Current rate flash sintering of nickel at ambient temperature in <1 min

Abstract

AbstractWe show that powder pressed specimens of nickel can be sintered to 99.96% density by injecting electrical current, without the use of a furnace. Full sintering could be accomplished in 10 to 52 s by changing the current rate from 5 to 1 A/s. In all instances, the samples sintered abruptly at a current density of ∼20 A mm−2. The grain size of the sintered samples was somewhat larger than the nickel powder particle size (∼60 μm vs. 40 μm). Tensile testing yielded a yield strength of 98 MPa, ultimate tensile stress of 323 MPa, and ductility of ∼17%. Four in‐operando measurements are reported: (i) sintering, (ii) the change in resistance with current density, (iii) the temperature, and (iv) electroluminescence. The change in resistance during flash sintering exhibited a high peak followed by a steep decline in resistance; the transient is attributed to the breakdown of particle–particle interface resistance. The same cycle repeated with the flash‐sintered, dense sample, did not show the spike, and gave reproducible results. The resistance data for these latter cycles, when viewed as a function of temperature exhibited sigmoidal behavior: initially lower, and then higher than the literature values. This unusual behavior reflects the influence of defects generated during flash. We have also measured the endothermic enthalpy, expressed by the difference between the in situ input electrical energy and the radiation, convection, and specific heat losses. Dividing by the formation energy of Frenkel pairs yields the concentration of defects, estimated to be 0.3–0.4 mol %. These concentrations are far above thermal equilibrium; it is concluded that flash of metals is a far from equilibrium phenomenon.