Finite-element analysis of indentation experiments in surface-coated materials

There are only a few methods suitable for a quantitative characterization of the mechanical properties of surface-coated materials; indentation testing is one of those methods. Within the last decade, a great deal of effort has been made to improve the indentation test and to gather information on the complete deformation process from experimental and numerical investigations. Following this line, this contribution concentrates on the numerical calculation of the elastic-plastic field of deformation in the specimen during the indentation process and the corresponding load-depth of indentation curves in dependence on the dominating parameters. The basic idea is to determine the influence of geometrical imperfections of the indenter on the—experimentally obtained—mechanical properties such as hardness and to provide methods which enable one to distinguish between properties of the system used for testing and the material investigated. Results obtained for uncoated and coated materials are compared. Paper was presented at the 1992 SEM Spring Conference on Experimental Mechanics held in Las Vegas, NV on June 8–11.     

DETERMINATION OF CREEP PARAMETERS FROM INDENTATION CREEP EXPERIMENTS

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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.     

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.     

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.     

Temperature Dependent Viscoelastic Properties of Polymers Investigated by Small-Scale Dynamic Mechanical Analysis

The temperature-dependent viscoelastic properties of polymers were investigated by small-scale dynamic mechanical analysis in the range of −100°C to 200°C. The polymers tested included glassy polymer (atactic polystyrene), semicrystalline polymer (high-density polyethylene) and rubbery polymer (polyisobutylene). The small-scale dynamic mechanical analyses were performed by using a flat-tip indenter with an oscillating displacement of amplitude 36 nm. The force amplitude and phase angle were measured, from which the storage modulus E′ and loss tangent tanδ were calculated. The results obtained from indentation experiments are consistent with those obtained from conventional dynamic mechanical analyzer (DMA). It is thus demonstrated that the indentation technique can quantitatively measure the temperature-dependent viscoelastic properties of polymers at small dimensions.     

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.     

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．     

A Load-Based Multiple-Partial Unloading Micro-Indentation Technique for Mechanical Property Evaluation

A load-based multiple-partial unloading micro-indentation technique has been developed for evaluating mechanical properties of materials. Comparing to the current prevailing nano/micro-indentation methods, which require precise measurements of the indentation depth and load, the proposed technique only measures indentation load and the overall indentation displacement (i.e. including displacement of the loading apparatus). Coupled with a multiple-partial unloading procedure during the indentation process, this technique results in a load-depth sensing indentation system capable of determining Young’s modulus of metallic alloys with flat, tubular, or curved architectures. Test results show consistent and correct elastic modulus values when performing indentation tests on standard alloys such as steel, aluminum, bronze, and single crystal superalloys. The proposed micro-indentation technique has led to the development of a portable load-depth sensing indentation system capable of on-site, in-situ material property measurement.     

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

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

Dual-indentation technique for the assessment of strength properties of cohesive-frictional materials

We propose a dual indentation technique for the assessment of the cohesion and friction angle of cohesive-frictional materials of the Mohr–Coulomb type. The technique is based on a computational implementation of the yield design theorems applied to conical indentation tests with different apex angles. The upper bound solutions are found to be very close to flat indentation solutions available for cohesive-frictional materials. On this basis we derive fundamental hardness-to-cohesion solutions in function of the friction angle and the apex angle. By studying the property of these dimensionless relations, we show that the ratio of two hardness measurements obtained from indentation tests with different apex angles, allows one to determine the friction angle. This dual indentation method is applied to Berkovich and Corner Cube indenter assimilated to equivalent cones of different apex angle. The method is validated for a ‘model’ material, metallic glass, which has recently been identified as a cohesive-frictional materials. The only input to the method are two hardness values which we obtain by microindentation on metallic glass. The outcome are values of the cohesion and friction angle, which are found to be in excellent agreement with reported cohesion and friction angle values of metallic glass obtained by macroscopic triaxial testing and comprehensive finite-element backanalysis of indentation curves.     

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.     

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.     

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.     

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.     

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.     

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 of the impact of a sharp indenter

The present work investigates the impact of a sharp indenter at low impact velocities. A one-dimensional model is developed by assuming that the variation of indentation load as a function of depth under dynamic conditions has the same parabolic form (Kick's Law) as under static conditions. The motion of the indenter as it indents and rebounds from the target is described. Predictions are made of the peak indentation depth, residual indentation depth, contact time, and rebound velocity as functions of the impact velocity, indenter mass and target properties. Finite element simulations were carried out to assess the validity of the model for elastoplastic materials. For rate-independent materials agreement with the model was good provided the impact velocity did not exceed certain critical values. For rate-dependent materials the relationship between load and depth in the impact problem is no longer parabolic and the model predictions cannot be applied to this case. The rate-dependent case can be solved by incorporating the relationship between the motion of the indenter and the dynamic flow properties of the material into the equation of motion for the indenter.     

DETERMINATION OF FRACTURE TOUGHNESS OF BRITTLE MATERIALS BY INDENTATION

Fracture toughness is one of the crucial mechanical properties of brittle materials such as glasses and ceramics which demonstrate catastrophic failure modes. Conventional standardized testing methods adopted for fracture toughness determination require large specimens to satisfy the plane strain condition. As for small specimens, indentation is a popular, sometimes exclusive testing mode to determine fracture toughness for it can be performed on a small flat area of the specimen surface. This review focuses on the development of indentation fracture theories and the representative testing methods. Cracking pattern dependent on indenter geometry and material property plays an important role in modeling, and is the main reason for the diversity of indentation fracture theories and testing methods. Along with the simplicity of specimen requirement is the complexity of modeling and analysis which accounts for the semi-empirical features of indentation fracture tests. Some unresolved issues shaping the gap between indentation fracture tests and standardization are also discussed.     

Modeling the indentation, penetration and cavitation of elastic membranes

An energy argument is used to predict the penetration of an elastic membrane by a rigid cylindrical indenter. We study a sequence of axisymmetric equilibrium deformations beginning with the indentation of a solid disc, followed by penetration of the membrane at a critical value of the indenter displacement, and ending in a state of cavitation in which the membrane is detached from the indenter and a central traction-free hole is maintained by boundary data alone.