[en] Thin films are used in a wide variety of computing and communication applications although their fatigue behavior and its dependence on alloying elements are not very well known. In this paper, we present an experimental implementation of a novel high-throughput fatigue testing method for metallic thin films. The methodology uses the fact that the surface strain amplitude of a vibrating cantilever decreases linearly from the fixed end to the free end. Therefore, a thin film attached to a vibrating cantilever will experience a gradient of strain and corresponding stress amplitudes along the cantilever. Each cantilever can be used to extract a lifetime diagram by measuring the fatigue-induced damage front that progresses along the cantilever during up to 10⁸ load cycles.

[en] In this study, the uniaxial tension-tension fatigue behavior of fully nanotwinned magnetron sputtered Cu-6wt%Al, Cu-2wt%Al, and Cu-10 wt%Ni is presented. These alloys have average twin thicknesses ranging from 4 to 8 nm, average grain widths from 90 to 180 nm, and tensile strengths from 1 to 1.5 GPa. In the high cycle regime (10³ to 10⁷ cycles), the nanotwinned alloys exhibit fatigue strengths ranging from 210 to 370 MPa, which is higher than previously observed in nanotwinned Cu (fatigue strengths between 80 and 200 MPa). Fatigue strengths are normalized by tensile strength for Cu alloys with different microstructures to study the correlation between tensile and fatigue properties. Post-mortem analysis of the materials reveals a newly observed deformation mechanism, where localized detwinning leads to intergranular fracture between columnar grains. Overall, materials displaying detwinning as a deformation mechanism show lower normalized fatigue strengths in comparison to materials that deform with slip band like behavior.

[en] Highlights: → New FIB-DIC method for the analysis of residual stress gradients in thin coatings. → Semi-automated incremental FIB ring-core milling successfully developed. → Developed procedure gives minimum re-deposition during FIBing. → Significant gradient of residual stress towards the coating/substrate interface detected. → Microstructural effects and elastic anisotropy were taken into account and corrected. - Abstract: A new methodology for the measurement of depth sensitive residual stress profiles of thin coatings with sub-micrometer resolution is presented. The two step method consists of incremental focused ion beam (FIB) ring-core milling, combined with high-resolution in situ SEM-FEG imaging of the relaxing surface and a full field strain analysis by digital image correlation (DIC). The through-thickness profile of the residual stress can be obtained by comparison of the experimentally measured surface strain with finite element modeling using Schajer's integral method. In this work, a chromium nitride (CrN) CAE-PVD 3.0 μm coating on steel substrate, and a gold MS-PVD 1.5 μm on silicon were selected for the experimental implementation. Incremental FIB milling was conducted using an optimized milling strategy that produces minimum re-deposition over the sample surface. Results showed an average residual stress of σ = -5.15 GPa in the CrN coating and σ = +194 MPa in the Au coating. These values are in reasonable agreement with estimates obtained by other conventional techniques. The depth profiles revealed an increasing residual stress from surface to the coating/surface interface for both coatings. This observation is likely related to stress relaxation during grain growth, which was observed in microstructural cross sections, as predicted by existing models for structure-stress evolution in PVD coatings. A correlation between the observed stress gradients and the in-service mechanical behavior of the coatings is proposed. Finally, critical aspects of the technique and the influence of microstructure and elastic anisotropy on stress analysis are analyzed and discussed.

[en] Open-cell graphitic foams were fabricated by chemical vapor deposition using nickel templates and their compressive responses were measured over a range of relative densities. The mechanical response required an interpretation in terms of a hierarchical micromechanical model, spanning 3 distinct length scales. The power law scaling of elastic modulus and yield strength versus relative density suggests that the cell walls of the graphitic foam deform by bending. The length scale of the unit cell of the foam is set by the length of the struts comprising the cell wall, and is termed level I. The cell walls comprise hollow triangular tubes, and bending of these strut-like tubes involves axial stretching of the tube walls. This length scale is termed level II. In turn, the tube walls form a wavy stack of graphitic layers, and this waviness induces interlayer shear of the graphitic layers when the tube walls are subjected to axial stretch. The thickness of the tube wall defines the third length scale, termed level III. We show that the addition of a thin, flexible ceramic Al₂O₃ scaffold stiffens and strengthens the foam, yet preserves the power law scaling. The hierarchical model gives fresh insight into the mechanical properties of foams with cell walls made from emergent 2D layered solids.

[en] High-purity Cu samples containing parallel columns of highly aligned nanotwins with median spacing of ∼25 nm were subjected to tension–compression cyclic loading by a high-throughput cyclic testing method. The methodology utilizes gradients in surface strain amplitude of a vibrating cantilever: one along the beam axis, with decreasing strain from the fixed to the free end of the beam, and the other through the foil thickness with decreasing strain from the surface to the neutral axis. Systematic microstructural investigations indicate that nanotwins are not stable under cyclic loading and that the applied strain amplitude has a strong influence on the resulting twin structure. In the highly stressed regions the detwinning process produces a twin free microstructure, allowing for subsequent extrusion and crack formation, and introduces fatal defects into structural parts