Microstructure and Indentation Size-Effect in Pure Niobium Subjected to SPD via ECAP and HPT

Abstract

A commercially pure niobium has been subjected to SPD at room temperature ( ~0.11 TM) via ECAP (90º, route BC) up to 16 passes and via HPT up to shear strains γ =1000. ECAP-ed samples show an equiaxed structure after 8 and 16 passes with a decreasing average grain size. The results show that both the microstructure and mechanical properties of ECAP-ed samples do not reach a steady state up to at least 16 passes. HPT samples show at outer region a finer structural size but similar hardness values at similar equivalent strains. The nanoindentation results show an evident indentation size-effect even for the most deformed samples. The hardness values at the nano level converge for the recrystallized, the ECAP-ed and the HPT samples. This implies that, at the nano level, when the geometrically necessary dislocation density overcomes significantly the (initial) statistically stored dislocation density, hardness depends mainly on the physical intrinsic properties of the material (Burgers modulus, bulk modulus...) and the contribution of bulk mechanical properties (i.e., bulk yield strength) to hardness is smoothed down. Strain-rate sensitivity (SRS) of plastic strength has been also measured by means of rate-jump nanoindentation tests. The SRS is proportional to the inverse of hardness.