Ti Grade 2 was prepared by cryogenic attritor milling in liquid nitrogen and liquid argon. Two types of milling balls were used—stainless steel balls and heavy tungsten carbide balls. The effect of processing parameters on particle size and morphology, contamination of powder and its microhardness was investigated. Milling in liquid nitrogen was not feasible due to excessive contamination by nitrogen. Minor reduction of particle size and significant alterations in particle morphology depended on type of milling balls and application of stearic acid as processing control agent. Heavily deformed ultra-fine grained (UFG) internal microstructure of powder particles was observed by the method of “transmission Kikuchi diffraction”.

Metastable β-Ti alloy Ti-15Mo was prepared by cryogenic ball milling in a slurry of liquid argon. Material remained ductile even at low temperatures, which suppressed particle refinement, but promoted intensive plastic deformation of individual powder particles. Repetitive deformation of powder particles is similar to the multidirectional rolling and resembles bulk severe plastic deformation (SPD) methods. Initial and milled powders were compacted by spark plasma sintering. Sintered milled powder exhibited a refined microstructure with small β-grains and submicrometer sized α-phase precipitates. The microhardness and the yield tensile strength of the milled powder after sintering at 850 °C attained 350 HV and 1200 MPa, respectively. Low ductility of the material can be attributed to high oxygen content originating from the cryogenic milling. This pioneering work shows that cryogenic milling followed by spark plasma sintering is able to produce two-phase β-Ti alloys with refined microstructure and very high strength levels.

The spark plasma sintering (SPS) technique was employed to prepare compacts from (i) gas-atomized and (ii) attritor-milled AE42 magnesium powder. Short attritor-milling was used mainly to disrupt the MgO shell covering the powder particles and, in turn, to enhance consolidation during sintering. Compacts prepared by SPS from the milled powder featured finer microstructures than compacts consolidated from gas-atomized powder (i.e., without milling), regardless of the sintering temperatures in the range of 400–550 °C. Furthermore, the grain growth associated with the increase in the sintering temperature in these samples was less pronounced than in the samples prepared from gas-atomized particles. Consequently, the mechanical properties were significantly enhanced in the material made of milled powder. Apart from grain refinement, the improvements in mechanical performance were attributed to the synergic effect of the irregular shape of the milled particles and better consolidation due to effectively disrupted MgO shells, thus suppressing the crack formation and propagation during loading. These results suggest that relatively short milling of magnesium alloy powder can be effectively used to achieve superior mechanical properties during consolidation by SPS even at relatively low temperatures.