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To develop transparent materials with superior mechanical properties, nanocrystalline magnesium aluminate (MgAl 2 O 4) spinel with grain sizes ranging from 3.7 to 80 nm has been synthesized by environmentally controlled pressure assisted sintering. In this study, we investigated the microstructure and grain size dependence of the mechanical properties of nanocrystalline MgAl 2 O 4 by performing transmission electron microscopy, nanoindentation, uniaxial micropillar compression, and micro-cantilever bending. Electron microscopy confirmed that the environmentally controlled pressure assisted sintering technique produces a nearly fully dense grain structure with a porosity of less than 1% in larger grain-sized ceramics and observably pore-free grain structures in the smaller grain-sized ceramics. Mechanical characterization revealed that nanoindentation hardness, compressive fracture strength, and fracture toughness each exhibit distinct grain size dependence. Our experimental results and numerical analyses point to a change in dominant strain accommodating mechanisms from dislocation-based plasticity to shear banding as the grain size is reduced, as previously suggested by the literature. Practical implications of the change in strain accommodation mechanisms manifest as the emergence of indentation size effect, weak grain size dependence of hardness and strength, and a ∼2-fold increase in apparent fracture toughness for the smaller grain-sized ceramics. [Display omitted] [ABSTRACT FROM AUTHOR]

Industrial application of superhard materials (Vickers hardness, HV > 40 GPa) such as diamond and cubic boron nitride is limited by high costs and complex routes of synthesis. Tungsten carbide (WC) is a common industrial material valued for its hardness, but falls well short of qualification as a superhard material even in its less common but harder binderless form (HV ∼ 26 GPa). Importantly, recent efforts have demonstrated the potential for alternative materials, such as WC, to achieve similar hardness to diamond and cubic boron nitride via microstructural refinement. However, despite recent advances in sintering technology, even the smallest grained binderless WC (< 100 nm) has failed to achieve HV values above 33 GPa. In this work, multiple hardening mechanisms are exploited through a unique sintering approach proving WC as a candidate superhard material. Environmentally Controlled – Pressure Assisted Sintering (EC-PAS) is utilized to produce > 99 % dense, binderless nanocrystalline WC ceramics with hardness as high as 39 GPa. The unprecedented WC hardness is attributed to the combined effects of small average crystallite size and, importantly, deformation-induced nanoscale intragranular defects including stacking faults. The demonstration of the superposition of multiple hardening mechanisms provides a new avenue to improve hardness of ceramics beyond traditional Hall-Petch hardening, yielding new classes of superhard materials. [Display omitted] [ABSTRACT FROM AUTHOR]