On the uniqueness of measuring elastoplastic properties from indentation: The indistinguishable mystical materials

Indentation is widely used to extract material elastoplastic properties from the measured force-displacement curves. One of the most well-established indentation techniques utilizes dual (or plural) sharp indenters (which have different apex angles) to deduce key parameters such as the elastic modulus, yield stress, and work-hardening exponent for materials that obey the power-law constitutive relationship. However, the uniqueness of such analysis is not yet systematically studied or challenged. Here we show the existence of “mystical materials”, which have distinct elastoplastic properties yet they yield almost identical indentation behaviors, even when the indenter angle is varied in a large range. These mystical materials are, therefore, indistinguishable by many existing indentation analyses unless extreme (and often impractical) indenter angles are used. Explicit procedures of deriving these mystical materials are established, and the general characteristics of the mystical materials are discussed. In many cases, for a given indenter angle range, a material would have infinite numbers of mystical siblings, and the existence maps of the mystical materials are also obtained. Furthermore, we propose two alternative techniques to effectively distinguish these mystical materials. The study in this paper addresses the important question of the uniqueness of indentation test, as well as providing useful guidelines to properly use the indentation technique to measure material elastoplastic properties.     

Experimental and numerical investigations of the deformation of soft materials under tangential loading

The surface ‘tensile test’, in which tangential loads are applied through surface mounted adhesive tapes, is a viable method for the assessment of mechanical properties of soft materials, particularly biological soft materials in vivo. In the present work the deformation pattern and force–displacement relationship in the surface tensile test were experimentally investigated using surface displacement analysis (SDA) and numerically simulated using finite element modelling. The experimental and FE results showed close agreement using silicone rubber as a model material. The force–displacement relationship was found to be dependent on the tape separations. SDA measurements and FE simulation showed that the displacement and strain fields were not uniform and the distribution pattern varies with tape separation. A combined experimental–numerical approach to inversely extract material properties using multiple tests with different length scales is proposed and assessed using a model material.     

Analysis of spherical indentation of superelastic shape memory alloys

Dimensional analysis and the finite element method are applied in this paper to study spherical indentation of superelastic shape memory alloys. The scaling relationships derived from dimensional analysis bridge the indentation response and the mechanical properties of a superelastic shape memory alloy. Several key variables of a superelastic indentation curve are revealed and examined. We prove that the bifurcation force in a superelastic indentation curve only relies on the forward transformation stress and the elastic properties of the initial austenite; and the return force in a superelastic indentation curve only relies on the reverse transformation stress and the elastic properties of the initial austenite. Furthermore, the dimensionless functions to determine the bifurcation force and the return force are proved to be identical. These results not only enhance our understanding of spherical indentation of superelastic shape memory alloys, but also provide the theoretical basis for developing a practicable method to calibrate the mechanical properties of a superelastic material from the spherical indentation test.     

On establishing elastic–plastic properties of a sphere by indentation testing

Instrumented indentation is a popular technique for determining mechanical properties of materials. Currently, the evaluation techniques of instrumented indentation are mostly limited to a flat substrate being indented by various shaped indenters (e.g., conical or spherical). This work investigates the possibility of extending instrumented indentation to non-flat surfaces. To this end, conical indentation of a sphere is investigated where two methodologies for establishing mechanical properties are explored. In the first approach, a semi-analytical approach is employed to determine the elastic modulus of the sphere utilizing the elastic unloading response (the “unloading slope”). In the second method, reverse analysis based on finite element analysis is used, where non-dimensional characteristic functions derived from the force–displacement response are utilized to determine the elastic modulus and yield strength. To investigate the accuracies of the proposed methodologies, selected numerical experiments have been performed and excellent agreement was obtained.     

Mechanics of indentation of plastically graded materials—II: Experiments on nanocrystalline alloys with grain size gradients

A systematic study of depth-sensing indentation was performed on nanocrystalline (nc) Ni-W alloys specially synthesized with controlled unidirectional gradients in plastic properties. A yield strength gradient and a roughly constant Young's modulus were achieved in the nc alloys, using electrodeposition techniques. The force vs. displacement response from instrumented indentation experiments matched very well with that predicted from the analysis of Part I of this paper. The experiments also revealed that the pile-up of the graded alloy around the indenter is noticeably higher than that for the two homogeneous reference alloys that constitute the bounding conditions for the graded material. These trends are also consistent with the predictions of the indentation analysis.     

Material characterization based on dual indenters

Extensive large strain-large deformation finite element analyses were carried out to investigate the response of elasto-plastic materials obeying power law-strain hardening during the loading and unloading process of instrumented indentation with conical indenters of different apex angles. The relationships between the characteristics of the indentation load–displacement curves and the elasto-plastic material properties were computationally established. A reverse analysis algorithm based on load–displacement curves obtained from dual indenters was presented. It was demonstrated that the proposed reverse analysis algorithm can uniquely recover the elasto-plastic material properties from the load–displacement curves of two conical indenters with different apex angles. The numerical results obtained are in good agreement with published values.     

Conical indentation of incompressible rubber-like materials

In the last decade, the indentation test has become a useful tool for probing mechanical properties of small material volumes. In this context, little has been done for rubber-like materials (elastomers), although there is pressing need to use instrumented indentation in biomechanics and tissue examination. The present work investigates the quasi-static normal instrumented indentation of incompressible rubber-like substrates by sharp rigid cones. A second-order elasticity analysis was performed in addition to finite element analysis and showed that the elastic modulus at infinitesimal strains correlates well with the indentation response that is the relation between the applied force and the resulting vertical displacement of the indentor’s tip. Three hyperelastic models were analyzed: the classic Mooney–Rivlin model, the simple Gent model and the one-term Ogden model. The effect of the angle of the cone was investigated, as well as the influence of surface friction. For blunt cones, the indentation response agrees remarkably well with the prediction of linear elasticity and confirms available experimental results of instrumented Vickers indentation.     

Indentation responses of piezoelectric films

Frictionless indentation responses of transversely isotropic piezoelectric film/rigid substrate systems under circular cylindrical indenter (i.e., punch), conical indenter (i.e., cone), and spherical indenter (i.e., sphere) are investigated. Both insulating and conducting indenters are considered. The technique of Hankel transformation is employed to derive the corresponding dual integral equations for the mixed boundary value indentation problems. For the two limiting cases of infinitely thick and infinitely thin piezoelectric films, closed-form solutions are obtained. For piezoelectric films of finite thickness, a numerical method is constructed to solve the dual integral equations and semi-empirical models having only two unknown parameters are proposed for the responses of indentation force, electric charge and electric potential, and contact radius. With the two parameters inferred from the numerical results, the semi-empirical formulae are found to provide good estimates of the indentation responses for the two limiting cases of infinitely thick and thin piezoelectric films, as well as those in between. The inferred parameters in the proposed semi-empirical formulae for normalized indentation force and electric charge are checked against four different piezoelectric materials and are found to be insensitive to the selection of piezoelectric materials. It is believed that the proposed semi-empirical indentation formulae are useful in developing experimental indentation techniques to extract the material properties of piezoelectric films.     

Improved reverse analysis for material characterization with dual sharp indenters

It was illustrated by the author in the previous work that combinations between material properties and indentation parameters can be used as mixed parameters in dimensionless functions to capture the indentation response of materials to single and dual sharp indenters. These issues are further extended in the present study. A parametric finite element analysis was performed to investigate the conical indentation response of elasto-plastic solids. Frictional effects are studied. Conical indenters of half-included angles from 50° to 88° are considered to examine several fundamental features of instrumented sharp indentation within the frame work of limit analysis. Regarding dimensional analysis, it is found that a Taylor series expansion according to the elastic indentation work-total indentation work ratio W_e/W_t can be used to improve dimensionless functions. Within this context, a new set of dimensionless functions is explicitly constructed for hardness and indentation parameters of single and dual indenters. Based on formulated functions, a reverse analysis with dual sharp indenters, which was previously proposed by the author, is improved to extract mechanical properties of materials.     

A computational study on the instrumented sharp indentations with dual indenters

Finite element analysis was performed to investigate the indentation response of elasto-plastic solids for conical indenters of half included angles of 60° and 70.3°. The interdependence indentation parameters resulting from a single indentation load–depth curve is considered. Regarding dimensional analysis, several dimensionless relationships are constructed as functions of the reduced elastic modulus-loading curvature ratio E¹/C and the strain hardening exponent n. Further, the duality between corresponding parameters with dual indenters is explored. Finally, a new method based on dual indenters is proposed to extract the strain hardening exponent and the reduced elastic modulus of an indented material. The accuracy of this method is verified and discussed with experimental data from the literature and representative materials.     

A study on robust indentation techniques to evaluate elastic–plastic properties of metals

Spherical indentation is studied based on numerical analysis and experiment, to develop robust testing techniques to evaluate isotropic elastic–plastic material properties of metals. The representative stress and plastic strain concept is critically investigated via finite element analysis, and some conditions for the representative values are suggested. The representative values should also be a function of material properties, not only indenter angle for sharp indenter and indentation depth for spherical indenter. The pros and cons of shallow and deep spherical indentation techniques are also discussed. For an indentation depth of 20% of an indenter diameter, the relationships between normalized indentation parameters and load–depth data are characterized, and then numerical algorithm to estimate material elastic–plastic curve is presented. From the indentation load–depth curve, the new approach provides stress–strain curve and the values of elastic modulus, yield strength, and strain-hardening exponent with an average error of less than 5%. The method is confirmed to be valid for various elastic properties of indenter. Experimental validation of the approach then is performed by using developed micro-indentation system. For the material severely disobeying power law hardening, a modified method to reduce errors of predicted material properties is contrived. It is found that our method is robust enough to get ideal power law properties, and applicable to input of more complex physics.     

Spherical indentation of incompressible rubber-like materials

In recent years, indentation tests have been proven very useful in probing mechanical properties of small volumes of materials. However, a class of materials that very little has been done in this direction is rubber-like materials (elastomers). The present work investigates the spherical indentation of incompressible rubber-like materials. The analysis is performed in the context of second-order hyperelasticity and is accompanied by finite element computations and an extensive experimental program with spherical indentors of different radii. Uniaxial tensile tests were also performed and it was found that the initial elastic modulus correlates well with the indentation response. The experiments suggest stiffer indentation response than that predicted by linear elasticity, which is somehow counter-intuitive, if the uniaxial material response is to be considered. Regarding the uniqueness of the inverse problem, that is to establish material properties from spherical indentation tests, the answer is disappointing. We prove that the inverse problem does not give unique answer regarding the constitutive relation, except for the initial stiffness.     

The effect of large deformation and material nonlinearity on gel indentation

A gel, an aggregate of polymers with solvents, has dual attributes of solid and liquid as solvent migrates in and out of the polymer network. Indentation has recently been used to characterize the mechanical properties of gels. This paper evaluates the effects of large deformation and material nonlinearity on gel indentation through theoretical modeling and finite element analysis. It is found that large deformation significantly affects the interpretation of the experimental observations and the classical relation between indentation force and depth has limitations for large deformation. The material nonlinearity does not play a very important role on indentation experiment so that the poroelasticity is a good approximation. Based on these observations, this paper proposes an alternative approach to measure the mechanical properties of gels, namely, uniaxial compression experiment.     

Influence of penetration depth and mechanical properties on contact radius determination for spherical indentation

Knowledge of the relationship between the penetration depth and the contact radius is required in order to determine the mechanical properties of a material starting from an instrumented indentation test. The aim of this work is to propose a new penetration depth–contact radius relationship valid for most metals which are deformed plastically by parabolic and spherical indenters. Numerical simulation results of the indentation of an elastic–plastic half-space by a frictionless rigid paraboloïd of revolution show that the contact radius–indentation depth relationship can be represented by a power law, which depends on the reduced Young’s modulus of the contact, on the strain hardening exponent and on the yield stress of the indented material. In order to use the proposed formulation for experimental spherical indentations, adaptation of the model is performed in the case of a rigid spherical indenter. Compared to the previous formulations, the model proposed in the present study for spherical indentation has the advantage of being accurate in the plastic regime for a large range of contact radii and for materials of well-developed yield stress. Lastly, a simple criterion, depending on the material mechanical properties, is proposed in order to know when piling-up appears for the spherical indentation.     

On the Measurement of two Independent Viscoelastic Functions with Instrumented Indentation Tests

In the present paper, a methodology for complete characterization of linear isotropic viscoelastic material with spherical instrumented indentation test is proposed. The developed method allows for measuring two independent viscoelastic functions, shear relaxation modulus and time-dependent Poisson’s ratio, from the indentation test data obtained at non-decreasing loading, but otherwise arbitrary. Finite element modelling (FEM) is relied upon for validating the proposed methodology and for quantifying the influence of experimental variables on the measurements accuracy. Spherical indentation experiments are performed on several viscoelastic materials: polyoxymethylene, bitumen and bitumen-filler mastics. The viscoelastic material functions obtained with the indentation tests are compared with the corresponding results from the standard mechanical tests. Numerical and experimental results presented indicate that the methodology proposed allows mitigating the machine compliance and loading rate effects on the accuracy of the viscoelastic indentation tests.     

The Nano-Jackhammer effect in probing near-surface mechanical properties

Because of its ease of implementation and insensitivity to indenter drift, dynamic indentation techniques have been frequently used to measure mechanical properties of bulk and thin film materials as a function of indenter displacement. However, the actual effect of the oscillating tip on the material response has not been examined. Recently, it has been shown that the oscillation used with dynamic indentation techniques alters the measured hardness value of ductile metallic materials, especially at depths less than 200 nm. The alteration in the hardness is due to the added energy associated with the oscillation which assists dislocation nucleation. Atomistic simulations on nickel thin films agree with experiments that more dislocations are nucleated during dynamic indents than with quasi-static indents. Through the analysis of quasi-static and dynamic indents made into nickel single crystals and thin films, a theory to describe this phenomenon is presented. This is coined the Nano-Jackhammer effect, a combination of dislocation nucleation and strain rate sensitivity caused by indentation with a superimposed dynamic oscillation.     

An analytical solution for a linear viscoelastic layer loaded with a cylindrical punch: Evaluation of the rebound indentation test with application for assessing viability of articular cartilage

A general closed-form solution for the so-called rebound indentation test’ is obtained for a cylindrical flat-ended punch indenting a linear viscoelastic layer lying on a rigid substrate. Under the assumption of time-independent Poisson's ratio, we derive closed-form analytical expressions for the contact force (in a displacement controlled regime) and for the indentation displacement (in a load-controlled regime) and we consider in detail the case of standard viscoelastic solid. Our results indicate that the rebound displacement (in other words the indentation displacement in the load-controlled stage) is independent of the relaxed elastic modulus and Poisson's ratio, and also of the layer's thickness. Our analytical solution can be used for layered samples of arbitrary materials exhibiting viscoelastic properties; however, since the rebound indentation test has been recently suggested for assessing the viability of biomedical materials, we have applied our theoretical framework to the identification of materials parameters from experiments on articular cartilage. In this context, we have found a pretty good agreement for the rebound deformation, even until the strain becomes relatively large.     

Indentation responses of piezoelectric films ideally bonded to an elastic substrate

The influences of elastic substrate on the indentation force, contact radius, electric potential and electric charge responses of piezoelectric film/substrate systems are investigated by the integral transform method. The film is assumed to be ideally bonded to the substrate and the contact interaction between the indenter and the film is assumed to be frictionless, with three kinds of axisymmetric insulating and conducting indenters (i.e., punch, cone and sphere) considered. Obtained results show that when the ratio of the contact radius to the film thickness is close to zero, the influences of the elastic substrate disappear and the indentation behaviors converge to the piezoelectric half space solutions while the indentation responses approach the corresponding ones of elastic half space as the ratio gets to infinity. The transition between the piezoelectric and the elastic half space indentation solutions for the film/substrate system is quantified in terms of the film thickness and the elasticity of the substrate. Finite element analysis on an insulating sphere indentation is conducted to verify the numerical calculations and good agreement is observed. The obtained results are believed to be useful for developing experimental techniques to extract the material properties of piezoelectric film/substrate systems.     

An analytical solution for a linear viscoelastic layer loaded with a cylindrical punch: Evaluation of the rebound indentation test with application for assessing viability of articular cartilage

A general closed-form solution for the so-called rebound indentation test’ is obtained for a cylindrical flat-ended punch indenting a linear viscoelastic layer lying on a rigid substrate. Under the assumption of time-independent Poisson's ratio, we derive closed-form analytical expressions for the contact force (in a displacement controlled regime) and for the indentation displacement (in a load-controlled regime) and we consider in detail the case of standard viscoelastic solid. Our results indicate that the rebound displacement (in other words the indentation displacement in the load-controlled stage) is independent of the relaxed elastic modulus and Poisson's ratio, and also of the layer's thickness. Our analytical solution can be used for layered samples of arbitrary materials exhibiting viscoelastic properties; however, since the rebound indentation test has been recently suggested for assessing the viability of biomedical materials, we have applied our theoretical framework to the identification of materials parameters from experiments on articular cartilage. In this context, we have found a pretty good agreement for the rebound deformation, even until the strain becomes relatively large.     

The frictional sliding response of elasto-plastic materials in contact with a conical indenter

Over the past decade, many computational studies have explored the mechanics of normal indentation. Quantitative relationships have been well established between the load–displacement hysteresis response and material properties. By contrast, very few studies have investigated broad quantitative aspects of the effects of material properties, especially plastic deformation characteristics, on the frictional sliding response of metals and alloys. The response to instrumented, depth-sensing frictional sliding, hereafter referred to as a scratch test, could potentially be used for material characterization. In addition, it could reproduce a basic tribological event, such as asperity contact and deformation, at different length scales for the multi-scale modeling of wear processes. For these reasons, a comprehensive study was undertaken to investigate the effect of elasto-plastic properties, such as flow strength and strain hardening, on the response to steady-state frictional sliding. Dimensional analysis was used to define scaling variables and universal functions. The dependence of these functions on material properties was assessed through a detailed parametric study using the finite element method. The strain hardening exponent was found to have a greater influence on the scratch hardness and the pile-up height during frictional sliding than observed in frictionless normal indentation. When normalized by the penetration depth, the pile-up height can be up to three times larger in frictional sliding than in normal indentation. Furthermore, in contrast to normal indentation, sink-in is not observed during frictional sliding over the wide range of material properties examined. Finally, friction between indenter and indented material was introduced in the finite element model, and quantitative relationships were also established for the limited effects of plastic strain hardening and yield strength on the overall friction coefficient. Aspects of the predictions of computational simulations were compared with experiments on carefully selected metallic systems in which the plastic properties were systematically controlled. The level of accuracy of the predicted frictional response is also assessed by recourse to the finite element method and by comparison with experiment.