Calibration issues for nanoindentation experiments: Direct atomic force microscopy measurements and indirect methods

This article discusses calibration issues for shallow depth nanoindentation experiments with Berkovich tips with respect to the accurate measurement of the diamond area function (DAF). For this purpose, two different calibration procedures are compared: (i) the direct measurement of the DAF through atomic force microscopy (AFM) imaging of the Berkovich tip at shallow depth and (ii) a novel indirect calibration method based on an iterative robust and converging scheme in which both reduced modulus and indentation hardness are simultaneously used. These results are obtained by indentation measurements on a standard specimen of fused silica, performed in the 0.5-200 mN load range with a Berkovich indenter. Direct tip shape measurements were carried out through different AFM methods. Comparisons with the standard indirect calibration procedure are also reported. For both the indirect calibration procedures a sensitivity and convergence study is presented. Microsc. Res. Tech. 73:996-1004, 2010.