Residual stress measurement at the micrometer scale: focused ion beam (FIB) milling and nanoindentation testing

"We present a new procedure for the determination of surface elastic residual stress by instrumented sharp indentation, based on nanoindentation testing on focused ion beam (FIB) milled micro-pillars. Finite element modeling (FEM) of strain relief after FIB milling of annular trenches demonstrates that full relaxation of pre-existing residual stress state occurs when the depth of the trench approaches the diameter of the remaining pillar. Considering this, the average residual stress present in the sample material can be calculated by the comparison of two different sets of load-depth curves, the first one obtained at the center of stress relieved pillars, the second on the undisturbed (residually stressed) surface. Analytical modeling of the contact stress distribution in non-halfspace conditions was adopted to take into consideration the additional boundary conditions given by the edges of pillars and the elastic properties of the substrate (in case of coatings). The results are presented for residual stress evaluation of a 3.8-mu m TiN coating on WC-Co substrate obtained by cathodic arc evaporation-physical vapor deposition (CAE-PVD) techniques, showing an average compressive stress state of -5.63 GPa. This result is in close agreement with the estimation obtained by XRD (sin(2) psi method) analysis of -5.84 GPa of the same sample, adopting the same elastic constants."