The plastic deformation behavior of Knoop indentations made in a soft, porous titanium/aluminum multilayered thin film on a hard silicon substrate is studied through use of the focused-ion-beam milling and imaging technique. Pileup is observed for indentations with depths larger than 30% of the total film thickness. Analysis of the indentation cross sections shows that plastic deformation around the indentation is partly accommodated by the closing of the pores within the multilayers. This densification process reduces the amount of pileup formed below that predicted by finite element simulations. Experimental results show that the pileup is formed by an increase of the titanium layer thickness near the edges of the indentation. The thickness increase is largest near the film/substrate interface and decreases toward the surface of the multilayered film. The amount of normal compression near the center of the indenter is characterized, and it is demonstrated that the deformation becomes more nonuniform with increasing indentation depth.

The plastic displacements around Knoop indentations made in hard titanium/aluminum multilayered films on soft aluminum alloy substrates have been studied. Indentations were cross-sectioned and imaged using focused-ion-beam (FIB) milling and high-resolution scanning electron microscopy (SEM), respectively. The FIB milling method has the advantage of removing material in a localized region without producing mechanical damage to the specimen. The micrographs of the cross-sectioned indentations indicate that most of the plastic deformation around the indentation is dominated by the soft aluminum substrate. There is a very small change in the multilayered film thickness around the indentation—less than 10%. The plastic deformation of the thin film resembles a membrane being deflected by a localized pressure gradient across the membrane. Stress-induced voids are also observed in the multilayered film, especially in the area around the indentation apex. The density and the size of the voids increase with indentation depth. Indentation sink-in effects are observed in all of the indentations inspected. Based on the experimental results, the amount of sink-in of the hard film–soft substrate composite is larger than the bulk substrate and film alone. This is confirmed by the finite element analyses conducted in this work.

A simple superposition solution for a point-loaded elastic plate on a soft substrate is proposed. The solution considers a “drumhead” being elastically bent into a compliant substrate that is viscoelastic-plastic. With simplifying assumptions it is found that the drumhead and substrate support loads proportional to δ1/2 and δ3/2, respectively, where δ is the vertical point displacement. At fixed displacement, relaxation proceeds at high loads, but if sufficiently unloaded, recovery or increased load results with time. Qualitative verification of the time-dependent drumhead solution is shown by relaxation and recovery data on polycarbonate covered by polysiloxane, composite or diamondlike carbon (DLC) coatings, and films.

We have used the interfacial force microscope to perform nanoindentations on Au single-crystal surfaces. We have observed two distinct regimes of plastic deformation, which are distinguished by the magnitude of discontinuities in load relaxation. At lower stresses, relaxation occurs in small deviations from elastic behavior, while at the higher stresses they take the form of large load drops, often resulting in complete relaxation of the applied load. These major events create a relatively wide plastic zone that subsequently deepens more rapidly than it widens. We discuss these findings in terms of contrasting models of dislocation processes in the two regimes.

In a nanometer order nanoindentation test, roundness or truncation of the indenter tip cannot be avoided. In this paper, we have analyzed the indentation problem of a rounded triangular indentation into a layered elastic half-space by a finite element analysis and then established a method to estimate the intrinsic elastic modulus of the film from the nanoindentation data. The method was applied to analyze the nanoindentation data of a less-than-10 nm penetration depth on a 10 nm thick diamondlike carbon film deposited on a 50 nm thick magnetic layer.

This paper presents a large-scale atomic resolution simulation of nanoindentation into a thin aluminum film using the recently introduced quasicontinuum method. The purpose of the simulation is to study the initial stages of plastic deformation under the action of an indenter. Two different crystallographic orientations of the film and two different indenter geometries (a rectangular prism and a cylinder) are studied. We obtain both macroscopic load versus indentation depth curves, as well as microscopic quantities, such as the Peierls stress and density of geometrically necessary dislocations beneath the indenter. In addition, we obtain detailed information regarding the atomistic mechanisms responsible for the macroscopic curves. A strong dependence on geometry and orientation is observed. Two different microscopic mechanisms are observed to accommodate the applied loading: (i) nucleation and subsequent propagation into the bulk of edge dislocation dipoles and (ii) deformation twinning.

A new method has been developed to achieve a better understanding of submicron indent-induced plastic deformation. This method combines numerical modeling and various experimental data and techniques. Three-dimensional discrete dislocation dynamics simulation and the finite element method (FEM) were used to model the experimental conditions associated with nanoindentation testing in fcc crystals. Transmission electron microscopy (TEM) observations of the indent-induced plastic volume and analysis of the experimental loading curve help in defining a complete set of dislocation nucleation rules, including the shape of the nucleated loops and the corresponding macroscopic loading. A validation of the model is performed through direct comparisons between a simulation and experiments for a nanoindentation test on a [001] copper single crystal up to 50 nm deep.

Variation of hardness with penetration in nanoindentation of a rough surface is a compound effect of variation in asperity geometry with penetration, designated geometric effect, and genuine property gradients with depth as may exist in a near-surface zone. We simulate indentation of a rough surface numerically to elucidate the geometric effects and validate it by some model “macro” experiments. Finally, we formulate a general framework to deconvolute genuine property variation by normalizing the measured hardness with the geometric effect.

Two experiments that probe the nature of the rapid transition from elastic to plastic deformation are described. The load, and therefore stress, at which this yield point occurs is shown to be relatively independent of temperature in an iron alloy. When stresses lower than those required to generate a yield point during loading are applied for times between seconds and minutes, yielding occurs while the sample is under an applied stress. The time to generate a yield point increases as the applied stress is decreased. The possibilities of dislocation glide loop nucleation, double kink nucleation, and dislocation breakaway from pinning points are examined. Only glide loop nucleation appears to match the experimental observations. Criteria based on the stress-volume requirements of glide loop nucleation and the stress field underneath an indenter are presented which qualitatively describe the experimental data.

The current method of analysis for hardness measurements by indentation is examined. Although the method is based on Sneddon's solution for an elastic stress field within a homogeneous half space indented by an elastically deformable indenter, it implicitly assumes a fixed indenter geometry. Therefore, if indentations are made on materials whose hardness or elastic modulus are close to those of the indenter, this method underestimates the contact area and, thus, overestimates the hardness and modulus values of the indented materials. A new method, based on the Hertz contact theory, is proposed that accounts for the elastic deformation of the indenter and provides a simple way to calculate the tip radius. The restrictions of this method are also indicated and discussed. Finally, the hardness and modulus for two recently developed films are measured by this method, and the results are compared with published finite element method (FEM) results.

The continuously recording indentation responses of a number of coated systems, mainly thin (<10 μm) hard nitride coatings on stainless steels and a powder metallurgy tool steel, have been explored using nanoindentation with indenter displacements increasing progressively to values greater than the coating thickness. The resultant load-displacement data have been analyzed not only to produce conventional load-displacement (P-δ) plots but also to examine the relationship between P and δ2. Recent models have proposed that there should be a linear P-δ2 relationship for homogeneous systems and that such plots have the potential to reveal the load/displacement regimes in which either the coating or the substrate, or both, are dominant in controlling the overall behavior of the coated system. By utilizing point-to-point differentiation of the P-δ2 relationship, this paper extends this approach to confirm not only that these different regimes of behavior may be readily experimentally identified in this way, but also that further details, such as the propagation of cracks, may be recognized. Our analysis also provides a valuable experimental link to models describing the near-surface deformation behavior of coated systems.

Methods for analyzing nanoindentation load-displacement data to determine hardness and elastic modulus are based on analytical solutions for the indentation of an elastic half-space by rigid axisymmetric indenters. Careful examination of Sneddon's solution for indentation by a rigid cone reveals several largely ignored features that have important implications for nanoindentation property measurement. Finite element and analytical results are presented that show corrections to Sneddon's equations are needed if accurate results are to be obtained. Without the corrections, the equations underestimate the load and contact stiffness in a manner that leads to errors in the measured hardness and modulus, with the magnitudes of the errors depending on the angle of the indenter and Poisson's ratio of the half-space. First order corrections are derived, and general implications for the interpretation of nanoindentation data are discussed.

In this study we combined nanoscratch testing with a multilayer sapphire and aluminum nitride single-substrate system to determine the effects of interface composition and structure on susceptibility to fracture of hard, thin tantalum nitride films. Nanoindentation tests showed that the elastic moduli of the tantalum nitride and aluminum nitride films, as well as the sapphire substrate, were essentially equal at 400 GPa. On both portions of the substrate, these tests also showed that near surface hardness was near 35 GPa. Nanoscratch tests triggered long blisters and circular spalls on both the sapphire and aluminum nitride portions of the substrate. The blisters showed that the tantalum nitride film was subjected to a compressive residual stress of −6.7 GPa. The spalls showed that failure occurred along the tantalum nitride film-substrate interface regardless of substrate composition. Most importantly, the blisters and spalls showed that the mode I componentof the fracture energies was essentially equal on both substrate materials at a value near 3.1 J/m2. These energies are on the order of the energies for metallic bonding.

Nanoindentations using a Berkovich diamond indenter have been made on 1, 2, and 5 μm thick 99.99% purity polycrystalline aluminum films thermally evaporated in vacuum on to 2 mm thick R-cut polished sapphire flats. The projected contact areas of the residual indentations were estimated from the unloading load-displacement curves, and some of the indentations were imaged with an atomic force microscope (AFM). It was found that a large majority of indents showed material pileup, and the projected areas of these indents, as measured with the AFM, were up to 50% greater than those calculated from the unloading curves. This discrepancy between the calculated and directly measured indentation areas has a strong influence on the derived values of Young's modulus and hardness of the aluminum films. Using a new analytical model, Young's modulus of the aluminum films has been determined to be in the range of 50–70 GPa, independent of the relative indentation depth. The composite nanohardness of the 1 and 2 μm thick films was found to have a load-independent value of 1 GPa, whereas the composite nanohardness of the 5 μm film decreased from 1 to 0.7 Gpa with increasing indenter penetration. Finally, it has been suggested that in order to improve the accuracy with which the mechanical properties of thin films or bulk specimens can be determined by nanoindentation techniques, the projected contact areas should be measured by direct methods, such as atomic force microscopy.

Micro/nanomechanical and tribological characterization of ultrathin amorphous carbon coatings, deposited by filtered cathodic arc (FCA), direct ion beam (IB), electron cyclotron resonance plasma chemical vapor deposition (ECR-CVD), and sputter (SP) deposition processes on Si substrate have been conducted using a nanoindenter with a nanoscratch attachment and an accelerated ball-on-flat tribometer. Coating thicknesses of 20, 10, 5 nm and, for the first time, 3.5 nm coatings have been investigated. It was found the FCA coating exhibits the highest hardness and elastic modulus, followed by the ECR-CVD, IB, and SP coatings. In general, the thicker coatings exhibited better scratch/wear performance than the thinner coatings due to their better load-carrying capacity as compared to the thinner coatings. At 20 nm, the FCA and ECR-CVD coatings show the best scratch and wear resistance, while the IB and ECR-CVD coatings show the best scratch and wear resistance at 10 nm. Five nanometer thick coatings show reasonable scratch and wear resistance, while 3.5 nm thick coatings show extremely low load-carrying capacity and poor scratch and wear resistance. It appears that the 3.5 nm coatings studied are unfeasible for scratch and wear resistance applications as of now.

Details of microindentation of silicon, such as the semiconductor-to-metal transformation, which takes place on loading, have been examined using spherical indenters. Various forms of silicon are studied, including heavily boron-doped wafers and silicon damaged and amorphized by ion implantation as well as material containing dislocations. Results indicate that only silicon, which contains high concentrations of point defects or is amorphous, exhibits mechanical properties that differ significantly from undoped, defect-free crystal. Amorphous silicon exhibits plastic flow under low indentation pressures and does not appear to undergo phase transformation on loading and unloading. Indentation of compound semiconductors is also studied and the load/unload behavior at room temperature is quite different from that of silicon. Both gallium arsenide and indium phosphide, for example, undergo slip-induced plasticity above a critical load.

A knowledge of the formation and rupture mechanisms for agglomerates is essential when seeking to model equipment designed to produce and process such materials. In the work described here, nanoindentation of “two-dimensional” agglomerate films, basically particulate coatings, was carried out to establish a means of identifying the generic breakage mechanisms for agglomerates. Selected applied load and penetration depth data in the range (0.02 mN and 700 nm, respectively) are provided as a function of the loading time during continuous loading for a model system composed rather of monodispersed colloidal silica particles (20–24 nm diameter) bound with a poly(methyl methacrylate) at 5 vol%. It is argued that these data enable the sequence of binder bridge failures to be observed, thus giving an indication of the breakage mechanism of the agglomerate and also the strength of the individual junctions. These data are also incorporated into a mechanical model that describes the rupture and deformation behavior of these planar agglomerate systems.

Subsolidus equilibria in air in the La2O3–Ga2O3–NiO system were studied with the aim of obtaining information on possible interactions between a LaGaO3-based solid electrolyte and NiO during preparation of the anode in solid oxide fuel cells (SOFC). No ternary compound was found. The tie lines are between La4Ga2O7 and La2NiO4, LaGaO3 and La2NiO4, LaGaO3 and NiO, and LaGaO3 and NiGa2O4.

Pulsed laser deposition has been used to make two sets of lead magnesium niobate thin films grown on single-crystal h100j MgO substrates. One set was fabricated using a perovskite-rich target while the other used a pyrochlore-rich target. It was found that the growth conditions required to produce almost 100% perovskite Pb(Mg1/3Nb2/3)O3 (PMN) films were largely independent of target crystallography. Films were characterized crystallographically using x-ray diffraction and plan view transmission electron microscopy, chemically using energy dispersive x-ray analysis, and electrically by fabricating a planar thin film capacitor structure and monitoring capacitance as a function of temperature. All characterization techniques indicated that perovskite PMN thin films had been successfully fabricated.

Carbon nitride films have been deposited using Penning-type opposed target dc reactive sputtering. These films show large (>10 μm2) continuous areas of nanocrystalline material in an amorphous matrix. Electron diffraction shows the nanocrystalline areas to have crystallography consistent with the β–C3N4 phase. Film chemistry analysis using Rutherford backscattering and Raman spectroscopy indicates that only carbon, nitrogen, and trace levels of hydrogen are present. Given this film chemistry and the fit of diffraction data to that predicted for the β–C3N4 structure, it seems likely that the sputtering parameters used have, indeed, produced continuous regions of the elusive β–C3N4 phase.