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.     

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.     

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.     

Analysis of elastic and plastic deformation associated with indentation testing of thin films on substrates

A study has been made of the elastic and plastic deformation associated with submicrometer indentation of thin films on substrates using the finite element method. The effects of the elastic and plastic properties of both the film and substrate on the hardness of the film/substrate composite are studied by determining the average pressure under the indenter as a function of the indentation depth. Calculations have been made for film/substrate combinations for which the substrate is either harder or softer than the film and for combinations for which the substrate is either stiffer or more compliant than the film. It is found, as expected, that the hardness increases with indentation depth when either the yield strength or the elastic modulus of the substrate is higher than that of the film. Correspondingly, the hardness decreases with indentation depth when the yield strength or elastic modulus of the substrate is lower than that of the film. Functional equations have been developed to predict the hardness variation with depth under these different conditions. Finite element simulation of the unloading portion of the load displacement curve permits a determination of the elastic compliance of the film/substrate composite as a function of indentation depth. The elastic properties of the film can be separated from those of the substrate using this information. The results are in good agreement with King's analytical treatment of this problem.     

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.     

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.      

Mechanics of indentation for piezoelectric thin films on elastic substrate

Frictionless normal indentation problem of rigid flat-ended cylindrical, conical and spherical indenters on piezoelectric film, which is either in frictionless contact with or perfectly bonded to an elastic half-space (substrate), is investigated. Both conducting and insulating indenters are considered. With Hankel transform, the general solutions of the homogeneous governing equations for the piezoelectric layer and the elastic half-space are presented. Using the boundary conditions for a vertical point force or a point electric charge, and the boundary conditions on the film/substrate interface, the Green’s functions can be obtained by solving sets of simultaneous linear algebraic equations. The solution of the indentation problem is obtained by integrating these Green’s functions over the contact area with unknown surface tractions or electric charge distribution, which will be determined from the boundary conditions on the contact surface between the indenter and the film. The solution is expressed in terms of dual integral equations that are converted to a Fredholm integral equation of the second kind and solved numerically. Numerical examples are also presented. The comparison between two film/substrate bonding conditions is made. It shows that the indentation rigidity of the film/substrate system is lower when the film is in frictionless contact with the substrate. The effects of the Young’s modulus and Poisson’s ratio of the elastic substrate, indenter electrical condition and indenter prescribed electric potential on the indentation responses are presented.     

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.     

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.     

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.     

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.     

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.     

On the determination of the Young’s modulus of thin films using indentation tests

The main difficulty with the characterization of thin coatings using depth-sensing indentation tests is related to the determination of the contributions of the substrate and the film to the measured properties. In this study, three-dimensional numerical simulations of the Vickers hardness test are used in order to examine the influence of the elastic and plastic properties of the substrate and the film on the composite’s Young’s modulus results. The hardness of the film is equal to or higher than the substrate hardness. A study of the stress distributions and the indentation geometry of composites, film/substrate, was performed, taking into account the relative mechanical properties of the film and substrate. In addition, stress evolution during indentation was studied, in order to quantify the critical indentation depth under which the substrate is not elastically deformed. The accurate evaluation of the Young’s modulus of the films using weight functions is also examined: some of these have previously been proposed and one was introduced for this study. Two different fitting procedures were used to compare the results obtained from eight fictive film/substrate combinations using six weight functions. The first procedure, commonly used, considers the substrate’s modulus as a known parameter in the fitting process. In the second, the film and the substrate’s modulus are considered as unknown variables that are calculated simultaneously during the fitting process. The validity of the conclusions obtained using the fictive materials was checked by applying the weight functions to four real composites.     

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.     

利用维氏和玻氏压头表征半导体材料断裂韧性

压痕法是测量材料断裂韧性 ($K_{\rm IC})$ 的常用方法之一, 如何根据不同的材料、不同的压头选择适合的公式, 是当前面临的一大问题. 因此,在不同载荷下对单晶硅 (111) 和碳化硅 (4H-SiC, 0001面) 这两种半导体材料进行了维氏微米硬度和玻氏纳米压痕实验, 对实验产生的裂纹长度$c$进行了统计分析, 并采用13个压痕公式计算材料的$K_{\rm IC}$, 开展了微米划痕实验, 验证压痕法评估半导体材料$K_{\rm IC}$的适用性. 研究结果表明: 为了消除维氏压痕实验产生的$c$的固有离散性, 需要多次测量取平均值; 裂纹长度与压痕尺寸的比值随压痕载荷的增大而增大; 材料的裂纹类型与载荷相关且低载荷下表现为巴氏裂纹, 高载荷下表现为中位裂纹; 与微米划痕实验得到的单晶硅和碳化硅材料的$K_{\rm IC}$平均值 (分别为0.96 MPa,$\cdot$,$\sqrt{\rm m}$和2.89 MPa,$\cdot$,$\sqrt{\rm m}$) 相比, 在同一压头下无法从13个公式中获得同时适用于单晶硅和碳化硅材料的压痕公式,但在同一材料下可以获得同时适用于维氏和玻氏压头的$K_{\rm IC}$计算公式; 基于中位裂纹系统发展而来的压痕公式更适合用于评估半导体材料的$K_{\rm IC}$, 且维氏压头下的$K_{\rm IC}$与玻氏压头下$K_{\rm IC}$的关系不是理论上的1.073倍, 应为1.13$\pm 压痕法是测量材料断裂韧性(K_(IC))的常用方法之一,如何根据不同的材料、不同的压头选择适合的公式,是当前面临的一大问题.因此,在不同载荷下对单晶硅(111)和碳化硅(4H-Si C, 0001面)这两种半导体材料进行了维氏微米硬度和玻氏纳米压痕实验,对实验产生的裂纹长度c进行了统计分析,并采用13个压痕公式计算材料的K_(IC),开展了微米划痕实验,验证压痕法评估半导体材料K_(IC)的适用性.研究结果表明:为了消除维氏压痕实验产生的c的固有离散性,需要多次测量取平均值;裂纹长度与压痕尺寸的比值随压痕载荷的增大而增大;材料的裂纹类型与载荷相关且低载荷下表现为巴氏裂纹,高载荷下表现为中位裂纹;与微米划痕实验得到的单晶硅和碳化硅材料的K_(IC)平均值(分别为0.96 MPa·m~(1/2)和2.89 MPa·m~(1/2))相比,在同一压头下无法从13个公式中获得同时适用于单晶硅和碳化硅材料的压痕公式,但在同一材料下可以获得同时适用于维氏和玻氏压头的K_(IC)计算公式;基于中位裂纹系统发展而来的压痕公式更适合用于评估半导体材料的K_(IC),且维氏压头下的K_(IC)与玻氏压头下K_(IC)的关系不是理论上的1.073倍,应为1.13±0.01.     

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.     

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.     

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．     

Indentation of a hard film on a soft substrate: Strain gradient hardening effects

The strain gradient work hardening is important in micro-indentation of bulk metals and thin metallic films, though the indentation of thin films may display very different behavior from that of bulk metals. We use the conventional theory of mechanism-based strain gradient plasticity (CMSG) to study the indentation of a hard tungsten film on soft aluminum substrate, and find good agreement with experiments. The effect of friction stress (intrinsic lattice resistance), which is important in body-center-cubic tungsten, is accounted for. We also extend CMSG to a finite deformation theory since the indentation depth in experiments can be as large as the film thickness. Contrary to indentation of bulk metals or soft metallic films on hard substrate, the micro-indentation hardness of a hard tungsten film on soft aluminum substrate decreases monotonically with the increasing depth of indentation, and it never approaches a constant (macroscopic hardness). It is also shown that the strain gradient effect in the soft aluminum substrate is insignificant, but that in the hard tungsten thin film is important in shallow indentation. The strain gradient effect in tungsten, however, disappears rapidly as the indentation depth increases because the intrinsic material length in tungsten is rather small.     

A numerical approach to indentation technique to evaluate material properties of film-on-substrate systems

Spherical indentation approach (Lee et al., 2005, Lee et al., 2010) for the evaluation of bulk material properties is extended to that for elastic–plastic properties of film-on-substrate systems. Our interest focuses on single isotropic, metallic, and elastic–plastic film on a substrate, and we do not consider the size effects in plasticity behavior. We first determine the optimal data acquisition location, where the strain gradient is the least and the effect of friction is negligible. Dimensional analysis affords the mapping parameters as functions of normalized indentation variables. An efficient way is further introduced to reduce both the number of analyses and the regression order of mapping functions. The new numerical approach to the film indentation technique is then proposed by examining the finite element solutions at the optimal point. With the new approach, the values of elastic modulus, yield strength, and strain-hardening exponent of film materials are successfully obtained from the spherical indentation tests. We have shown that the effective property ranges such as indenter properties, substrate modulus, and E/E_s ratio can be extended without additional simulations and even loss of accuracy. For other ranges of variables or other properties, which are not dealt with in this study, this methodology is applicable through resetting FEA variables and finding proper normalized parameters.