Size effect in the initiation of plasticity for ceramics in nanoindentation

The indentation size effect has been observed for many years and is usually associated with increasing hardness as the depth of indentation is reduced for pyramidal indenters. The indentation size effect for spherical indenters has recently been associated with an increase in the yield stress of metals proportional to the inverse cube root of indenter radius [Spary, I.J., Bushby, A.J., Jennett, N.M., 2006. On the indentation size effect in spherical indentation. Philos. Mag. 86 (33), 5581-5593]. Here we investigate ceramic materials where the yield point is high enough to be easily distinguished in nanoindentation tests. A robust method for determining the yield point from a nanoindentation test with spherical indenters is presented. The results for a range of ceramics confirm that the increase in yield pressure is directly proportional to the inverse cube root of indenter radius. Furthermore, the yield pressure is also shown to be proportional to the inverse square root of the contact radius. Revisiting data in the literature shows that this inverse square root relationship is also true for pyramidal indenters. This implies that the indentation size effect is driven by the contact area rather than by the depth of indentation or by the indenter radius.     

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.     

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.     

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.     

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.     

Two new expanding cavity models for indentation deformations of elastic strain-hardening materials

Two expanding cavity models (ECMs) are developed for describing indentation deformations of elastic power-law hardening and elastic linear-hardening materials. The derivations are based on two elastic–plastic solutions for internally pressurized thick-walled spherical shells of strain-hardening materials. Closed-form formulas are provided for both conical and spherical indentations, which explicitly show that for a given indenter geometry indentation hardness depends on Young’s modulus, yield stress and strain-hardening index of the indented material. The two new models reduce to Johnson’s ECM for elastic-perfectly plastic materials when the strain-hardening effect is not considered. The sample numerical results obtained using the two newly developed models reveal that the indentation hardness increases with the Young’s modulus and strain-hardening level of the indented material. For conical indentations the values of the indentation hardness are found to depend on the sharpness of the indenter: the sharper the indenter, the larger the hardness. For spherical indentations it is shown that the hardness is significantly affected by the strain-hardening level when the indented material is stiff (i.e., with a large ratio of Young’s modulus to yield stress) and/or the indentation depth is large. When the indentation depth is small such that little or no plastic deformation is induced by the spherical indenter, the hardness appears to be independent of the strain-hardening level. These predicted trends for spherical indentations are in fairly good agreement with the recent finite element results of Park and Pharr.     

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.      

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.     

平头压痕试验确定热障涂层弹性模量的方法研究

本文模拟了典型热障涂层(TBC)结构在平头压痕作用下的力学响应,重点研究利用平头压痕法确定TBC涂层弹性模量的方法。研究发现k(单位压入应力下压头的压入位移)不仅与材料的性质有关,还与压头的半径有关。本文提出:通过两个不同尺寸的平压头可以同时确定陶瓷层和粘结层的弹性模量。     

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)     

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．     

Analytical and experimental determination of the material intrinsic length scale of strain gradient plasticity theory from micro- and nano-indentation experiments

The enhanced gradient plasticity theories formulate a constitutive framework on the continuum level that is used to bridge the gap between the micromechanical plasticity and the classical continuum plasticity. They are successful in explaining the size effects encountered in many micro- and nano-advanced technologies due to the incorporation of an intrinsic material length parameter into the constitutive modeling. However, the full utility of the gradient-type theories hinges on one's ability to determine the intrinsic material length that scales with strain gradients, and this study aims at addressing and remedying this situation. Based on the Taylor's hardening law, a micromechanical model that assesses a nonlinear coupling between the statistically stored dislocations (SSDs) and geometrically necessary dislocations (GNDs) is used here in order to derive an analytical form for the deformation-gradient-related intrinsic length-scale parameter in terms of measurable microstructural physical parameters. This work also presents a method for identifying the length-scale parameter from micro- and nano-indentation experiments using both spherical and pyramidal indenters. The deviation of the Nix and Gao [Mech. Phys. Solids 46 (1998) 411] and Swadener et al. [J. Mech. Phys. Solids 50 (2002) 681; Scr. Mater. 47 (2002) 343] indentation size effect (ISE) models’ predictions from hardness results at small depths for the case of conical indenters and at small diameters for the case of spherical indenters, respectively, is largely corrected by incorporating an interaction coefficient that compensates for the proper coupling between the SSDs and GNDs during indentation. Experimental results are also presented which show that the ISE for pyramidal and spherical indenters can be correlated successfully by using the proposed model.     

The capillary force in micro- and nano-indentation with different indenter shapes

The influence of the indenter shapes and various parameters on the magnitude of the capillary force is studied on the basis of models describing the wet adhesion of indenters and substrates joined by liquid bridges. In the former, we consider several shapes, such as conical, spherical and truncated conical one with a spherical end. In the latter, the effects of the contact angle, the radius of the wetting circle, the volume of the liquid bridge, the environmental humidity, the gap between the indenter and the substrate, the conical angle, the radius of the spherical indenter, the opening angle of the spherical end in the truncated conical indenter are included. The meniscus of the bridge is described using a circular approximation, which is reasonable under some conditions. Different dependences of the capillary force on the indenter shapes and the geometric parameters are observed. The results can be applicable to the micro- and nano-indentation experiments. It shows that the measured hardness is underestimated due to the effect of the capillary force.     

考虑压头尖端曲率的弹塑性材料硬度的解答形式

结合近来发表的对金属材料采用球形压头的微压痕实验结果及Johnson对应原理，讨论了在传统弹塑性理论下锥形压头在计及压头顶端曲率半径影响时硬度的解答形式．进而得出结论：压头尖端曲率半径不是引起尺度效应的根源，相反，它会使尺度效应减弱．     

考虑压头曲率半径和应变梯度的微压痕分析

在压头尖端曲率半径取100nm的前提下，采用Chen和Wang的应变梯度理论，对微压痕实验进行了系统的数值分析. 首先通过拟合载荷-位移实验曲线的后半段来确定材料的屈服应力和幂硬化指数值,然后用有限元方法数值模拟压痕实验，并将计算得到的整段载荷-位移曲线及硬度-位移曲线和实验结果进行了比较. 结果表明应变梯度理论所预测的计算结果和实验结果很好地符合,包括压痕深度在亚微米和微米范围内的整段曲线.     

Simulation of micro-indentation hardness of FCC single crystals by mechanism-based strain gradient crystal plasticity

The size effect observed in the micro-indentation of FCC single crystal copper is modelled by the employment of mechanism-based strain gradient crystal plasticity (MSG-CP). The total slip resistance in each active system is assumed to be due to a mixed population of forest obstacles arising from both statistically stored and geometrically necessary dislocations. The MSG-CP constitutive model is implemented into the Abaqus/Standard FE platform by developing the User MATerial subroutine UMAT. The simulation of micro-indentation hardness on (0 0 1) and (1 1 1) single crystal copper, with a conical indenter having a sharp tip, a conical indenter with a spherical tip and a three-sided Berkovich indenter, is undertaken. The phenomena of pile-up and sink-in have been observed in the simulation and dealt with by appropriate use of the contact analysis function in Abaqus. These phenomena have been taken into account in the determination of the contact areas and hence the average indentation depth for anisotropic single crystals. The depth dependence of the micro-indentation hardness, the size effect, is calculated. The micro-hardness results from the simulation are compared with those of the published experimental ones in the literature and a good agreement is found.     

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.     

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.     

Depth-sensing indentation of a transversely isotropic elastic layer: Second-order asymptotic models for canonical indenters

Simple analytical approximations to the frictionless indentation problem for a transversely isotropic layer are obtained for spherical, conical, and pyramidal indenters as well as for axisymmetric indenters of power-low profile and self-similar non-axisymmetric indenters. These approximations are asymptotically exact in the small-contact limit. The results obtained are validated in the case of an isotropic layer for spherical and conical indenters.     

Cylindrical nano-indentation on metal film/elastic substrate system with discrete dislocation plasticity analysis: A simple model for nano-indentation size effect

The cylindrical nano-indentation on metal film/elastic substrate is computationally studied using two-dimensional discrete dislocation plasticity combined with the commercial software ANSYS®, with a focus on the storage volume for geometrically necessary dislocations (GNDs) inside the films and the nano-indentation size effect (NISE). Our calculations show that almost all GNDs are stored in a rectangular area determined by the film thickness and the actual contact width. The variations of indentation contact width with indentation depth for various film thicknesses and indenter radii are fitted by an exponential relation, and then the GND density underneath the indenter is estimated. Based on the Taylor dislocation model and Tabor formula, a simple model for the dependence of the nano-indentation hardness of the film/substrate system on the indentation depth, the indenter radius and the film thickness is established, showing a good agreement with the present numerical results.