3D Printing of MgAl₂O₄ Spinel Mesh and Densification Through Pressure-Less Sintering and Hot Isostatic Pressing

MgAl₂O₄ spinel mesh with micro-features of 410 and 250 μm unit cell length and rib thickness, respectively, was three-dimensional (3D) printed and sintered followed by Hot Isostatic Pressing (HIPing). A stable colloidal dispersion of spinel in polymer-water solution was prepared and 3D-printed using a 30-gauge needle (∼100 μm inner diameter) on a regenHU 3D-Discovery bioprinter. Samples were characterized for their density and microstructure. Samples with near theoretical density after HIPing was subjected to mechanical property evaluation such as hardness by Vickers indentation and elastic modulus using nanoindentation technique. Microstructure of sintered samples across the ribs have shown graded grain structure with finer grains near the edges (0.7 μm average) with occasional porosity and coarser grains toward the center of the rib (5.2 μm average). HIPing resulted in substantial grain growth and the average grain size was found to be 10.9 μm (with a variation in the grain size of 2.2 μm along the edges and 13.1 μm at the center of the rib) exhibiting close packed and dense microstructure. Finer grains toward the edges may probably be due to the flow behavior during printing process and lower distribution of the powder loading along the edges resulting in low green density. This relatively higher porosity pining the grain growth under the extremely low heating rate employed for the controlled shrinkage to maintain the integrity of the sample. 3D printed samples after HIPing exhibited a density of 3.57 g/cc and hardness of 12.95 GPa, which are at par with the samples processed through conventional ceramic processing techniques. Nanoindentation studies employing maximum load of 45 mN with depth have shown an elastic modulus of 238 ± 15 GPa. MgAl₂O₄ spinel mesh 3D printed in this study is a potential prospective candidate that can be explored for cranioplasty procedures and other biomedical applications.