Whenever a nanoindent is placed near an edge, such as the free edge of the specimen or heterophase interface intersecting the surface, the elastic discontinuity associated with the edge produces artifacts in the load–depth data. Unless properly handled in the data analysis, the artifacts can produce spurious results that obscure any real trends in properties as functions of position. Previously, we showed that the artifacts can be understood in terms of a structural compliance, Cs, which is independent of the size of the indent. In the present work, the utility of the SYS (Stone, Yoder, Sproul) correlation is demonstrated in its ability to remove the artifacts caused by Cs. We investigate properties: (i) near the surface of an extruded polymethyl methacrylate rod tested in cross section, (ii) of compound corner middle lamellae of loblolly pine (Pinus taeda) surrounded by relatively stiff wood cell walls, (iii) of wood cell walls embedded in a polypropylene matrix with some poorly bonded wood–matrix interfaces, (iv) of AlB2 particles embedded in an aluminum matrix, and (v) of silicon-on-insulator thin film on substrate near the free edge of the specimen.

Despite active development over the past 15 years, contemporary nanoindentation methods still suffer serious drawbacks, particularly long thermal stabilization and thermal drift, which limit the duration of the measurements to only a short period of time. The presented work introduces a novel ultra nanoindentation method that uses loads from the μN range up to 50 mN, is capable of performing long-term stable measurements, and has negligible frame compliance. The method is based on a novel patented design, which uses an active top referencing system. Several materials were used to demonstrate the performance of the method. The measurements with hold at maximum load confirm extremely low levels of instrument thermal drift. The presented Ultra Nanoindentation Tester opens new possibilities for testing thin films and long-term testing, including creep of polymers at high resolution without the need of long thermal stabilization.

Internal microstructural length scales play a fundamental role in the strength and ductility of a material. Grain boundaries in nanocrystalline structures and heterointerfaces in nanolaminates can restrict dislocation propagation and also act as a source for new dislocations, thereby affecting the detailed dynamics of dislocation-mediated plasticity. Atomistic simulation has played an important and complementary role to experiment in elucidating the nature of the dislocation/interface interaction, demonstrating a diversity of atomic-scale processes covering dislocation nucleation, propagation, absorption, and transmission at interfaces. This article reviews some atomistic simulation work that has made progress in this field and discusses possible strategies in overcoming the inherent time scale challenge of finite temperature molecular dynamics.

This study proposes a method developed to simultaneously solve contact hardness and reduced modulus by loading and unloading coefficients together with the inclined angle of an indenter. The ratios of the applied load to the squared slopes of load–depth curves during loading and unloading processes were used to determine loading and unloading coefficients. The values of the contact area estimated by the present method were found to be precise for a variety of materials. Compared to the reduced modulus, errors due to underestimated contact area were found more significant in the evaluation of contact hardness.

In the present paper the formulas for the stiffnesses of a new and more general surface tester concept are given and discussed. The concept is based on the idea that the next generation of surface testers will provide the means to use all degrees of freedom of movement a probe on a sample surface could perform. Thus, in addition to the ordinary normal stiffness, lateral and tilting stiffness are measured, as well as twisting stiffness, and then used in the subsequent parameter determination of the investigated materials. It is shown in the paper that such a concept would not only solve classical problems such as “pileup” and “sink-in” completely, but it would also supersede the need of area-function calibration for the indenter tips and allow direct measurement of local intrinsic and residual stresses, anisotropy, and many other things, too.

A data analysis procedure has been developed to estimate the contact area in an elasto-plastic indentation of a thin film bonded to a substrate. The procedure can be used to derive the elastic modulus and hardness of the film from the indentation load, displacement, and contact stiffness data at indentation depths that are a significant fraction of the film thickness. The analysis is based on Yu's elastic solution for the contact of a rigid conical punch on a layered half-space and uses an approach similar to the Oliver-Pharr method for bulk materials. The methodology is demonstrated for both compliant films on stiff substrates and the reverse combination and shows improved accuracy over previous methods.

In this study, nucleation of dislocations in magnesium oxide (MgO) during nanoindentation with a spherical indenter is investigated. For flat and defect-free surfaces prepared by chemo/mechanical polishing, reversible load–displacement curves have been obtained for load as high as 300 mN, whereas on a cleaved MgO surface, pop-in and plastic deformation occur at 10 mN with the same indenter. Furthermore, these reversible curves deviate from the Hertz contact theory. Indented areas have then been characterized by atomic force microscopy and nanoetching. In some cases, few slip lines are observed for reversible indentation tests. However, the slip lines position indicate that the nucleation process of the corresponding dislocations is different from that involved during a pop-in phenomenon.

In the present work a new equation to determine the internal material length scale for strain gradient plasticity theories from two independent experiments (uniaxial and nanoindentation tests) is introduced. The applicability of the presented equation is verified for conventional grained as well as for ultrafine-grained copper and brass with different amounts of prestraining. A significant decrease of the experimentally determined internal material length scale is found for increasing dislocation densities due to prestraining. Conventional mechanism strain gradient plasticity theory is used for simulating the indentation response, using experimentally determined material input data as the yield stress, the work-hardening behavior and the internal material length scale. The work-hardening behavior and the yield stress were taken from the uniaxial experiments, whereas the internal material length scale was calculated using the yield stress from the uniaxial experiment, the macroscopic hardness H0 and the length scale parameter h* following from the nanoindentation experiment. A good agreement between the measured and calculated load–displacement curve and the hardness is found independent of the material and the microstructure.

This work uses crystal plasticity finite element simulations to elucidate the role of elastoplastic anisotropy in instrumented indentation P–hs curve measurements in face-centered cubic (fcc) crystals. It is shown that although the experimental fluctuations in the loading stage of the P–hs curves can be attributed to anisotropy, the variability in the unloading stage of the experiments is much greater than that resulting from anisotropy alone. Moreover, it is found that the conventional procedure used to evaluate the contact variables ruling the unloading P–hs curve introduces an uncertainty that approximates to the more fundamental influence of anisotropy. In view of these results, a robust procedure is proposed that uses contact area measurements in addition to the P–hs curves to extract homogenized J2-plasticity-equivalent mechanical properties from single crystals.

Using the extended Hertzian approach (EHA), the “effectively shaped indenter” corresponding to Pharr's concept is described in terms of a parameter set {d0,d2,d4,d6}, which can be determined by a fitting procedure from the unloading curve of an indentation experiment. Owing to the limited accuracy of measurement, a given experimental curve may in principle correspond to more than one such parameter set. Based on indentation experiments with a Berkovich indenter into fused silica, we have investigated the influence of the fitting procedure itself on the results. We suggest a certain manual fitting procedure, which delivered a yield strength Y = (7.1 ± 0.1) GPa independent of the maximum load. Manual fitting always includes some degree of subjectivity, however, both Y and the elastic field as a whole proved to be relatively robust against modifications of the parameter set. We also suggest a preliminary objective procedure, which delivered Y = 6.8 − 7.1 GPa. In addition, we have performed finite element method (FEM) simulations of elastic–plastic indentations of a conical indenter into a von Mises solid with a yield strength of Y = 7.0 GPa. The simulated unloading curve was analyzed using the EHA in the same manner as the experimental curves, and yield strength of 6.95 GPa was obtained being very close to the input value of the FEM.

Atomistic simulations of nanoindentation of a 20-nm-thick Ni thin film oriented in the [111] direction were carried out to study the effects of indenter velocity and radii, interatomic potentials, and the boundary conditions used to represent the substrate. The simulation results were compared directly with experimental results of Ni thin film of the same thickness and orientation. It was found that the high indenter velocity does not affect the hardness value significantly. Different radii used for indentation also have negligible effects on the hardness value. Two different interatomic potentials were tested, giving significantly different hardness values but both within 20% of the experimental result. Different boundary conditions used to represent the substrate have a significant effect for relatively deep indentation simulations.

In this work, the effects of indenter tip roundness on the load–depth indentation curves were analyzed using finite element modeling. The tip roundness level was studied based on the ratio between tip radius and maximum penetration depth (R/hmax), which varied from 0.02 to 1. The proportional curvature constant (C), the exponent of depth during loading (α), the initial unloading slope (S), the correction factor (β), the level of piling-up or sinking-in (hc/hmax), and the ratio hmax/hf are shown to be strongly influenced by the ratio R/hmax. The hardness (H) was found to be independent of R/hmax in the range studied. The Oliver and Pharr method was successful in following the variation of hc/hmax with the ratio R/hmax through the variation of S with the ratio R/hmax. However, this work confirmed the differences between the hardness values calculated using the Oliver–Pharr method and those obtained directly from finite element calculations; differences which derive from the error in area calculation that occurs when given combinations of indented material properties are present. The ratio of plastic work to total work (Wp/Wt) was found to be independent of the ratio R/hmax, which demonstrates that the methods for the calculation of mechanical properties based on the indentation energy are potentially not susceptible to errors caused by tip roundness.

For elastic–plastic contacts, we propose a complete description of the plastic strain field beneath the indenter during indentation and scratch with a spherical indenter (with R, the tip radius), as a function of the testing conditions, defined by the geometrical strain, noted a/R (with a, the contact radius), and the local friction coefficient μloc. The main parameter of the description is the level of the plastic deformation imposed during test into amorphous polymeric surfaces, related in first approximation to the ratio a/R. An equivalent average plastic strain, noted (εp)av, is calculated over a representative plastically deformed volume, both for indentation and scratch tests. The equivalent average plastic strain (εp)av, is observed to increase with the ratio a/R, as predicted by the empirical Tabor's rule, but also with the local friction coefficient μloc for a given ratio a/R, especially during scratching. The plastic zone dimensions and the plastic strain gradient developed beneath the moving tip are shown to depend both on the geometrical strain a/R and also on the friction coefficient μloc.

The present paper deals with the plastic deformation process into metallic materials occurring in the subindenter region during the loading cycle of spherical indentation test. Load–indentation-depth curve and plastic strains field evolution in the region beneath the indenter are examined using finite element analysis (FEA). The FE model was set up and validated by comparison with experimental spherical indentations carried out on two different materials (Al6082-T6, AISI H13) under four different friction conditions, corresponding to friction coefficients equal to 0.0, 0.1, 0.3, and 0.5. It is confirmed that friction effects on load–indentation-depth curves are negligible for the investigated penetration depths, whereas the plastic deformation process is affected by the contact conditions. The investigation shows that, although the L–h curve is not affected by the contact conditions up to medium values of the penetration depth, remarkable effects are produced in the overall plastic core under the indenter. A strong correlation between plastic strains field and friction coefficient is especially observed at low values of this parameter, whereas a saturation of the phenomena is found for medium-high values of the friction coefficient.

The hydrogen effect on dislocation nucleation in FeAl single crystal with (100) surface orientation has been examined with the aid of a specifically designed nanoindentation setup for in situ electrochemical experiments. The effect of the electrochemical potential on the indent load–displacement curve, especially the unstable elastic-plastic transition (pop-in), was studied in detail. The observations showed a reduction in the pop-in load for both samples due to in situ hydrogen charging, which is reproducibly observed within sequential hydrogen charging and discharging. Clear evidence is provided that hydrogen atoms facilitate homogeneous dislocation nucleation.

The spherical indentation strength of a lead zirconate titanate (PZT) piezoelectric ceramic was investigated under poled and unpoled conditions and with different electrical boundary conditions (arising through the use of insulating or conducting indenters). Experimental results show that the indentation strength of the poled PZT is higher than that of the unpoled PZT. The strength of a poled PZT under a conducting indenter is higher than that under an insulating indenter. Poling direction (with respect to the direction of indentation loading) did not significantly affect the strength of material. Complementary finite element analysis (FEA) of spherical indentation of an elastic, linearly coupled piezoelectric half-space is conducted for rationalizing the experimental observations. Simulations show marked dependency of the contact stress on the boundary conditions. In particular, contact stress redistribution in the coupled problem leads to a change in the fracture initiation, from Hertzian cracking in the unpoled material to subsurface damage initiation in poled PZT. These observations help explain the experimental ranking of strength the PZT in different material conditions or under different boundary conditions.