Metrological Comparison of Indirect Calibration Methods for Nanoindentation: A Bootstrap-Based Approach.

Area shape function and frame compliance are the most critical parameters in nanoindentation, as they control measurement accuracy and represent the largest contributions to measurement uncertainty. Despite the availability of direct calibration methods, indirect calibrations are the most practical and fast. Thus, the indirect calibration methods proposed in ISO 14577-2 are most typically applied in academic and industrial research, as well as in quality controls. Previous research has highlighted some criticalities, but a holistic metrological framework was missing. This work aims to compare the performances of indirect calibration methods for area shape function and frame compliance in the nano-range, considering different alternatives suggested in the standard and most recent literature. The comparison will be based on uncertainty estimation using bootstrap estimation, which will innovatively highlight and introduce the effect of the nanoindentation dataset in the uncertainty estimation. The results show that the optimization of accuracy and uncertainty in mechanical characterization is achieved by indenting pairs of certified reference materials, resulting in a more robust approach to calibration experimental conditions than methods that require a single sample to be indented.