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The synthesis of the nickel oxide-gadolinium doped ceria (NiO-GDC with 65:35 wt.%) nanocomposite powders with a stoichiometry of Gd0.1Ce0.9O1.95 was performed via fast solution combustion technique; using three different mixing methods: (i) CM (metal cations in an aqueous solution), (ii) HM (hand mortar), and (iii) BM (ball milling). The nanocomposite powders were calcined at 700 °C for 2 h and characterized by Transmission Electron Microscopy (TEM), X-ray fluorescence (XRF), and X-ray Diffraction XRD. The TEM and XRD analyses evidenced the well-dispersed NiO and GDC crystallites with the absence of secondary phases, respectively. Later, the calcined powders (NiO-GDC nanocomposites) were compacted and sintered at 1500 °C for 2 h. The microhardness of the sintered nanocomposites varies in accordance with the synthesis approach: a higher microhardness of 6.04 GPa was obtained for nanocomposites synthesized through CM, while 5.94 and 5.41 GPa were obtained for ball-milling and hand-mortar approach, respectively. Furthermore, it was observed that regardless of the long time-consuming ball-milling process with respect to the hand mortar, there was no significant improvement in the electrical properties.

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