The preparation of highly dense bulk materials with a grain size in the range of a few to a few hundreds nanometers is currently the objective of numerous studies. In our research we have achieved a measure of success in this regard by using the methods of mechanically-activated, field-activated, pressure-assisted synthesis, MAFAPAS, which has been patented, and mechanically-activated spark plasma sintering, MASPS. Both methods, which consist of the combination of a mechanical activation step followed by a consolidation step under the simultaneous influence of an electric field and mechanical pressure, have led to the formation of dense nanostructured ceramics, intermetallics, and composites, such as, MoSi2 FeAl, NbAl3, and TiN-TiB2. In this report, both one-step synthesis-consolidation and sintering of different nanostructured materials by SPS and FAPAS were investigated. .

An investigation was performed to evaluate the potential of the spark plasma sintering process in producing dense nanostructured materials. Microstructured and nanostructured nickel was sintered by SPS starting from nickel powder (APS 3–7 μm) in the as‐received state and after a mechanical activation using a high‐energy ball mill. First, a sintering study to determine SPS processing conditions to reach full densification was carried out with specimens 50 mm in diameter and 10 mm in height. In a second step, an experimental investigation was undertaken with dense nickel disks to generate tensile properties. The tensile tests were performed at a strain rate of 10⁻³ s⁻¹ with specimens 16 mm in gage length and 4 mm in gage diameter. Tensile ductility in excess of 40% was reached with the microstructured nickel. For the nanostructured nickel, high yield stresses in excess of 600 MPa were measured with a tensile ductility of 30%. These results were analyzed through densification and microstructure measurements.

A FeCoNi(B_0.5Si_0.5) high-entropy alloy with the face-centered cubic (FCC) crystal structure was synthesized by mechanical alloying and spark plasma sintering (SPS). Phase evolution, microstructure, morphology and annealing behaviors were investigated. It was found that a single FCC solid solution appears after 50 h of milling. The grain size was 10 nm after 150 h of milling. Microstructure parameters were calculated by the Rietveld fitting of the X-ray Diffraction patterns. Magnetic characterizations of milled and annealed powders at 650 °C for 1 h were investigated. The heat treatment improves the magnetic properties of the milled powders by enhancing the saturation magnetization value from 94.31 to 127.30 emu/g and decreasing the coercivity from 49.07 to 29.57 Oe. The cohabitation of the FCC phase with the equilibrium crystalline phases observed after annealing is responsible of this magnetic softening. The as-milled powder was also consolidated by spark plasma sintering at 750 and 1000 °C. The obtained specimen consolidated at 750 °C improved the coercivity to 25.06 Oe and exhibited a compressive strength of 1062 Mpa and Vickers hardness of 518 ± 14 HV, with a load of 2 kN. The nanoindentation technique with the Berkovich indentor gave hardness and indentation elastic modulus of 6.3 ± 0.3 Gpa (~640 HV) and 111 ± 4 Gpa for samples consolidated by SPS at 750 °C.