotopes. A feedstock of Ta4AlC3 MAX phase powder, polyamide spheres and wax was used to obtain different porous TaCx grades with bimodal pore size distributions. The 'green' bodies underwent de-binding and vacuum annealing to decompose the MAX phase, whereas a reference material was also produced from commercial TaC powders. The thermal stability of the porous TaCx ceramics was assessed at ISOL-relevant conditions by heating in high vacuum up to 2200 degrees C. The MAX phase-derived TaCx porous ceramics evolved from biphasic TaCx/alpha-Ta2C to single-phase TaCx at higher temperatures, due to carbon incorporation. The porous TaCx microstructure was stable at 2200 degrees C with a specific surface area stabilizing at similar to 0.25 m(2)/g and thermal conductivity of 1-4 W/m K.
New bulk MAX phase-based ceramics were synthesized in the Ta–Hf–Al–C and Ta–Nb–Al–C systems. Specifically, (Ta1-x,Hfx)4AlC3 and (Ta1-x,Nbx)4AlC3 stoichiometries with x = 0.05, 0.1, 0.15, 0.2, 0.25 were targeted by reactive hot pressing of Ta2H, HfH2, NbH0.89, Al and C powder mixtures at 1550 °C in vacuum. The produced ceramics were characterized in terms of phase composition and microstructure by X-ray diffraction, scanning electron microscopy, electron probe microanalysis and scanning transmission electron microscopy. The investigation confirmed the existence of such M-site solid solutions with low solute concentrations, as predicted by first-principles calculations. These calculations also predicted a linear trend in lattice parameter evolution with increasing Hf concentration, in agreement with the experimental results. In order to increase the low phase purity of the produced ceramics, Sn was added to form (Ta1-x,Hfx)4(Al0.5,Sn0.5)C3 and (Ta1-x,Nbx)4(Al0.5,Sn0.5)C3 double solid solutions, thus resulting in a higher content of the 413 MAX phase compounds in the produced ceramics.
The present work describes a synthesis route for bulk Ta4AlC3 MAX phase ceramics with high phase purity. Pressure assisted densification was achieved by both hot pressing and spark plasma sintering of tantalum hydride, aluminium and carbon powder mixtures in the 1200-1650{\deg}C range. The phases present and microstructures were characterized as a function of the sintering temperature by X-ray diffraction and scanning electron microscopy. High-purity alfa-Ta4AlC3 was obtained by hot pressing at 1500{\deg}C for 30 min at 30 MPa. The beta-Ta4AlC3 allotrope was observed in the samples produced by SPS. The elastic modulus, Vickers hardness, flexural strength and single-edge V-notch beam fracture toughness of the high-purity bulk sample were determined. The thermal decomposition of Ta4AlC3 into tantalum carbide and Al vapor in high vacuum at 1200{\deg}C and 1250{\deg}C was also investigated, as a possible processing route to produce porous tantalum carbide components.