Nano-structured MgAl₂O₄ spinel consolidated by high pressure spark plasma sintering (HPSPS)

Nano-structured transparent polycrystalline magnesium aluminate spinel (PMAS) was fabricated using a high pressure (up to 1000 MPa) spark plasma sintering (HPSPS) apparatus and various properties of the spinel, such as transparency, micro-structure and mechanical properties (specifically, hardness and fracture toughness), were tested. Using a creep densification model, it was concluded that densification in the final stage of HPSPS is controlled by grain boundary sliding (GBS), rather than by oxygen diffusion. The average grain size of PMAS fabricated under 400 MPa pressure at 1200 °C was about 170 nm, while for samples fabricated under 1000 MPa at 1000 °C the average grain size was remarkably smaller (about 50 nm). HRTEM analysis clearly demonstrated clean grain boundaries and triple points with no evidence for the existence of amorphous regions. Fully dense specimens displayed in-line transmittance higher than 80%. It was moreover established that hardness and fracture toughness values did not depend on the indentation load applied. Finally, hardness values for grains sized between tens of microns and tens of nm strictly followed the Hall-Petch relationship.