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.     

单晶硅的纳米力学响应及其相变机制

硅在大规模集成电路、MEMS/NEMS、半导体工业中具有不可替代作用,但是目前对硅的塑性变形及其相变机制的理解远未成熟.采用大规模分子动力学模拟研究(100)面的单晶硅在球形金刚石压头纳米压入过程中的纳米力学响应、相变过程和相分布规律.结果表明:在弹性变形阶段载荷-压深曲线与Hertz接触理论预测结果相吻合.两者的分离点准确地预示了塑性变形的发生.金刚石结构的Si-I相向体心结构的BCT5相转变导致了单晶硅初始的塑性变形.初始形成的BCT5相在次表面形成了一个倒置的金字塔形结构.Si-II相的形成则稍微滞后一些.在较大的载荷下BCT5在压入面上形成一个四重对称的图案分布.相对于小压头条件下大的BCT5相区,大压头更有利于SiII相的发展.卸载后生成的高压Si-II相和BCT5相全部转变为非晶硅.研究结果确认了单晶硅纳米压入中BCT5相的存在;揭示了单晶硅塑性变形的相变机理,即Si-I转变为BCT5和Si-II相;并强调了Si-I相向BCT5相转变对于单晶硅塑性变形的重要作用.     

镍单晶薄膜纳米压痕的准连续介质模拟

用准连续介质方法模拟了大规模原子的镍薄膜在纳米压痕下发生初始塑性变形的行为.主要得到了:(1) 载荷-位移响应.在载荷位移曲线上除了反应晶体弹性性质的直线外还有数次的载荷突然下降过程.(2) 位错形核现象.与载荷-位移曲线上的载荷突然下降相对应的在受压的晶体上发现了位错形核现象,说明载荷的下降是因为位错形核引起的.(3) 位错的发射机制.用Peierls-Nabarro位错模型以及能量法分析了位错的发射机制,理论值与计算值吻合较好.(4) 几何必需位错密度.用一个简单的模型计算了几何必须位错密度.此外还考虑了边界条件对模拟结果的影响.     

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.     

An indentation technique for estimating the energy density as fracture toughness with Berkovich indenter for ductile bulk materials

A technique is proposed to estimate the energy density as fracture toughness for ductile bulk materials with an indentation system equipped with a Berkovich indenter based on the theory of plastic deformation energy transforming into the indentation energy of fracture. With progressive increase of penetration loads, the material damage is exhibited on the effective elastic modulus. A quadratic polynomial relationship between the plastic penetration depth and penetration load, and an approximate linear relationship between logarithmic plastic penetration depth and logarithmic effective elastic modulus are exhibited by indentation investigation with Berkovich indenter. The parameter of damage variable is proposed to determine the critical effective elastic modulus at the fracture point. And the strain energy density factor is calculated according to the equations of penetration load, plastic penetration depth and effective elastic modulus. The fracture toughness of aluminum alloy and stainless steel are evaluated by both indentation tests and K_IC fracture toughness tests. The predicted S_cr values of indentation tests are in good agreement with experimental results of CT tests.     

ANALYSIS ON PSEUDO-STEADY INDENTATION CREEP

Theoretical analysis and finite element （FE） simulation have been carried out for a constant specific load rate （CSLR） indentation creep test. Analytical results indicate that both the representative stress and the indentation strain rate become constant after a transient period. Moreover, the FE simulation reveals that both the contours of equivalent stress and equivalent plastic strain rate underneath the indenter evolve with geometrical self-similarity. This suggests that pseudo-steady indentation creep occurs in the region beneath the indenter. The representative points in the region are defined as the ones with the equivalent stress equal to the representative stress. In addition, it is revealed that the proportionality between indentation strain rate and equivalent plastic strain rate holds at the representative points during the pseudo-steady indentation creep of a power law material. A control volume （CV） beneath the indenter, which governs the indenter velocity, is identified. The size of the CV at the indented surface is approximately 2.5 times the size of the impression. The stress exponent for creep can be obtained from the pseudosteady indentation creep data. These results demonstrate that the CSLR testing technique can be used to evaluate creep parameters with the same accuracy as conventional uniaxial creep tests.     

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.     

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)     

Quasicontinuum multiscale modeling of the effect of rough surface on nanoindentation behavior

Roughness of surface has as an important influence on identifying the mechanical behavior and performance of crystalline metals. In this study, nanoindentation simulations are conducted by the two dimensional quasicontinuum method to determine the load–penetration response and the critical load associated with the onset of plasticity in rough surfaces of a face-centered cubic single crystal copper. The arithmetic roughness index, ranging between 2 and 13 Å, is used to specify the roughness of surface. Results of indentation with different roughnesses are in good agreement with previous studies for the indenter size of 10–140 Å. The resultant load–penetration scattering, which stems from the roughness, indicates different dislocation nucleation steps, different subsequent dislocations intervals and varying stiffness values of samples. It can be concluded that the surface roughness has a significant effect on the first dislocation emission because of the indenter position and surface interactions beneath it. Moreover, the critical penetration depth for the first dislocation emission increases by the increase of the contact area between the indenter and surface.

     

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.     

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.     

The Influence of Indenter Tip Imperfection and Deformability on Analysing Instrumented Indentation Tests at Shallow Depths of Penetration on Stiff and Hard Materials

We report on the difficulties of extracting plastic parameters from constitutive equations derived by instrumented indentation tests on hard and stiff materials at shallow depths of penetration. As a general rule, we refer here to materials with an elastic stiffness more than 10 % of that of the indenter and a yield strain higher than 1 %, as well as to penetration depths less than ～ 5 times the characteristic tip defect length of the indenter. We experimentally tested such a material (an amorphous alloy) by nanoindentation. To describe the mechanical response of the test, namely the force-displacement curve, it is necessary to consider the combined effects of indenter tip imperfections and indenter deformability. For this purpose, an identification procedure has been carried out by performing numerical simulations (using Finite Element Analysis) with constitutive equations that are known to satisfactorily describe the behaviour of the tested material. We propose a straightforward procedure to address indenter tip imperfection and deformability, which consists of firstly taking account of a deformable indenter in the numerical simulations. This procedure also involves modifying the experimental curve by considering a truncated length to create artificially the material’s response to a perfectly sharp indentation. The truncated length is determined directly from the loading part of the force-displacement curve. We also show that ignoring one or both of these issues results in large errors in the plastic parameters extracted from the data.     

QUASICONTINUUM SIMULATION OF NANOINDENTATION OF NICKEL FILM

A large-scale atom simulation of nanoindentation into a thin nickel film using thequasicontinuum method was performed. The initial stages of the plasticity deformation of nickelwere studied. Several useful results were obtained as follows: (1)The response of the load versusindentation depth—on the load versus indentation depth curve, besides the straight parts cor-responding to the elastic property of nickel, the sudden drop of the load occurred several times;(2) The phenomena of dislocation nucleation—the dislocation nucleation took place when theload descended, which makes it clear that dislocation nucleation causes the drop of the load;(3)The mechanism of the dislocation emission—the Peierls-Nabarro dislocation model and a pow-erful criterion were used to analyze the dislocation emission. And the computational value was ingood agreement with the predict value; (4) The density of geometrically necessary dislocations.A simple model was used to obtain the density of geometrically necessary dislocations beneaththe indenter. Furthermore, the influence of the boundary conditions on the simulation results wasdiscussed.     

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.     

The plastic zone size in indentation experiments: The analogy with the expansion of a spherical cavity

This paper provides in-depth examinations of the well-known analogy between indentation experiments and the expansion of a spherical cavity. Closed-form solutions are derived for the extension of the plastic zone in perfectly plastic and strain hardening solids. The theoretical analysis takes into account the role of elastic and plastic deformations in the overall contact response, leading to accurate solutions for cavity inflation. Presently proposed analogy is based on comprehensive finite element simulations of conical, spherical and pyramidal indentation, which allow us to find a correspondence between the parameters describing the contact response and those in expanding cavity formulations. Such parametrical identification has the advantage to hold true both in expanding cavity formulations for perfectly plastic solids and in those derived herein for strain hardening solids. Attention is given to the assessment of the plastic zone along the indented surface, as well as to quantify the influence of further plastic flow induced upon load removal on the plastic zone size.     

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.     

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.     

Delamination mechanism maps for a strong elastic coating on an elastic–plastic substrate subjected to contact loading

Hard wear resistant coatings that are subjected to contact loading sometimes fail because the coating delaminates from the substrate. In this report, systematic finite element computations are used to model coating delamination under contact loading. The coating and substrate are idealized as elastic and elastic–plastic solids, respectively. The interface between coating and substrate is represented using a cohesive zone law, which can be characterized by its strength and fracture toughness. The system is loaded by an axisymmetric, frictionless spherical indenter. We observe two failure modes: shear cracks may nucleate just outside the contact area if the indentation depth or load exceeds a critical value; in addition, tensile cracks may nucleate at the center of the contact when the indenter is subsequently removed from the surface. Delamination mechanism maps are constructed which show the critical indentation depth and force required to initiate both shear and tensile cracks, as functions of relevant material properties. The fictitious viscosity technique for avoiding convergence problems in finite element simulations of crack nucleation and growth on cohesive interfaces allows us to explore a wider parametric space that a conventional cohesive model cannot handle. Numerical results have also been compared to analytical analyses of asymptotic limits using plate bending and membrane stretching theories, thus providing guidelines for interpreting the simulation results.     

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.