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.     

Determining the Elastic Modulus of Compliant Thin Films Supported on Substrates from Flat Punch Indentation Measurements

Instrumented indentation is a technique that can be used to measure the elastic properties of soft thin films supported on stiffer substrates, including polymer films, cellulosic sheets, and thin layers of biological materials. When measuring thin film properties using indentation, the effect of the substrate must be considered. Most existing models for determining the properties of thin films from indentation measurements were developed for metal and dielectric films bonded to semiconductor substrates and have been applied to systems with film-substrate modulus ratios between 0.1 and 10. In the present work, flat punch indentation of a thin film either bonded to or in contact with a substrate is examined using finite element modeling. A broad range of film-substrate modulus ratios from 0.0001 to 1 are investigated. As the substrate is effectively rigid compared to the film when the film-substrate modulus ratio is less than 0.0001, the results are also useful for understanding systems with lower film-substrate modulus ratios. The effects of the contact radius, film thickness, elastic properties, and friction between the film and the substrate on the measured stiffness were quantified using finite element modeling in order to understand how the elastic properties of the film can be extracted from indentation measurements. A semi-analytical model was developed to describe the finite element modeling results and facilitate the use of the results to analyze experimental measurements. The model was validated through analysis of indentation measurements of thin polyethylene sheets that were supported on substrates of various stiffness.     

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 Discontinuous Elastic Interface Transfer Model of Thin Film Nanoindentation

A new model of thin film indentation that accounted for an apparent discontinuity in elastic strain transfer at the film/substrate interface was developed. Finite element analysis suggested that numerical values of strain were not directly continuous across the interface; the values in the film were higher when a soft film was deposited on a hard substrate. The new model was constructed based on this discontinuity; whereby, separate weighting factors were applied to account for the influence of the substrate in strain developed in the film and vice-versa. By comparing the model to experimental data from thirteen different amorphous thin film materials on a silicon substrate, constants in each weighting factor were found to have physical significance in being numerically similar to the bulk scale Poisson’s ratios of the materials involved. When employing these material properties in the new model it was found to provide an improved match to the experimental data over the existing Doerner and Nix and Gao models. Finally, the model was found to be capable of assessing the Young’s modulus of thin films that do not exhibit a flat region as long as the bulk Poisson’s ratio is known.     

不锈钢表面等离子合金化渗铜层的纳米力学性能研究

为了研究不锈钢渗铜层的纳米力学性能,本文采用等离子表面合金化技术在304不锈钢表面制备了渗铜层。利用纳米压入硬度仪,采用连续刚度测试法,对渗铜层以及不锈钢基体的表面和横截面的纳米力学性能进行了测试,得到了纳米压入过程的载荷-压入深度曲线,发现渗铜层抵抗外载荷的能力低于不锈钢基体。并得到了渗铜层和不锈钢基体的表面、横截面方向的硬度以及杨氏模量,经对比得到渗铜层的杨氏模量和硬度都要比不锈钢基体的低,并且渗铜层的力学性能表现出各向异性。对纳米压入的数据进行分析,发现渗铜层在小尺度压入时硬度和杨氏模量表现出明显的"尺度效应"。     

Effect of CNT length and CNT-matrix interphase in carbon nanotube (CNT) reinforced composites

The load transfer mechanisms and effective moduli of single-walled nanotube (SWNT) reinforced composites are studied using a continuum model. A “critical” fiber length is defined for full load transfer by numerically evaluating the strain-energy-changes for different fiber lengths. The effective longitudinal Young’s modulus and bulk modulus of the composite are derived. The effect of the interphase is also discussed. The results indicate the fiber length is critical both to the load transfer efficiency and effective moduli of the composite. The SWNT-matrix interphase plays an important role in load transfer efficiency but affects the effective moduli only slightly.     

Numerical simulation of debonding of adhesively bonded joint

This paper describes a numerical method to simulate the debonding of adhesively bonded joints. Assuming that the adhesive thickness and the adhesive Young’s modulus are small with respect to the characteristic length of the joint and to the Young’s modulus of the adherents, a simplified model is derived in the case of large displacements using the asymptotic expansion technique. Then, the problem of the crack growth is stated, in the case of a stable growth, as the search of the local minima of the total energy of the joint, sum of the mechanical energy and the Griffith’s fracture energy. This is made using the Newton’s method. To this end, the expressions of the first and second derivatives of the mechanical energy with respect to a crack front displacement are derived analytically. Finally, numerical examples are presented, highlighting the unstable character of the crack growth at initiation.     

Extraction of Mechanical Properties with Second Harmonic Detection for Dynamic Nanoindentation Testing

In this article, a new method based on the detection of the second harmonic of the displacement signal to determine mechanical properties of materials from dynamic nanoindentation testing, is presented. With this technique, the Young’s modulus and hardness of homogeneous materials can be obtained at small penetration depths from the measurement of the second harmonic amplitude. With this innovative method, the measurement of the normal displacement is indirectly used, avoiding the need for very precise contact detection. Moreover, the influence of the tip defect and thermal drift on the measurements are reduced. This method was used for dynamic nanoindentation tests performed on fused silica and on an amorphous polymer (PMMA) because these materials are supposed not to exhibit an indentation size effect at small penetration depths. The amplitude of the second harmonic of the displacement signal was correctly measured at small depths, allowing to calculate the Young’s modulus and the hardness of the tested materials. The mechanical properties calculated with this method are in good agreement with values obtained from classical nanoindentation tests.     

An inverse problem in film/substrate indentation: extracting both the Young’s modulus and thickness of films

In an indentation test, the effective Young’s modulus of a film/substrate bilayer heterostructure varies with the indentation depth, a phenomenon known as the substrate effect. In previous studies investigating this, only the Young’s modulus of the film was unknown. Once the effective Young’s modulus of a film/substrate structure is determined at a given contact depth, the Young’s modulus of the film can be uniquely determined, i.e., there is a one-to-one relation between the Young’s modulus of the film and the film/substrate effective Young’s modulus. However, at times it is extremely challenging or even impossible to measure the film thickness. Furthermore, the precise definition of the layer/film thickness for a two-dimensional material can be problematic. In the current study, therefore, the thickness of the film and its Young’s modulus are treated as two unknowns that must be determined. Unlike the case with one unknown, there are infinite combinations of film thickness and Young’s modulus which can yield the same effective Young’s modulus for the film/substrate. An inverse problem is formulated and solved to extract the Young’s modulus and thickness of the film from the indentation depth-load curve. The accuracy and robustness of the inverse problem-solving method are also demonstrated.     

An Instrumented Indentation Method for Young’s Modulus Measurement with Accuracy Estimation

The relationships between indentation responses and Young’s modulus of an indented material were investigated by employing dimensional analysis and finite element method. Three representative tip bluntness geometries were introduced to describe the shape of a real Berkovich indenter. It was demonstrated that for each of these bluntness geometries, a set of approximate indentation relationships correlating the ratio of nominal hardness/reduced Young’s modulus H _n /E _r and the ratio of elastic work/total work W _e/W can be derived. Consequently, a method for Young’s modulus measurement combined with its accuracy estimation was established on basis of these relationships. The effectiveness of this approach was verified by performing nanoindentation tests on S45C carbon steel and 6061 aluminum alloy and microindentation tests on aluminum single crystal, GCr15 bearing steel and fused silica.     

Three-dimensional modeling of the mechanical property of linearly elastic open cell foams

Three-dimensional Voronoi models are developed to investigate the mechanical behavior of linearly elastic open cell foams. Dependence of the Young’s modulus, Poisson’s ratio and bulk modulus of the foams on the relative density is evaluated through finite element analysis. Obtained results show that in the low density regime the Young’s modulus and bulk modulus of random Voronoi foams can be well represented by those of Kelvin foams, and are sensitive to the geometric imperfections inherent in the microstructure of foams. In contrast, the compressive plateau stress of the foams is less sensitive to the imperfections. Failure surface of the foams subject to multi-axial compression is determined and is found to comply with the maximum compressive principal stress criterion, consistent with available experimental observations on polymer foams. Numerical results also show that elastic buckling of cell edges at microscopic level is the dominant mechanism responsible for the compressive failure of elastic open cell foams.     

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.     

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.     

二维材料力学行为的压痕测试

准确了解二维材料的力学性能对于推动其应用具有重要意义, 无基底压痕技术是目前最广泛采用的二维材料力学性能测试方法之一, 本文综述了二维材料压痕研究的最新进展以及所面临的问题, 并对将来的研究工作进行了展望.无基底压痕技术是将二维材料转移到带有沟槽或柱形孔的基底上, 制备二维材料"梁"和"鼓"模型, 然后利用原子力显微镜测量其在压针作用下的载荷--位移关系, 最后通过基于连续介质薄膜导出的压痕响应分析模型拟合实验结果, 估算出二维材料的弹性模量和本征强度.由于二维材料的厚度远小于连续介质薄膜, 来自于压头以及基底孔侧壁的范德华力对二维材料的压痕响应具有显著影响, 造成二维材料与传统压痕分析模型中的基本假设不符, 导致不能准确预测二维材料的弹性模量; 另外, 由于传统压痕模型无法准确描述二维材料在大变形下的非线性行为, 以及由缺陷等引起的应力集中, 导致由压痕测试表征的二维材料(特别是多晶二维材料)本征强度具有较大的偏差. 因此, 一方面需要正确了解由压痕技术获得的二维材料力学性能, 另一方面还需对目前的研究方法做进一步的改进和完善.      

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.     

用能量法分析层状材料弹性接触问题

利用能量法分析了层状材料（薄膜／基体）弹性接触问题，得到了具有一阶精度的闭合解，给出了求解薄膜弹性模量和泊松比的表达式，并与有限元的数值解进行了比较。二者比较结果表明：在工程材料范围内，理论解与数值解相差在6％以内；同时表明单相材料中剪切模量与弹性模量之间的关系也适用层状材料中的薄膜材料。在数值解的基础上，讨论了薄膜厚度与压头半径的比值对求解精度的影响，发现此比值对精度影响不大。通过对层状材料等效泊松比与等效弹性模量的定义，给出了用压痕实验测定薄膜泊松比与弹性模量的方法。     

Finite deformation continuum model for single-walled carbon nanotubes

A continuum-based model for computing strain energies and estimating Young’s modulus of single-walled carbon nanotubes (SWCNTs) is developed by using an energy equivalence-based multi-scale approach. A SWCNT is viewed as a continuum hollow cylinder formed by rolling up a flat graphite sheet that is treated as an isotropic continuum plate. Kinematic analysis is performed on the continuum level, with the Hencky (true) strain and the Cauchy (true) stress being employed to account for finite deformations. Based on the equivalence of the strain energy and the molecular potential energy, a formula for calculating Young’s modulus of SWCNTs is derived. This formula, containing both the molecular and continuum scale parameters, directly links macroscopic responses of nanotubes to their molecular structures. Sample numerical results show that the predictions by the new model compare favorably with those by several existing continuum and molecular dynamics models.     

Indentation tests investigation of mechanical behavior of two-dimensional materials

准确了解二维材料的力学性能对于推动其应用具有重要意义, 无基底压痕技术是目前最广泛采用的二维材料力学性能测试方法之一, 本文综述了二维材料压痕研究的最新进展以及所面临的问题, 并对将来的研究工作进行了展望.无基底压痕技术是将二维材料转移到带有沟槽或柱形孔的基底上, 制备二维材料"梁"和"鼓"模型, 然后利用原子力显微镜测量其在压针作用下的载荷--位移关系, 最后通过基于连续介质薄膜导出的压痕响应分析模型拟合实验结果, 估算出二维材料的弹性模量和本征强度.由于二维材料的厚度远小于连续介质薄膜, 来自于压头以及基底孔侧壁的范德华力对二维材料的压痕响应具有显著影响, 造成二维材料与传统压痕分析模型中的基本假设不符, 导致不能准确预测二维材料的弹性模量; 另外, 由于传统压痕模型无法准确描述二维材料在大变形下的非线性行为, 以及由缺陷等引起的应力集中, 导致由压痕测试表征的二维材料(特别是多晶二维材料)本征强度具有较大的偏差. 因此, 一方面需要正确了解由压痕技术获得的二维材料力学性能, 另一方面还需对目前的研究方法做进一步的改进和完善.     

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.     

Very Large Poisson’s Ratio with a Bounded Transverse Strain in Anisotropic Elastic Materials

In a recent paper by Ting and Chen [18] it was shown by examples that Poisson’s ratio can have no bounds for all anisotropic elastic materials. With the exception of cubic materials, the examples presented involve a very large transverse strain. We show here that a very large Poisson’s ratio with a bounded transverse strain exists for all anisotropic elastic materials. The large Poisson’s ratio with a bounded transverse strain occurs when the axial strain is in the direction very near or at the direction along which Young’s modulus is very large. In fact the transverse strain has to be very small for the material to be stable. If the non-dimensionalized Young’s modulus is of the order δ⁻¹, where δ is very small, the axial strain, the transverse strain and Poisson’s ratio are of the order δ, δ^1/2 and δ^−1/2, respectively. Mathematics Subject Classifications (2000) 74B05, 74E10.T.C.T. Ting: Professor Emeritus of University of Illinois at Chicago and Consulting Professor of Stanford University.