The correlation of the indentation size effect measured with indenters of various shapes

Experimental results are presented which show that the indentation size effect for pyramidal and spherical indenters can be correlated. For a pyramidal indenter, the hardness measured in crystalline materials usually increases with decreasing depth of penetration, which is known as the indentation size effect. Spherical indentation also shows an indentation size effect. However, for a spherical indenter, hardness is not affected by depth, but increases with decreasing sphere radius. The correlation for pyramidal and spherical indenter shapes is based on geometrically necessary dislocations and work-hardening. The Nix and Gao indentation size effect model (J. Mech. Phys. Solids 46 (1998) 411) for conical indenters is extended to indenters of various shapes and compared to the experimental results.     

The indenter tip radius effect in micro- and nanoindentation hardness experiments.

Nix and Gao established an important relation between the microindentation hardness and indentation depth. Such a relation has been verified by many microindentation experiments (indentation depths in the micrometer range), but it does not always hold in nanoindentation experiments (indentation depths approaching the nanometer range). Indenter tip radius effect has been proposed by Qu et al. and others as possibly the main factor that causes the deviation from Nix and Gao's relationship. We have developed an indentation model for micro- and nanoindentation, which accounts for two indenter shapes, a sharp, conical indenter and a conical indenter with a spherical tip. The analysis is based on the conventional theory of mechanism-based strain gradient plasticity established from the Taylor dislocation model to account for the effect of geometrically necessary dislocations. The comparison between numerical result and Feng and Nix's experimental data shows that the indenter tip radius effect indeed causes the deviation from Nix-Gao relation, but it seems not be the main factor. The project supported by the National Natural Science Foundation of China (10121202) and the Ministry of Education of China (20020003023)     

Determination of mechanical properties by instrumented indentation

The paper reviews the current state of the depth-sensing indentation (sometimes called nanoindentation), where the information on material behaviour and properties is obtained from the indenter load and depth, measured continuously during loading and unloading. It is shown how the contact parameters and principal characteristics are determined using pointed or spherical indenters. Indentation tests can be used for the measurement of hardness and elastic modulus, and also of the yield stress and for the construction of stress–strain diagrams, for the determination of the work of indentation and its components. Most devices use monotonic loading and unloading, but some also enable measurement under a small harmonic signal added to the basic monotonously increasing load. This makes possible continuous measurement of contact stiffness and the study of dynamic properties and the determination of properties of coatings. One section is devoted to the measurement on viscoelastic-plastic materials, where the delayed deforming must be considered during the measurement as well as in data evaluation. Instrumented indentation can also be used for the study of creep under high temperatures. The paper also discusses the errors arising in depth-sensing measurements and informs briefly about some other possibilities of the method.     

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.     

Polymer indentation: Numerical analysis and comparison with a spherical cavity model

Three dimensional analyses of indentation of a polymer by a rigid indenter are carried out. The polymer is characterized by a finite strain elastic-viscoplastic constitutive relation and the calculations are carried out with a dynamic finite element program used to simulate quasi-static behavior. Two types of indenter are considered; a conical indenter and a pyramidal indenter. For each indenter type, different values of the sharpness of the indenter are considered and two rates of indentation are analyzed. Significant sink-in is found to occur in all cases considered. The amount of sink-in is found to be smaller for sharper indenters. The calculated values of both the nominal and true hardness do not differ significantly for the two indenter shapes. An expanding spherical cavity model is also considered and the predictions of this model are compared with the finite element results for various indenter shapes and indentation rates. The spherical cavity model is found to give fairly good agreement with the predictions of the finite element analyses for the nominal polymer hardness for both indenter shapes.     

A NUMERICAL STUDY OF INDENTATION WITH SMALL SPHERICAL INDENTERS

The finite element method for the conventional theory of mechanism-based strain gradient plasticity is used to study the indentation size effect. For small indenters （e.g., radii on the order of 10μm）, the maximum allowable geometrically necessary dislocation （GND） density is introduced to cap the GND density such that the latter does not become unrealistically high. The numerical results agree well with the indentation hardness data of iridium. The GND density is much larger than the density of statistically stored dislocations （SSD） underneath the indenter, but this trend reverses away from the indenter. As the indentation depth （or equivalently, contact radius） increases, the GND density decreases but the SSD density increases.     

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.     

纳米压痕过程的三维有限元数值试验研究

采用有限元方法模拟了纳米压痕仪的加、卸载过程，三维有限元模型考虑了纳米压痕仪的标准Berkovich压头．介绍了有限元模型的几何参数、边界条件、材料特性与加载方式，讨论了摩擦、滑动机制、试件模型的大小对计算结果的影响，进行了计算结果与标准试样实验结果的比较，证实了模拟的可靠性．在此基础上，重点研究了压头尖端曲率半径对纳米压痕实验数据的影响．对比分析了尖端曲率半径r＝0与r＝100nm两种压头的材料压痕载荷—位移曲线．结果表明，当压头尖端曲率半径r≠0时，基于经典的均匀连续介质力学本构理论、传统的实验手段与数据处理方法，压痕硬度值会随着压痕深度的减小而升高．     

Orientation effect on the Boussinesq indentation of a transversely isotropic piezoelectric material

Three-dimensional finite element analysis was used to study the effect of the angle between the loading direction and the axisymmetric direction on the indentation behavior of a transversely isotropic piezoelectric half-space by a cylindrical indenter of flat end. Two cases were considered in the analysis, which included (a) the indentation by an insulating indenter, and (b) the indentation by a conducting indenter. Both the indentation load and the indentation-induced potential were found to be proportional to the indentation depth. Using the simulation results and the analytical relationship for the indentation by a rigid, insulating indenter, semi-analytical relationships were developed between the indentation load and the indentation depth and between the indentation-induced potential on the indenter and the indentation depth for the conducting indenter, respectively. The proportionality between the indentation-induced potential and the indentation depth is only a function of the angle between the loading direction and the poling direction, independent of the type of indenters, which may be used to measure the relative direction of the loading axis to the axisymmetric axis of transversely piezoelectric materials from the indentation test.     

The indentation modulus of elastically anisotropic materials for indenters of arbitrary shape

The contact of an indenter of arbitrary shape on an elastically anisotropic half space is considered. It is demonstrated in a theorem that the solution of the contact problem is the one that maximizes the load on the indenter for a given indentation depth. The theorem can be used to derive the best approximate solution in the Rayleigh-Ritz sense if the contact area is a priori assumed to have a certain shape. This approach is used to analyze the contact of a sphere and an axisymmetric cone on an anisotropic half space. The contact area is assumed to be elliptical, which is exact for the sphere and an approximation for the cone. It is further shown that the contact area is exactly elliptical even for conical indenters when a limited class of Green's functions is considered. If only the first term of the surface Green's function Fourier expansion is retained in the solution of the axisymmetric contact problem, a simpler solution is obtained, referred to as the equivalent isotropic solution. For most anisotropic materials, the contact stiffness determined using this approach is very close to the value obtained for both conical and spherical indenters by means of the theorem. Therefore, it is suggested that the equivalent isotropic solution provides a quick and efficient estimate for quantities such as the elastic compliance or stiffness of the contact. The “equivalent indentation modulus”, which depends on material and orientation, is computed for sapphire and diamond single crystals.     

Stiffness relations for piezoelectric indentation of flat and non-flat punches of arbitrary planform: Applications to probing nanoelectromechanical properties of materials

Stiffness relations for voltage-dependent contact mechanics of piezoelectric material are derived for an indenter of arbitrary planform under normal force, centrally or non-centrally applied, and electric charge distribution at the base. Relations between indentation depth, indentation force, electric potential and electric charge are explicitly given in terms of indenter's geometry and piezoelectric material constants. The analysis covers indenters with non-flat base approximated by a second-order surface; elliptic paraboloid is considered as an example. In the case of the elliptic non-flat planform, the derived stiffness relations are exact; otherwise, they are approximate and are shown to have good accuracy. The stiffness relations are given in elementary functions and are obtained by utilizing the recently established principle of correspondence between the piezoelectric and purely elastic problems. Besides contributing to extension of Hertzian mechanics to piezoelectric materials, these results are essential for quantitative interpretation of the scanning probe microscopy and piezoelectric nanoindentation data on piezoelectric, ferroelectric, and multiferroic materials.     

The equivalent axisymmetric model for Berkovich indenters in power-law hardening materials

Nix and Gio [Nix, W.D., Gao, H.J., 1998. Indentation size effects in crystalline materials: a law for strain gradient plasticity. Journal of the Mechanics and Physics of Solids 46, 411–425] established an important relation between the micro-indentation hardness and indentation depth for axisymmetric indenters. For the Berkovich indenter, however, this relation requires an equivalent cone angle. Qin et al. [Qin, J., Huang, Y., Xiao, J., Hwang, K.C., 2009. The equivalence of axisymmetric indentation model for three-dimensional indentation hardness. Journal of Materials Research 24, 776–783] showed that the widely used equivalent cone angle from the criterion of equal base area leads to significant errors in micro-indentation, and proposed a new equivalence of equal cone angle for iridium. It is shown in this paper that this new equivalence holds for a wide range of plastic work hardening materials. In addition, the prior equal-base-area criterion does not hold because the Berkovich indenter gives much higher density of geometrically necessary dislocations than axisymmetric indenter. The equivalence of equal cone angle, however, does not hold for Vickers indenter.     

Contact with stick zone between an indenter and a thin incompressible layer

The dominant asymptotic term for the indentation of a thin elastic incompressible layer by an axisymmetric rigid indenter is considered. Complete adhesion is supposed everywhere in the contact area or else in a given inner region surrounded by an annular frictionless zone. Both the problems are formulated in the form of systems of coupled dual integral equations. Using operators transforming kernels of the Hankel transform into kernels of the Weber–Orr transform, the dual integral equations are reduced to systems of Fredholm integral equations of the second kind whose structures permit deriving asymptotic solutions. Simple expressions for the contact stresses, the penetration depth, and the contact radius in the case of an unknown contact area are obtained. Explicit formulae, derived for the flat and power law indenter profiles, allow us to analyze how stick and frictionless zones affect mechanical characteristics. Results manifest that the punch penetration exhibits strong sensitivity to contact conditions inspite of the fact that the radial traction is small. A conical indenter is less sensitive than flat-ended and spherical indenters.     

Spherical indentation of freestanding circular thin films in the membrane regime

We present theoretical and experimental results to describe the mechanics of indentation of a clamped circular membrane with a frictionless spherical indenter. Analytical expressions and numerical simulations are presented for the relationships between contact radius, finite indentation strains (and stresses), pre-stretch, loads and deflection. These closed-form solutions are contrasted with point-load models that neglect the contact size (i.e. classical Schwerin-type solutions), and lead to important differences in the indentation strain and load-deflection response. The accuracy of these closed form expressions is illustrated by comparisons with detailed numerical results and experiments on thin elastomer films. We show that the closed-form solutions can be used to extract mechanical properties from indentation testing of freestanding films, with important implications for developing new tests on nanoscale films and/or compliant materials such as polymers and biological substances.     

Comparison between Berkovich,Vickers and conical indentation tests: A three-dimensional numerical simulation study

Three-dimensional numerical simulations of Berkovich, Vickers and conical indenter hardness tests were carried out to investigate the influence of indenter geometry on indentation test results of bulk and composite film/substrate materials. The strain distributions obtained from the three indenters tested were studied, in order to clarify the differences in the load–indentation depth curves and hardness values of both types of materials. For bulk materials, the differentiation between the results obtained with the three indenters is material sensitive. The indenter geometry shape factor, β, for evaluating Young’s modulus for each indenter, was also estimated. Depending on the indenter geometry, distinct mechanical behaviours are observed for composite materials, which are related to the size of the indentation region in the film. The indentation depth at which the substrate starts to deform plastically is sensitive to indenter geometry.     

Mechanics of indentation of plastically graded materials—I: Analysis

The introduction of controlled gradients in plastic properties is known to influence the resistance to damage and cracking at contact surfaces in many tribological applications. In order to assess potentially beneficial effects of plastic property gradients in tribological applications, it is essential first to develop a comprehensive and quantitative understanding of the effects of yield strength and strain hardening exponent on contact deformation under the most fundamental contact condition: normal indentation. To date, however, systematic and quantitative studies of plasticity gradient effects on indentation response have not been completed. A comprehensive parametric study of the mechanics of normal indentation of plastically graded materials was therefore undertaken in this work by recourse to finite element method (FEM) computations. On the basis of a large number of computational simulations, a general methodology for assessing instrumented indentation response of plastically graded materials is formulated so that quantitative interpretations of depth-sensing indentation experiments could be performed. The specific case of linear variation in yield strength with depth below the indented surface is explored in detail. Universal dimensionless functions are extracted from FEM simulations so as to predict the indentation load versus depth of penetration curves for a wide variety of plastically graded engineering metals and alloys for interpretation of, and comparisons with, experimental results. Furthermore, the effect of plasticity gradient on the residual indentation pile-up profile is systematically studied. The computations reveal that pile-up of the graded alloy around the indenter, for indentation with increasing yield strength beneath the surface, is noticeably higher than that for the two homogeneous reference materials that constitute the bounding conditions for the graded material. Pile-up is also found to be an increasing function of yield strength gradient and a decreasing function of frictional coefficient. The stress and plastic strain distributions under the indenter tip with and without plasticity gradient are also examined to rationalize the predicted trends. In Part II of this paper, we compare the predictions of depth-sensing indentation and pile-up response with experiments on a specially made, graded model Ni-W alloy with controlled gradients in nanocrystalline grain size.     

Explicit approximations of the indentation modulus of elastically orthotropic solids for conical indenters

The elastic problem of the contact between an axisymmetric indenter and a general anisotropic (21 independent elastic constants) half space has not been solved explicitly in closed form. Implicit methods to determine the indentation modulus originate from the work of Willis [J. Mech. Phys. Solids 14 (1966) 163]; and are now available for conical, parabolic and spherical indenters [Philos. Mag. A 81 (2001) 447; J. Mech. Phys. Solids 51 (2003) 1701]. The particular case of orthotropy has also been investigated [ASME J. Tribol. 115 (1193) 650, 125 (2003) 223]. This paper proposes an explicit solution for the indentation moduli of a transversely isotropic medium and a general orthotropic medium under rigid conical indentation in the three principal material symmetry directions. The half-space Green’s functions are interpolated from their exact extreme values, then integrated and finally simplified. The proposed closed form expressions are in very good agreement with the implicit solution schemes of [Philos. Mag. A 81 (2001) 447; J. Mech. Phys. Solids 51 (2003) 1701].     

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.     

An expanding cavity model incorporating strain-hardening and indentation size effects

An expanding cavity model (ECM) for determining indentation hardness of elastic strain-hardening plastic materials is developed. The derivation is based on a strain gradient plasticity solution for an internally pressurized thick-walled spherical shell of an elastic power-law hardening material. Closed-form formulas are provided for both conical and spherical indentations. The indentation radius enters these formulas with its own dimensional identity, unlike that in classical plasticity based ECMs where indentation geometrical parameters appear only in non-dimensional forms. As a result, the newly developed ECM can capture the indentation size effect. The formulas explicitly show that indentation hardness depends on Young’s modulus, yield stress, strain-hardening exponent and strain gradient coefficient of the indented material as well as on the geometry of the indenter. The new model reduces to existing classical plasticity based ECMs (including Johnson’s ECM for elastic–perfectly plastic materials) when the strain gradient effect is not considered. The numerical results obtained using the newly developed model reveal that the hardness is indeed indentation size dependent when the indentation radius is very small: the smaller the indentation, the larger the hardness. Also, the indentation hardness is seen to increase with the Young’s modulus and strain-hardening level of the indented material for both conical and spherical indentations. The strain-hardening effect on the hardness is observed to be significant for materials having strong strain-hardening characteristics. In addition, it is found that the indentation hardness increases with decreasing cone angle of the conical indenter or decreasing radius of the spherical indenter. These trends agree with existing experimental observations and model predictions.     

基于能量密度等效的超弹性压入模型与双压试验方法

针对超弹性材料压入问题, 本文基于能量密度中值等效原理, 提出了描述球、平面、锥3类压头独立压入下载荷、深度、压头几何尺寸和Mooney-Rivlin本构关系参数之间关系的半解析超弹性压入模型(semi-theoretical hyperelastic-material indentation model, SHIM), 进而提出了球、平面、锥压入组合的双压试验方法(indentation method due to dual indenters, IMDI). 正向验证表明, 基于系列超弹性材料的本构关系参数, 由SHIM分别预测的球、平面、锥3类压入下的载荷-位移曲线与有限元分析(finite element analysis, FEA)结果之间密切吻合; 反向验证表明, 基于系列超弹性材料的FEA条件本构关系下3类压入的载荷-位移曲线, 由双压试验方法预测的Mooney-Rivlin本构关系与FEA条件本构关系密切吻合. 针对3种超弹性橡胶, 完成了球、平面、锥压入试验, 应用双压试验方法获得的3组Mooney-Rivlin本构关系均与单轴拉伸试验结果吻合良好.