Metrological Comparison of Available Methods to Correct Edge-Effect Local Plasticity in Instrumented Indentation Test.

The Instrumented Indentation Test (IIT) mechanically characterizes materials from the nano to the macro scale, enabling the evaluation of microstructure and ultra-thin coatings. IIT is a non-conventional technique applied in strategic sectors, e.g., automotive, aerospace and physics, to foster the development of innovative materials and manufacturing processes. However, material plasticity at the indentation edge biases the characterization results. Correcting such effects is extremely challenging, and several methods have been proposed in the literature. However, comparisons of these available methods are rare, often limited in scope, and neglect metrological performance of the different methods. After reviewing the main available methods, this work innovatively proposes a performance comparison within a metrological framework currently missing in the literature. The proposed framework for performance comparison is applied to some available methods, i.e., work-based, topographical measurement of the indentation to evaluate the area and the volume of the pile-up, Nix-Gao model and the electrical contact resistance (ECR) approach. The accuracy and measurement uncertainty of the correction methods is compared considering calibrated reference materials to establish traceability of the comparison. Results, also discussed in light of the practical convenience of the methods, show that the most accurate method is the Nix-Gao approach (accuracy of 0.28 GPa, expanded uncertainty of 0.57 GPa), while the most precise is the ECR (accuracy of 0.33 GPa, expanded uncertainty of 0.37 GPa), which also allows for in-line and real-time corrections.