Showing papers on "Indentation published in 2015"

Spherical nanoindentation stress–strain curves

Abstract: Although indentation experiments have long been used to measure the hardness and Young's modulus, the utility of this technique in analyzing the complete elastic–plastic response of materials under contact loading has only been realized in the past few years – mostly due to recent advances in testing equipment and analysis protocols. This paper provides a timely review of the recent progress made in this respect in extracting meaningful indentation stress–strain curves from the raw datasets measured in instrumented spherical nanoindentation experiments. These indentation stress–strain curves have produced highly reliable estimates of the indentation modulus and the indentation yield strength in the sample, as well as certain aspects of their post-yield behavior, and have been critically validated through numerical simulations using finite element models as well as direct in situ scanning electron microscopy (SEM) measurements on micro-pillars. Much of this recent progress was made possible through the introduction of a new measure of indentation strain and the development of new protocols to locate the effective zero-point of initial contact between the indenter and the sample in the measured datasets. This has led to an important key advance in this field where it is now possible to reliably identify and analyze the initial loading segment in the indentation experiments. Major advances have also been made in correlating the local mechanical response measured in nanoindentation with the local measurements of structure at the indentation site using complementary techniques. For example, it has been shown that the combined use of Orientation Imaging Microscopy (OIM, using Electron BackScattered Diffraction (EBSD)) and nanoindentation on polycrystalline metallic samples can yield important information on the orientation dependence of indentation yield stress, which can in turn be used to estimate percentage increase in the local slip resistance in deformed samples. The same methods have been used successfully to probe the intrinsic role of grain boundaries in the overall mechanical deformation of the sample. More recently, these protocols have been extended to characterize local mechanical property changes in the damaged layers in ion-irradiated metals. Similarly, the combined use of Raman spectroscopy and nanoindentation on samples of mouse bone has revealed tissue-level correlations between the mineral content at the indentation site and the associated local mechanical properties. The new protocols have also provided several new insights into the buckling response in dense carbon nanotube (CNT) brushes. These and other recent successful applications of nanoindentation are expected to provide the critically needed information for the maturation of physics-based multiscale models for the mechanical behavior of most advanced materials. In this paper, we review these latest developments and identify the future challenges that lie ahead.

A novel pillar indentation splitting test for measuring fracture toughness of thin ceramic coatings

Abstract: The fracture toughness of thin ceramic films is an important material property that plays a role in determining the in-service mechanical performance and adhesion of this important class of engineering materials. Unfortunately, measurement of thin film fracture toughness is affected by influences from the substrate and the large residual stresses that can exist in the films. In this paper, we explore a promising new technique that potentially overcomes these issues based on nanoindentation testing of micro-pillars produced by focused ion beam milling of the films. By making the pillar diameter approximately equal to its length, the residual stress in the upper portion of the pillar is almost fully relaxed, and when indented with a sharp Berkovich indenter, the pillars fracture by splitting at reproducible loads that are readily quantified by a sudden displacement excursion in the load displacement behaviour. Cohesive finite element simulations are used for analysis and development of a simple relationship...

Comparative simulation study of the structure of the plastic zone produced by nanoindentation

Abstract: Using molecular-dynamics simulation, we study nanoindentation in fcc (Cu and Al) and bcc (Fe and Ta) metals by a spherical indenter and investigate the size of the plastic zone generated. We find that while it does not strongly depend on crystal structure, surface orientation, and indentation parameters, the extent of the plastic zone is substantially larger before the retraction of the indenter. After retraction, the results are in good agreement with available published data. Plasticity develops by the generation, propagation and reaction of dislocations; they fall into two groups, those that adhere to the indentation pit, and those that have been emitted either into the substrate interior or glide along the surface. The total length of the dislocation network generated roughly follows available geometrical estimates; results for individual surface orientations may, however, differ quite strongly. The radial distribution of the dislocations attached to the indentation pit is computed; as a rule it shows a maximum at some depth below the indentation pit.

Hardness and toughness of sodium borosilicate glasses via Vickers's indentations

Abstract: This study investigates the mechanical response of sodium borosilicate (SBN) glasses as a function of their chemical composition Vickers's indentation tests provide an estimate of the material hardness ( H V ) and indentation fracture toughness ( K C VIF ) plus the amount of densification/shear flow processes Sodium content significantly impacts the glass behavior under a sharp indenter Low sodium glasses maintain high connected networks and low Poisson's ratios ( ν ) This entails significant densification processes during deformation Conversely, glasses with high sodium content, ie large ν , partake in a more depolymerized network favoring deformation by shear flow As a consequence, indentation patterns differ depending on the processes occurring Densification processes appear to hinder the formation of half-penny median–radial cracks Increasing ν favors shear flow and residual stresses enhance the development of half-penny median–radial cracks Hence, K C VIF decreases linearly with ν

Driving force for indentation cracking in glass: composition, pressure and temperature dependence

Abstract: The occurrence of damage at the surface of glass parts caused by sharp contact loading is a major issue for glass makers, suppliers and end-users. Yet, it is still a poorly understood problem from the viewpoints both of glass science and solid mechanics. Different microcracking patterns are observed at indentation sites depending on the glass composition and indentation cracks may form during both the loading and the unloading stages. Besides, we do not know much about the fracture toughness of glass and its composition dependence, so that setting a criterion for crack initiation and predicting the extent of the damage yet remain out of reach. In this study, by comparison of the behaviour of glasses from very different chemical systems and by identifying experimentally the individual contributions of the different rheological processes leading to the formation of the imprint—namely elasticity, densification and shear flow—we obtain a fairly straightforward prediction of the type and extent of the microcracks which will most likely form, depending on the physical properties of the glass. Finally, some guidelines to reduce the driving force for microcracking are proposed in the light of the effects of composition, temperature and pressure, and the areas for further research are briefly discussed.

Dynamic nanoindentation testing for studying thermally activated processes from single to nanocrystalline metals

Abstract: Nanoindentation experiments are widely used for assessing the local mechanical properties of materials. In recent years some new exciting developments have been performed for also analyzing thermally activated processes using indentation based techniques. This paper focuses on how thermally activated dislocation mechanisms can be assessed by indentation strain rate jump as well as creep testing. Therefore, a small overview is given on thermally activated dislocation mechanism and how indentation data from pointed indenters can be interpreted in terms of uniaxial macroscopic testing. This requires the use of the indentation strain rate as introduced by Lucas and Oliver as well as the concepts of Taylor hardening together with Johnson expanding cavity model. These concepts are then translated to nanoindentation strain rate jump tests as well as nanoindentation long term creep test, where the control of the indenter tip movement as well as the determination of the contact are quite important for reliable data. It is furthermore discussed, that for a steady state hardness test, the interpretation of the hardness data is straightforward and comparable to macroscopic testing. For other conditions where size effects play a major role, hardness data need to be interpreted with consideration for the microstructural length scale with respect to the contact radius. Finally strain rate jump testing and long term creep testings are used to assess different thermally activated mechanisms in single to nanocrystalline metals such as: Motion of dislocation kink pairs in bcc sx-W, Grain boundary processes in nc-Ni and ufg-Al, and the Portevin-le Chatelier effect in ufg-AA6014.

In situ Nanoindentation Study of Plastic Co-deformation in Al-TiN Nanocomposites

Abstract: We performed in situ indentation in a transmission electron microscope on Al-TiN multilayers with individual layer thicknesses of 50 nm, 5 nm and 2.7 nm to explore the effect of length scales on the plastic co-deformability of a metal and a ceramic. At 50 nm, plasticity was confined to the Al layers with easy initiation of cracks in the TiN layers. At 5 nm and below, cracking in TiN was suppressed and post mortem measurements indicated a reduction in layer thickness in both layers. The results demonstrate the profound size effect in enhancing plastic co-deformability in nanoscale metal-ceramic multilayers.

Elastic coupling between layers in two-dimensional materials

Abstract: Two-dimensional materials, such as graphene and MoS2, are films of a few atomic layers in thickness with strong in-plane bonds and weak interactions between the layers. The in-plane elasticity has been widely studied in bending experiments where a suspended film is deformed substantially; however, little is known about the films' elastic modulus perpendicular to the planes, as the measurement of the out-of-plane elasticity of supported 2D films requires indentation depths smaller than the films' interlayer distance. Here, we report on sub-angstrom-resolution indentation measurements of the perpendicular-to-the-plane elasticity of 2D materials. Our indentation data, combined with semi-analytical models and density functional theory, are then used to study the perpendicular elasticity of few-layer-thick graphene and graphene oxide films. We find that the perpendicular Young's modulus of graphene oxide films reaches a maximum when one complete water layer is intercalated between the graphitic planes. This non-destructive methodology can map interlayer coupling and intercalation in 2D films.

Large scale atomistic simulation of size effects during nanoindentation: Dislocation length and hardness

Abstract: The present paper studies the size effects during nanoindentation in Ni thin films using large scale atomistic simulation. The main focus of this paper is to evaluate the available theoretical models of size effects during nanoindentation using atomistic simulation. First, the dislocation nucleation and evolution in the simulated samples are studied. In the next step, the plastic zone size is obtained for each sample at several indentation depths incorporating the dislocation visualization. The results show that the plastic zone size divided by the contact radius is not a constant factor and varies as the indentation depth changes. The total length of dislocations located in the plastic zone is measured in the simulated samples and compared to that of the corresponding theoretical models. The results obtained from the atomistic simulation verify the theoretical predictions of the dislocation length. Next, the variation of hardness obtained directly from the molecular dynamics outputs, which is the indentation force over the contact area, is studied. In the case of conical indenter, the theoretical predictions of hardness have been verified using both experiments and simulations, and the current simulation shows the same trend, i.e. the hardness decreases as the indentation depth increases. However, in the cases of flat indenters, the theoretical models have not been validated using any experiments or simulations. Here, in the cases of flat indenters, the simulation results verify the theoretical predictions of hardness. They show that the hardness increases as the indentation depth increases. The variation of dislocation density as a function of indentation depth is then studied. In the case of nanoindentation experiment, the validity of Taylor hardening model, i.e. the relation between the hardening and dislocation density, which has not been previously studied with full atomistic details, is investigated. Accordingly, the hardness obtained directly from the simulation is compared with the one calculated from the dislocation density and theoretical size effects models.

Measuring the mechanical properties of plant cells by combining micro-indentation with osmotic treatments

Abstract: Growth in plants results from the interaction between genetic and signalling networks and the mechanical properties of cells and tissues. There has been a recent resurgence in research directed at understanding the mechanical aspects of growth, and their feedback on genetic regulation. This has been driven in part by the development of new micro-indentation techniques to measure the mechanical properties of plant cells in vivo. However, the interpretation of indentation experiments remains a challenge, since the force measures results from a combination of turgor pressure, cell wall stiffness, and cell and indenter geometry. In order to interpret the measurements, an accurate mechanical model of the experiment is required. Here, we used a plant cell system with a simple geometry, Nicotiana tabacum Bright Yellow-2 (BY-2) cells, to examine the sensitivity of micro-indentation to a variety of mechanical and experimental parameters. Using a finite-element mechanical model, we found that, for indentations of a few microns on turgid cells, the measurements were mostly sensitive to turgor pressure and the radius of the cell, and not to the exact indenter shape or elastic properties of the cell wall. By complementing indentation experiments with osmotic experiments to measure the elastic strain in turgid cells, we could fit the model to both turgor pressure and cell wall elasticity. This allowed us to interpret apparent stiffness values in terms of meaningful physical parameters that are relevant for morphogenesis.

The compelling case for indentation as a functional exploratory and characterization tool

Abstract: The utility of indentation testing for characterizing a wide range of mechanical properties of brittle materials is highlighted in light of recent articles questioning its validity, specifically in relation to the measurement of toughness. Contrary to assertion by some critics, indentation fracture theory is fundamentally founded in Griffith–Irwin fracture mechanics, based on model crack systems evolving within inhomogeneous but well-documented elastic and elastic–plastic contact stress fields. Notwithstanding some numerical uncertainty in associated stress intensity factor relations, the technique remains an unrivalled quick, convenient and economical means for comparative, site-specific toughness evaluation. Most importantly, indentation patterns are unique fingerprints of mechanical behavior and thereby afford a powerful functional tool for exploring the richness of material diversity. At the same time, it is cautioned that unconditional usage without due attention to the conformation of the indentation patterns can lead to overstated toughness values. Limitations of an alternative, more engineering approach to fracture evaluation, that of propagating a precrack through a “standard” machined specimen, are also outlined. Misconceptions in the critical literature concerning the fundamental nature of crack equilibrium and stability within contact and other inhomogeneous stress fields are discussed.

Indentation of Ultrathin Elastic Films and the Emergence of Asymptotic Isometry

Abstract: We study the indentation of a thin elastic film floating at the surface of a liquid. We focus on the onset of radial wrinkles at a threshold indentation depth and the evolution of the wrinkle pattern as indentation progresses far beyond this threshold. Comparison between experiments on thin polymer films and theoretical calculations shows that the system very quickly reaches the far from threshold regime, in which wrinkles lead to the relaxation of azimuthal compression. Furthermore, when the indentation depth is sufficiently large that the wrinkles cover most of the film, we recognize a novel mechanical response in which the work of indentation is transmitted almost solely to the liquid, rather than to the floating film. We attribute this unique response to a nontrivial isometry attained by the deformed film, and we discuss the scaling laws and the relevance of similar isometries to other systems in which a confined sheet is subjected to weak tensile loads.

Microstructure-dependent deformation behaviour of bcc-metals – indentation size effect and strain rate sensitivity

Abstract: In this work, the indentation size effect and the influence of the microstructure on the time-dependent deformation behaviour of body-centred cubic (bcc) metals are studied by performing nanoindentation strain rate jump tests at room temperature. During these experiments, the strain rate is abruptly changed, and from the resulting hardness difference the local strain rate sensitivity has been derived. Single-crystalline materials exhibit a strong indentation size effect; ultrafine-grained metals have nearly a depth-independent hardness. Tungsten as a bcc metal shows the opposite behaviour as generally found for face-centered cubic metals. While for UFG-W only slightly enhanced strain rate sensitivity was observed, SX-W exhibits a pronounced influence of the strain rate on the resulting hardness at room temperature. This is due to the effects of the high lattice friction of bcc metals at low temperatures, where the thermally activated motion of screw dislocations is the dominating deformation mechanisms, w...

Indentation of a rigid sphere into an elastic substrate with surface tension and adhesion.

Abstract: The surface tension of compliant materials such as gels provides resistance to deformation in addition to and sometimes surpassing that owing to elasticity. This paper studies how surface tension c...

Investigation of the response to low velocity impact and quasi-static indentation loading of particle-toughened carbon-fibre composite materials

Abstract: This work investigates damage caused by low velocity impact and quasi-static indentation loading in four different particle-toughened composite systems, and one untoughened system. For impact tests, a range of energies were used between 25 and 50 J. For QSI, coupons were interrupted at increasing loading point displacement levels from 2 to 5 mm to allow for monitoring of damage initiation and propagation. In both loading cases, non-destructive inspection techniques were used, consisting of ultrasonic C-scan and X-ray micro-focus computed tomography. These techniques are complemented with instrumentation to capture force–displacement data, whereby load-drops are associated with observed damage modes. Key results from this work highlight particular issues regarding strain-rate sensitivity of delamination development and an earlier onset of fibre fracture associated with particle-toughened systems. These issues, in addition to observations on the role of micro-scale events on damage morphology, are discussed with a focus on material development and material testing practices.

On the failure load and mechanism of polycrystalline graphene by nanoindentation

Abstract: Nanoindentation has been recently used to measure the mechanical properties of polycrystalline graphene. However, the measured failure loads are found to be scattered widely and vary from lab to lab. We perform molecular dynamics simulations of nanoindentation on polycrystalline graphene at different sites including grain center, grain boundary (GB), GB triple junction, and holes. Depending on the relative position between the indenter tip and defects, significant scattering in failure load is observed. This scattering is found to arise from a combination of the non-uniform stress state, varied and weakened strengths of different defects, and the relative location between the indenter tip and the defects in polycrystalline graphene. Consequently, the failure behavior of polycrystalline graphene by nanoindentation is critically dependent on the indentation site, and is thus distinct from uniaxial tensile loading. Our work highlights the importance of the interaction between the indentation tip and defects, and the need to explicitly consider the defect characteristics at and near the indentation site in polycrystalline graphene during nanoindentation.

Analysis of the mechanical response of biomimetic materials with highly oriented microstructures through 3D printing, mechanical testing and modeling.

Abstract: Many biomineralized organisms have evolved highly oriented nanostructures to perform specific functions. One key example is the abrasion-resistant rod-like microstructure found in the radular teeth of Chitons (Cryptochiton stelleri), a large mollusk. The teeth consist of a soft core and a hard shell that is abrasion resistant under extreme mechanical loads with which they are subjected during the scraping process. Such remarkable mechanical properties are achieved through a hierarchical arrangement of nanostructured magnetite rods surrounded with α-chitin. We present a combined biomimetic approach in which designs were analyzed with additive manufacturing, experiments, analytical and computational models to gain insights into the abrasion resistance and toughness of rod-like microstructures. Staggered configurations of hard hexagonal rods surrounded by thin weak interfacial material were printed, and mechanically characterized with a cube-corner indenter. Experimental results demonstrate a higher contact resistance and stiffness for the staggered alignments compared to randomly distributed fibrous materials. Moreover, we reveal an optimal rod aspect ratio that lead to an increase in the site-specific properties measured by indentation. Anisotropy has a significant effect (up to 50%) on the Young's modulus in directions parallel and perpendicular to the longitudinal axis of the rods, and 30% on hardness and fracture toughness. Optical microscopy suggests that energy is dissipated in the form of median cracks when the load is parallel to the rods and lateral cracks when the load is perpendicular to the rods. Computational models suggest that inelastic deformation of the rods at early stages of indentation can vary the resistance to penetration. As such, we found that the mechanical behavior of the system is influenced by interfacial shear strain which influences the lateral load transfer and therefore the spread of damage. This new methodology can help to elucidate the evolutionary designs of biomineralized microstructures and understand the tolerance to fracture and damage of chiton radular teeth.

High temperature indentation of helium-implanted tungsten

Abstract: Nanoindentation has been performed on tungsten, unimplanted and helium-implanted to ~600 appm, at temperatures up to 750 °C. The hardening effect of the damage was 0.90 GPa at 50 °C, but is negligible above 450 °C. The hardness value at a given temperature did not change on re-testing after heating to 750 °C. This suggests that the helium is trapped in small vacancy complexes that are stable to at least 750 °C, but which can be bypassed due to increased dislocation mobility (cross slip or climb) above 450 °C.