Sharp Indenter Tip Research Articles

Lower hardness than strength: The auxetic composite microstructure of limpet tooth.

The limpet tooth is widely recognized as nature's strongest material, with reported strength values up to 6.5 GPa. Recently, microscale auxeticity has been discovered in the leading part of the tooth, providing a possible explanation for this extreme strength. Utilizing micromechanical experiments, we find hardness values in nanoindentation that are lower than the respective strength observed in micropillar compression tests. Using micromechanical modeling, we show that this unique behavior is a result of local tensile strains during indentation, originating from the microscale auxeticity. As the limpet tooth lacks ductility, these tensile strains lead to microdamage in the auxetic regions of the microstructure. Consequently, indentation with a sharp indenter always probes a damaged version of the material, explaining the lower hardness and modulus values gained from nanoindentation. Micropillar tests were found to be mostly insensitive to such microdamage due to the lower applied strain and are therefore the suggested method for characterizing auxetic nanocomposites. STATEMENT OF SIGNIFICANCE: This work explores the micromechanical properties of limpet teeth, nature's strongest biomaterial, using micropillar compression testing and nanoindentation. The limpet tooth microstructure consists of ceramic nanorods embedded in a matrix of amorphous SiO2 and arranged in a pattern that leads to local auxetic behavior. We report lower values for nanoindentation hardness than for compressive strength, a unique behavior usually not achievable in conventional materials. Utilizing micromechanical finite element simulations, we identify the reason for this behavior to be microdamage formation resultant of the auxetic behavior, sharp indenter tip and lack of ductility of the limpet tooth microstructure. This formation of microdamage is not expected in micropillar compression tests due to lower locally imposed strain.

High-Temperature Dynamic Mechanical Properties Characterization of Polymer Coatings via Nanoindentation

Abstract Polymer coatings are widely used in industrial applications. The mechanical properties of these polymer coatings are known to vary with temperature and deformation rate. The characterization of the dynamic mechanical properties of these coatings at high temperatures via traditional uniaxial testing is challenging often due to their brittleness and small size. In this paper, the mechanical properties of polymer coatings are reported with emphasis on their dynamic mechanical properties at temperatures up to 280 °C characterized by a dynamic nanoindentation technique with a sharp indenter tip. Nanoindentation was used to characterize the mechanical response with emphasis on dynamic mechanical properties of polymer coatings enclosed in a high-temperature stage. To verify the method, the viscoelastic properties of a reference polyethylene terephthalate polyester film were also characterized by uniaxial cyclic tensile testing which exhibited an excellent agreement with the proposed technique. The proposed nanoindentation method can be applied to other polymer coatings and thin films that are used in applications at high temperatures.

Assessment of small-scale deformation characteristics and stress-strain behavior of NiTi based shape memory alloy using nanoindentation

The study is focused to understand the micro-mechanisms that govern the deformation behavior of a Ni-rich NiTi alloy at the sub-micron scale. This alloy undergoes reversible stress induced martensitic transformation leading to pseudoelasticity. Correspondingly, significant strain recoverability is noted. In this investigation, nanoindentation is utilized as the primary experimental tool. Various parameters including the indenter tip configuration, size and applied load levels are varied systematically. It is observed that compared to the most commonly used sharp Berkovich indenter tip, blunt spherical tip imposes reduced amount of strain and strain-gradient within the indentation volume. This opens up the window for systematically varying the sequential deformation modes in NiTi. Further in-depth analysis revealed that optimum combination of indenter tip configuration, size and applied load level is prerequisite to appreciate the pseudoelastic mechanism in NiTi. Most importantly, a tailored and simplified protocol is formulated for converting nanoindentation load-displacement response to corresponding indentation-stress-strain behavior for pseudoelastic alloy. These indentation-stress-strain curves featuring the signature deformation characteristics of NiTi alloy are realized without utilizing any specialized experimental modes. In a nutshell, this study highlights the importance of choosing adequate nanoindentation parameters for assessing the functional characteristics of pseudoelastic NiTi system at sub-micron scale. Accordingly, overall localized deformation behavior of this unique alloy is investigated.

Indentation-Induced Structural Changes in Vitreous Silica Probed by in-situ Small-Angle X-Ray Scattering

The transient (or permanent) structural modifications which occur during local deformation of oxide glasses are typically studied on the basis of short-range data, for example, obtained through vibrational spectroscopy. This is in contrast to macroscopic observations, where variations in material density can usually not be explained using next-neighbor correlations alone. Recent experiments employing low-frequency Raman spectroscopy have pointed-out this issue, emphasizing that the deformation behavior of glasses is mediated through structural heterogeneity and drawing an analogy to granular media. Here, we provide additional support to this understanding, using an alternative experimental method. Structural modification of vitreous silica in the stress field of a sharp diamond indenter tip was monitored by in-situ small-angle X-ray scattering. The influenced zone during loading and after unloading was compared, demonstrating that changes in the position of the first sharp diffraction peak (FSDP) directly in the center of the indent are of permanent character. On the other hand, variations in the amplitude of electron density fluctuations appear to fully recover after load release. The lateral extent of the modifications and their relaxation are related to the short- to intermediate-range structure and elastic heterogeneity pertinent to the glass network. With support from Finite Element Analysis, we suggest that different structural length scales govern shear and isotropic compaction in vitreous silica.

Assessment of Small-Scale Deformation Characteristics and Stress-Strain Behavior of NiTi Based Shape Memory Alloy Using Nanoindentation

The study is focused on appreciating the micro-mechanisms that govern the deformation behavior of a Ni-rich NiTi alloy at the sub-micron scale. This alloy undergoes reversible stress-induced-martensitic-transformation leading to pseudoelasticity. Correspondingly, significant strain recoverability is noted. In this investigation, nanoindentation is utilized as the primary experimental tool. Various parameters including the indenter tip configuration, size and applied load levels are varied systematically. It is observed that compared to the most commonly used sharp Berkovich indenter tip, blunt spherical tip imposes reduced amount of strain and strain-gradient within the indentation volume. This opens up the window for systematically varying the sequential deformation modes in NiTi. Further in-depth analysis revealed that optimum combination of indenter tip configuration, size and applied load level is prerequisite to appreciate the pseudoelastic mechanism in NiTi. Most importantly, a tailored and simplified protocol is formulated for converting nanoindentation load-displacement response to corresponding indentation-stress-strain behavior for pseudoelastic alloy. These indentation-stress-strain curves featuring the signature deformation characteristics of NiTi alloy are realized without utilizing any specialized experimental modes. In a nutshell, this study highlights the importance of choosing adequate nanoindentation parameters for assessing the functional characteristics of pseudoelastic NiTi system at sub-micron scale. Accordingly, overall localized deformation behavior of this unique alloy is appreciated.

In situ transmission electron microscopy deformation and mechanical responses of additively manufactured Ni-based superalloy

In situ nanodeformation by sharp indenter tip on nanopillars of various sizes was applied on an additively manufactured Ni-based alloy containing equiaxed grains and nano-features for the first time. In situ microscopy compression results showed more homogeneous deformation of the smaller nanopillars (compression mode) than the larger ones (indentation mode) due to their length and the contact area between the nanopillar and the indenter tip established during in situ deformation tests. Finite element modeling indicated a higher average stress level in smaller nanopillars. The local mechanical response of additively manufactured 718 was similar to a wrought 718 alloy.

Solitonic State in Microscopic Dynamic Failures

Onset of permanent deformation in crystalline materials under a sharp indenter tip is accompanied by nucleation and propagation of defects. By measuring the spatio-temporal strain field near the indenter tip during indentation tests, we demonstrate that the dynamic strain history at the moment of a displacement burst carries characteristics of the formation and interaction of local excitations, or solitons. We show that dynamic propagation of multiple solitons is followed by a short time interval where the propagating fronts can accelerate suddenly. As a result of such abrupt local accelerations, duration of the fast-slip phase of a failure event is shortened. Our results show that formation and annihilation of solitons mediate the microscopic fast weakening phase, during which extreme acceleration and collision of solitons lead to non-Newtonian behavior and Lorentz contraction, i.e., shortening of solitons’ characteristic length. The results open new horizons for understanding dynamic material response during failure and, more generally, complexity of earthquake sources.

Characterization of elastic-plastic coated material properties by indentation techniques using optimisation algorithms and finite element analysis

Determination of the material properties of coated thin films on substrates has always been complicated due to the influence of the substrate deformation on the thin film behaviour. In this study, indentation tests are used to continuously capture the indentation load, P, as a continuous function of the depth of penetration, h, into the indented specimen. Numerical optimisation schemes are used to extract elastic-plastic material properties of thin film coating materials from an indentation loading–unloading curve. Material parameters with non-linear isotropic hardening are determined by minimizing the least squares error (LSE) between target data and the results obtained from FE analysis of the indentation test. Lagrange linear interpolation polynomial (LLIP) and Cubic B-Spline approach are used for axisymmetric conical model and three-dimensional Berkovich model, respectively, to obtain the relationship between the applied load and penetration depth in the loading–unloading curve. This study also considers a global optimisation approach using a load–displacement curve based on a sharp indenter tip applied to HA coating on Ti–6Al–4 V substrate, Al2O3 coating on Al substrate and Cr coating on SS substrate. Additionally, in order to maintain FE analysis accuracy, multiple starting points are performed to obtain the correct material properties. The proposed optimisation algorithm is shown to achieve excellent convergence even when the initial guess values are much greater or less than the target values and hence is potentially considered for characterising intrinsic material properties of coated thin films on substrates that exhibit significant elastic-plastic deformation.

Comparison of test methods estimating the stiffness of ultrathin coatings

A key engineering parameter of thin coatings is their stiffness. Stiffness characterization of ultrathin coatings with a nanometer scale thickness is experimentally challenging. In this work, three feasible methods have been used to estimate the Young’s modulus of metal coatings on polymer films. The methods are: (1) nanoindentation, (2) strain-induced elastic buckling and (3) peak-force measurements integrated in atomic force microscopy. The samples were prepared by atomic layer deposition of TiO2 (6 and 20 nm thick) and mixed oxides of TiO2 and Al2O3 (4 and 20 nm thick). The differences in estimated Young’s modulus are interpreted in terms of the underlying assumptions and test conditions. Their specific advantages and drawbacks are also compared and discussed. In particular, the nanoindentation necessitates a sufficiently sharp indenter tip to make localized measurements dominated by the coating. The strain-induced elastic buckling method is simple in practice, but showed a large scatter due to variation in local coating thickness and irregular deformation patterns. The stiffness characterization using atomic force microscopy gave the most consistent results, due to a sharp tip with a radius comparable to the thinnest coating thickness. All methods gave a higher Young’s modulus for the TiO2 coating than for the mixed oxide coating, with a variation within one order of magnitude between the methods.

Indentation damage evaluation on metal-coated thin-films stacked structure

Abstract

Comparison of the Young’s moduli of polymers measured from nanoindentation and bending experiments

Spherical and conical nanoindentation experiments were performed for the same polymer specimens to compare Young’s moduli measured from the elastic loading and unloading curves, and bending experiments. Finite-element simulation was employed to ensure pure elastic deformation during spherical nanoindentation. The moduli measured from the elastic loading curves using Hertz’s contact law are very close to the bending moduli, because both measurements were conducted under the same elastic deformation. However, the moduli measured from the elastic unloading curves are up to 60% higher than the bending moduli owing to plastic deformation close to the sharp conical indenter tip.

On anomalous depth-dependency of the hardness of NiTi shape memory alloys in spherical nanoindentation

Abstract

Nanoscale Thermomechanics of Wear-Resilient Polymeric Bilayer Systems

We explore the effect of an ultrathin elastic coating to optimize the mechanical stability of an underlying polymer film for nanoscale applications. The coating consists of a several nanometer thin plasma-polymerized norbornene layer. Scanning probes are used to characterize the system in terms of shear-force-induced wear and thermally assisted indentation. The layer transforms a weakly performing polystyrene film into a highly wear-resistive system, ideal for high-density and low-power data storage applications. The result can be understood from the indentation characteristics with a hot and sharp indenter tip. The latter gives rise to a deformation mode in the fully plastic regime, enabling a simple interpretation of the results. The softening transition and the yield stress of the system on a microsecond time scale and a nanometer size scale were obtained. We show that the plastic deformation is governed by yielding in the polystyrene sublayer, which renders the overall system soft for plastic deformation. The ultrathin protection layer contributes as an elastic skin, which shields part of the temperature and pressure and enables the high wear resistance against lateral forces. Moreover, the method of probing polymers at microsecond and nanometer size scales opens up new opportunities for studying polymer physics in a largely unexplored regime. Thus, we find softening temperatures of more than 100 °C above the polystyrene glass transition, which implies that for the short interaction time scales the glassy state of the polymer is preserved up to this temperature.

Deformation of plastically compressible hardening-softening-hardening solids

Motivated by a model of the response of vertically aligned carbon nanotube (VACNT) pillars in uniaxial compression, we consider the deformation of a class of compressible elastic-viscoplastic solids with a hardeningsoftening-hardening variation of flow strength with plastic strain. In previous work (Hutchens et al. 2011) a constitutive relation was presented and used to model the response of VACNT pillars in axisymmetric compression. Subsequently, it was found that due to a programming error the constitutive relation presented in the paper (Hutchens et al. 2011) was not the one actually implemented. In particular, the plastic flow rule actually used did not satisfy plastic normality. Here, we present the constitutive formulation actually implemented in the previous work (Hutchens et al. 2011). Dynamic, finite deformation, finite element calculations are carried out for uniaxial compression, uniaxial tension and for indentation of a “half-space” by a conical indenter tip. A sequential buckling-like deformation mode is found in compression when there is plastic non-normality and hardeningsoftening-hardening. The same material characterization gives rise to a Luders band-like deformation mode in tension. When there is a deformation mode with a sharp front along mesh boundaries, the overall stress-strain response contains high frequency oscillations that are a mesh artifact. The responses of non-softening solids are also analyzed and their overall stress-strain behavior and deformation modes are compared with those of hardening-softening-hardening solids. We find that indentation with a sharp indenter tip gives a qualitatively equivalent response for hardening and hardening-softening-hardening solids.

Nanoindentation Behavior of Muscovite Subjected to Repeated Loading

A series of repeated loading nanoindentation experiments were performed on muscovite with a sharp indenter tip and loading direction normal to the basal plane, and the maximum load (Fmax⁡) was varied between 0.05 and 2.0 mN to examine the influences of load level on the modes of nanoscale deformation and the resulting estimation of hardness and elastic modulus. A critical maximum load, (Fmax⁡)crit, of about 0.25–0.5 mN marks the material’s completely different responses to repeated loading. If Fmax⁡<(Fmax⁡)crit, fully closed, completely reversible loading-unloading (L/U) hysteresis loops were observed with characteristic smooth, nonlinear curves, which can be attributed to the formation and annihilation of incipient kink bands. If Fmax⁡>(Fmax⁡)crit, dispersed L/U loops characterized by nonrecoverable deformation and randomly occurring pop-ins in the loading section of the loops were observed; moreover, it appears that pop-ins are the major cause for the dispersion of the L/U loops. For the latter case, after a few L/U cycles, pop-ins tend to disappear, and the L/U loops start to merge together, resulting in the shakedown of the repeated loading. A comparison of the unloading section of the loops indicates that the contact stiffness increases with the number of L/U cycles, or the mineral exhibits cyclic hardening behavior. The resulting influences on the hardness and elastic modulus are evaluated against those obtained by monotonic loading and further discussed in accordance with indentation size effects and underlying nanoscale deformation mechanisms at different load levels.

An analysis of nanoindentation in linearly elastic solids

The conventional method to extract elastic properties in the nanoindentation of linearly elastic solids relies primarily on Sneddon’s solution (1948). The underlying assumptions behind Sneddon’s derivation, namely, (1) an infinitely large incompressible specimen; (2) an infinitely sharp indenter tip, are generally violated in nanoindentation. As such, correction factors are commonly introduced to achieve accurate measurements. However, little is known regarding the relationship between the correction factors and how they affect the overall accuracy. This paper first proposes a criterion for the specimen’s geometry to comply with the first assumption, and modifies Sneddon’s elastic relation to account for the finite tip radius effect. The relationship between the finite tip radius and compressibility of the specimen is then examined and a composite correction factor that involves both factors, derived. The correction factor is found to be a function of indentation depth and a critical depth is derived beyond which, the arbitrary finite tip radius effect is insignificant. Techniques to identify the radius of curvature of the indenter and to decouple the elastic constants ( E and ν) for linear elastic materials are proposed. Finally, experimental results on nanoindentation of natural latex are reported and discussed in light of the proposed modified relation and techniques.

Wear behaviour of dental enamel at the nanoscale with a sharp and blunt indenter tip

Two different diamond nanoindenter tips, a rounded conical (∼1200 nm radius) and a sharp cube corner (20–50 nm radius) were used to abrade bovine enamel. Square abraded areas (2 μm × 2 μm, 5 μm × 5 μm, 10 μm × 10 μm) were generated with loads that varied from 50 μN to 500 μN depending on the indenter tip. In addition normal and lateral forces were simultaneously measured along 10 μm single scratched lines with the sharp cube corner tip. SEM (scanning electron microscopy) and TEM (transmission electron microscopy) were also used to characterise the worn areas and debris. Two different wear mechanisms were observed depending on the geometry of the tip. The rounded tip generates a predominantly elastic contact that mainly compresses and plastically deforms the superficial material and generates severe shear deformation within the sub-surface material which, under certain conditions, fractures and removes material from the sample. The sharp tip cuts into and ploughs the enamel creating a wedge or ridge of material ahead of itself which eventually detaches. This sequence is repeated continuously for every passage of the sharp indenter tip. The different mechanisms are discussed in terms of abrading tip contact angle and enamel microstructure.

Small scale, grain size and substrate effects in nano-indentation experiment of film–substrate systems

The mechanical properties of film–substrate systems have been investigated through nano-indentation experiments in our former paper (Chen, S.H., Liu, L., Wang, T.C., 2005. Investigation of the mechanical properties of thin films by nano-indentation, considering the effects of thickness and different coating–substrate combinations. Surf. Coat. Technol., 191, 25–32), in which Al–Glass with three different film thicknesses are adopted and it is found that the relation between the hardness H and normalized indentation depth h/ t, where t denotes the film thickness, exhibits three different regimes: (i) the hardness decreases obviously with increasing indentation depth; (ii) then, the hardness keeps an almost constant value in the range of 0.1–0.7 of the normalized indentation depth h/ t; (iii) after that, the hardness increases with increasing indentation depth. In this paper, the indentation image is further investigated and finite element method is used to analyze the nano-indentation phenomena with both classical plasticity and strain gradient plasticity theories. Not only the case with an ideal sharp indenter tip but also that with a round one is considered in both theories. Finally, we find that the classical plasticity theory can not predict the experimental results, even considering the indenter tip curvature. However, the strain gradient plasticity theory can describe the experimental data very well not only at a shallow indentation depth but also at a deep depth. Strain gradient and substrate effects are proved to coexist in film–substrate nano-indentation experiments.

Depth-Dependent Hardness Characterization by Nanoindentation using a Berkovich Indenter with a Rounded Tip

AbstractThe height difference Δhb between the ideally sharp Berkovich indenter tip and a Δhb rounded tip was measured by direct observation using atomic force microscopy (AFM). The accuracy of the indirect area function method for measuring h was confirmed. The Δhb indentation size effects (ISE) in (100) single crystal copper, (100) single crystal tungsten, and fused quartz were characterized by applying the ISE model considering the rounded tip effect. The model fits the data these materials well, even though fused quartz does not deform by dislocations. However, a very small value of the ISE characteristic length h' was obtained for fused quartz. The present h' value for (100) copper is 32% larger than a previously-measured value for polycrystalline copper. This may indicate that grain boundaries suppress the dislocation activity envisioned in the ISE model.

Deformation behavior of Ni 3Al single crystals during nanoindentation

The deformation behavior of (1 1 1), (1 1 0) and (0 0 1) oriented Ni 3Al single crystals was investigated by means of nanoindentation. Upon loading with the blunt and sharp indenter tips, the crystal deforms elastically in the initial stage followed by plastic deformation of which the onset is characterized by an obvious displacement burst (or pop-in) in the loading curve. This pop-in corresponds to homogeneous nucleation of dislocation loops under the indenter. When a sharp indenter tip was used, a major pop-in can be identified at a large load (∼7 mN for (1 1 1) crystal) in the plastic regime on loading. The major pop-in may be correlated with the special dislocation structure of the K–W locks in the Ni 3Al crystals that are formed during loading. The pop-in behavior during plastic deformation of Ni 3Al crystals is found to be closely related to the crystal orientation, pre-existing dislocation density in the sample surface, loading rate, and holding (at a constant sub-critical load) time as well. Pop-ins were also observed at critical loads in unloading processes.