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Nanolaminates are extensively studied due to their unique properties, such as impact resistance, high fracture toughness, high strength, and resistance to radiation damage. Varieties of nanolaminates are being fabricated to achieve high strength and fracture toughness. In this study, one such nanolaminate fabricated through accumulative roll bonding (Cu(16)/Nb(16) ARB nanolaminate, where 16 nm is the layer thickness) was used as a test material. Cu(16)/Nb(16) ARB nanolaminate exhibits crystallographic anisotropy due to the existence of distinct interfaces along the rolling direction (RD) and the transverse direction (TD). Nanoindentation was executed using a Berkovich tip, with the main axis oriented either along TD or RD of the Cu(16)/Nb(16) ARB nanolaminate. Subsequently, height profiles were obtained along the main axis of the Berkovich indent for both TD and RD using scanning probe microscopy (SPM), which was later used to estimate the pile-up along the RD and TD. The RD exhibited more pile-up than the TD due to the anisotropy of the Cu(16)/Nb(16) ARB interface and the material plasticity along the TD and RD. An axisymmetric 2D finite element analysis (FEA) was also performed to compare/validate nanoindentation data, such as load vs. displacement curves and pile-up. The FEA simulated load vs. displacement curves matched relatively well with the experimentally generated load–displacement curves, while qualitative agreement was found between the simulated pile-up data and the experimentally obtained pile-up data. The authors believe that pile-up characterization during indentation is of great importance to documenting anisotropy in nanolaminates.

This work reports results from quasi-static nanoindentation measurements of iron, in the un-strained state and subjected to 15% tensile pre-straining at room temperature, 125 °C and 300 °C, in order to extract room temperature hardness and elastic modulus as a function of indentation depth. The material is found to exhibit increased disposition for pile-up formation due to the pre-straining, affecting the evaluation of the mechanical properties of the material. Nanoindentation data obtained with and without pre-straining are compared with bulk tensile properties derived from the tensile pre-straining tests at various temperatures. A significant mismatch between the hardness of the material and the tensile test results is observed and attributed to increased pile-up behaviour of the material after pre-straining, as evidenced by atomic force microscopy. The observations can be quantitatively reconciled by an elastic modulus correction applied to the nanoindentation data, and the remaining discrepancies explained by taking into account that strain hardening behaviour and nano-hardness results are closely affected by dynamic strain ageing caused by carbon interstitial impurities, which is clearly manifested at the intermediate temperature of 125 °C.

The paper presents a statistical study of nanoindentation results obtained in seven European laboratories that have joined a round robin exercise to assess methods for the evaluation of indentation size effects. The study focuses on the characterization of ferritic/martensitic steels T91 and Eurofer97, envisaged as structural materials for nuclear fission and fusion applications, respectively. Depth-controlled single cycle measurements at various final indentation depths, force-controlled single cycle and force-controlled progressive multi-cycle measurements using Berkovich indenters at room temperature have been combined to calculate the indentation hardness and the elastic modulus as a function of depth applying the Oliver and Pharr method. Intra- and inter-laboratory variabilities have been evaluated. Elastic modulus corrections have been applied to the hardness data to compensate for materials related systematic errors, like pile-up behaviour, which is not accounted for by the Oliver and Pharr theory, and other sources of instrumental or methodological bias. The correction modifies the statistical hardness profiles and allows determining more reliable indentation size effects.