Development of modular cryogenic indentation apparatus for investigating micro-region mechanical properties of materials

Abstract

High-precision cryogenic micromechanical testing apparatuses are of significant importance in investigating the micro-region mechanical properties and deformation behaviors of materials at cryogenic temperatures. In this study, a modular cryogenic indentation apparatus was designed and developed utilizing a contact-atmosphere hybrid refrigeration technique with a minimum temperature of −150 °C. The temperature of both the indenter tip and the specimen was independently controlled through a dual-channel proportional–integral–derivative (PID) feedback loop to eliminate contact thermal drift to within 0.1 nm/s. The application of cryogenic nitrogen (N2) atmosphere refrigeration eliminated additional stiffness at the indenter tip completely. The feasibility of the apparatus was demonstrated through calibrations and tests conducted on standard fused silica and single crystal nickel. Highly accurate indentation curves and micro-region mechanical properties of single crystal nickel were obtained at variable cryogenic temperatures. With decreasing temperature, both slip bands and pile-up around residual indentation imprints were weakened. Notably, at −150 °C, the slip bands disappeared, and the phenomenon of pile-up was replaced by sink-in. This developed cryogenic indentation apparatus will be a powerful tool to reveal the effect of cryogenic temperatures on the evolution mechanisms of materials’ micro-region mechanical properties.