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.     

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.     

A study on the determination of plastic properties of metals by instrumented indentation using two sharp indenters

An earlier optimisation approach proposed by Luo et al. [Luo, J., Lin, J., Dean, T. A., 2006. A Study on the Determination of Mechanical Properties of a power-law Material by Its Indentation Force-Depth Curve. Philosophical Magazine, 86(19), 2881-2905], which is based on the assumption that the instrumented indentation force-depth response of an elastic–plastic material is a linear combination of the corresponding elastic and elastic–perfect plastic materials, is extended in this work to extract mechanical properties of a power-law material from two given experimental indentation P–h curves for conical indenters of half included angles of 60° and 70.3°. It was found that the non-uniqueness problem encountered in the single P–h curve optimisation approach is effectively removed by the two P–h curves optimisation. The appropriateness of the use of second half included angle of 60° is discussed. For the five representative materials Al, Ti, Fe, Ni and steel, it was found that the maximum relative prediction errors for E, σ_y and n are 2%, 10.4% and 11.3%, respectively. The prediction accuracy of mechanical properties E, σ_y and n is generally better than other methods reported in the literature.     

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.     

测量界面软铬层力学性质的纳米压入法

为了测量双层铬的界面软铬层力学性质,提出了化学腐蚀基体法,通过溶解掉基体制备没有基体支撑的自由铬层,将在横截面内线状显示的界面转化为界面表面(铬层与基体相连接的面),避免了横截面不能显示界面表面的缺点。对界面表面进行纳米压入实验和借助于表征薄膜力学性质的表面压入能量法,测得了描述界面软铬层力学性质的弹性模量和压入弹、塑性功等参数。     

Phenomenological study of parabolic and spherical indentation of elastic-ideally plastic material

A phenomenological study of parabolic and spherical indentation of elastic ideally plastic materials was carried out by using precise results of finite elements calculations. The study shows that no “pseudo-Hertzian” regime occurs during spherical indentation. As soon as the yield stress of the indented material is exceeded, a deviation from the, purely elastic Hertzian contact behaviour is found. Two elastic–plastic regimes and two plastic regimes are observed for materials of very large Young modulus to Yield stress ratio, E/σ_y. The first elastic–plastic regime corresponds to a strong evolution of the indented plastic zone. The first plastic regime corresponds to the commonly called “fully plastic regime”, in which the average indentation pressure is constant and equal to about three times the yield stress of the indented material. In this regime, the contact depth to penetration depth ratio tends toward a constant value, i.e. h_c/h = 1.47. h_c/h is only constant for very low values of yield strain (σ_y/E lower than 5 × 10^?6) when aE¹/Rσ_y is higher than 10,000. The second plastic regime corresponds to a decrease in the average indentation pressure and to a steeper increase in the pile-up. For materials with very large E/σ_y ratio, the second plastic regime appears when the value of the non-dimensional contact radius a/R is lower than 0.01. In the case of spherical and parabolic indentation, results show that the first plastic regime exists only for elastic-ideally plastic materials having an E/σ_y ratio higher than approximately 2.000.     

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.     

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.     

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.     

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.     

On establishing elastic–plastic properties of a sphere by indentation testing

Instrumented indentation is a popular technique for determining mechanical properties of materials. Currently, the evaluation techniques of instrumented indentation are mostly limited to a flat substrate being indented by various shaped indenters (e.g., conical or spherical). This work investigates the possibility of extending instrumented indentation to non-flat surfaces. To this end, conical indentation of a sphere is investigated where two methodologies for establishing mechanical properties are explored. In the first approach, a semi-analytical approach is employed to determine the elastic modulus of the sphere utilizing the elastic unloading response (the “unloading slope”). In the second method, reverse analysis based on finite element analysis is used, where non-dimensional characteristic functions derived from the force–displacement response are utilized to determine the elastic modulus and yield strength. To investigate the accuracies of the proposed methodologies, selected numerical experiments have been performed and excellent agreement was obtained.     

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。     

Effective elastic modulus of film-on-substrate systems under normal and tangential contact

Load and depth sensing indentation methods have been widely used to characterize the mechanical properties of the thin film-substrate systems. The measurement accuracy critically depends on our knowledge of the effective elastic modulus of this heterogeneous system. In this work, based on the exact solution of the Green's function in Fourier space, we have derived an analytical relationship between the surface tractions and displacements, which depends on the ratio of the film thickness to contact size and the generalized Dundurs parameters that describe the modulus mismatch between the film and substrate materials. The use of the cumulative superposition method shows that the contact stiffness of any axisymmetric contact is the same as that of a flat-ended punch contact. Therefore, assuming a surface traction of the form of [1−(r/a)²]^−1/2 with radial coordinate r and contact size a, we can obtain an approximate representation of the effective elastic moduli, which agree extremely well with the finite element simulations for both normal and tangential contacts. Motivated by a recently developed multidimensional nanocontact system, we also explore the dependence of the ratio of tangential to normal contact stiffness on the ratio of film thickness to contact radius and the Dundurs parameters. The analytical representations of the correction factors in the relationship between the contact stiffness and effective modulus are derived at infinite friction conditions.     

Investigation of Near-Surface Mechanical Properties of Materials Using Atomic Force Microscopy

As ultra-thin films or small-scale structures become widely used in electronics and biology, knowledge concerning their near-surface mechanical properties of the materials is increasingly important. Atomic force microscopy (AFM) is employed to determine near-surface elastic modulus via force-penetration curves acquired during indentation. Samples include polydimethylsiloxane (PDMS), parylene, mica, and single-crystal silicon, and indentations are performed with single-crystal silicon and silicon nitride AFM tips. An analysis algorithm based on the secant modulus method is proposed to extract the true penetration curves from the experimental displacement curves. The penetration data is then analyzed in terms of Hertzian model to estimate the elastic modulus. Three concerns in applying nanoscale AFM indentation to the measurement of the elastic modulus of an ultra-thin material are addressed. First, the effect of the lateral force caused by the inclined angle of the cantilevered probe is investigated theoretically and by numerical simulation. A second concern is local plastic deformation induced by a sharp probe tip. In this case, numerical results show a relatively small effect on the force-penetration curves if the plastic deformation is limited to the central area below the probe tip. The deviation of the elastic-plastic simulation from the elastic estimation depends on the yield strength of the material. Finally, the effect of stiffness matching between the AFM probe and the sample is a key issue that is studied numerically, and appropriate stiffness matching criteria are suggested.     

A computational study on the instrumented sharp indentations with dual indenters

Finite element analysis was performed to investigate the indentation response of elasto-plastic solids for conical indenters of half included angles of 60° and 70.3°. The interdependence indentation parameters resulting from a single indentation load–depth curve is considered. Regarding dimensional analysis, several dimensionless relationships are constructed as functions of the reduced elastic modulus-loading curvature ratio E¹/C and the strain hardening exponent n. Further, the duality between corresponding parameters with dual indenters is explored. Finally, a new method based on dual indenters is proposed to extract the strain hardening exponent and the reduced elastic modulus of an indented material. The accuracy of this method is verified and discussed with experimental data from the literature and representative materials.     

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.      

Stress-Dependent Elastic Behaviour of a Titanium Alloy at Elevated Temperatures

In this study the influence of stress and temperature on the elastic modulus during fully-reversed low cycle fatigue of the titanium alloy Ti6242 is examined. The change of the elastic properties with stress manifests itself in a crescent-like shaped hysteresis loop of stress vs. plastic strain at very low amplitudes, i.e. below the technical yield stress. A quadratic extension of Hooke??s law with a second constant ??k?? is applied. The parameters are determined all along the unloading curve in tension and compression. The approach results in the alignment of the hysteresis loop so that they become vertical, i.e. the elastic strain is accurately described. The value and sign of ??k?? depend on whether the deformation occurs in tension or compression. Like the Young??s modulus E ₀, ??k?? also depends on temperature. At temperatures up to 550°C the values of ??k?? in tension and compression do not change during fatigue life. However, at 650°C thermally activated slip processes lead to changes of both, E ₀ and ??k??.     

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.     

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.