Young’s Modulus Measurement Using a Simplified Transparent Indenter Measurement Technique

In material nano- and micro-indentation research, it is well accepted to use the initial unloading stiffness of the load-depth curve to determine the material’s Young’s modulus. This approach requires the use of high-precision displacement sensors in order to calibrate the loading apparatus system compliance and thus obtain the load-depth curve accurately. In this research, using a transparent spherical indenter coupled with a multi-partial unloading technique, we present a simpler approach to measure the material’s Young’s modulus. Experimental results of several metallic alloys and related discussions are presented.     

High Temperature Nanoindentation of PMR-15 Polyimide

This paper presents the high temperature nanoindentation experiments performed on an aerospace polymer resin–PMR-15 polyimide. The sharp-tipped Berkovich nanoindenter equipped with a hot-stage heating system was used. The indentation experiments were performed using the “hold-at-the-peak” method at various indenter holding times and unloading rates. The creep effect was seen to decrease with increasing holding time and/or unloading rate. Procedures used to minimize the creep effect are investigated at both ambient and elevated temperatures so that the correct contact depth (together with modulus and hardness) can be determined from nanoindentation load-depth curve. The temperature dependent mechanical properties of PMR-15 are measured through the current nanoindenter and results are consistent with those obtained from macroscopic tests.     

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.     

金属材料的强度与应力-应变关系的球压入测试方法

压入法获取材料单轴应力-应变关系和抗拉强度对服役结构完整性评价有重要的基础意义.假定材料均匀连续、各向同性、应力应变关系符合Hollomon律,基于能量等效假定,即代表性体积单元(representativevolume element, RVE)的vonMises等效和有效变形域内能量中值等效假定,本文提出了关联材料载荷、深度、球压头直径和Hollomon律的四参数半解析球压入(semi-analyticalspherical indentation,SSI)模型.通过球压入载荷-深度试验关系获得材料的应力-应变关系和抗拉强度.考虑压入过程中的损伤效应,针对金属材料提出了用于球压入测试的材料弹性模量修正模型.对11种延性金属材料完成了球压入试验,采用本文提出的球压入试验方法测到的弹性模量、应力-应变关系和抗拉强度与单轴拉伸试验结果吻合良好.      

Material characterization based on dual indenters

Extensive large strain-large deformation finite element analyses were carried out to investigate the response of elasto-plastic materials obeying power law-strain hardening during the loading and unloading process of instrumented indentation with conical indenters of different apex angles. The relationships between the characteristics of the indentation load–displacement curves and the elasto-plastic material properties were computationally established. A reverse analysis algorithm based on load–displacement curves obtained from dual indenters was presented. It was demonstrated that the proposed reverse analysis algorithm can uniquely recover the elasto-plastic material properties from the load–displacement curves of two conical indenters with different apex angles. The numerical results obtained are in good agreement with published values.     

Determination of elastic and plastic mechanical properties of dentin based on experimental and numerical studies

The aim of this study is to investigate the change of mechanical properties of human dentin due to aging and spatial variation. Sections of coronal dentin are made from human molars in three groups: young, mid-aged, and old patients. A nanoindentation test is conducted from regions near the pulp to the dentin-enamel junction (DEJ) to evaluate the load-depth indentation response and determine Young's modulus and hardness. Based on the loading and unloading load-displacement curves in nanoindentation, a numerical model of plastic damage is used to study the plastic and the damage behaviors and the contribution to the degradation in the unloading stiffness. The experimental results show that Young's modulus of the inner dentin is significantly lower than that of outer dentin in each age group. Compared with the young dentin, the old dentin has greater hardness and Young's modulus with similar spatial variations. The magnitudes of the yield strength and the damage variable are also affected by aging and vary with spatial locations. In the same age group, the yield strength in inner dentin is lower than those in middle and outer dentin, more damage occurs with similar spatial variations, and the yield strength of young dentin is generally lower and causes more damage compared with those in both the mid-aged and old groups.     

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.     

Scaling relationships in conical indentation of elastic-perfectly plastic solids

Using dimensional analysis and finite element calculations we derive several scaling relationships for conical indentation into elastic-perfectly plastic solids. These scaling relationships provide new insights into the shape of indentation curves and form the basis for understanding indentation measurements, including nano- and micro-indentation techniques. They are also helpful as a guide to numerical and finite element calculations of conical indentation problems. Finally, the scaling relationships are used to reveal the general relationships between hardness, contact area, initial unloading slope, and mechanical properties of solids.     

Oliver–Pharr indentation method in determining elastic moduli of shape memory alloys—A phase transformable material

Instrumented indentation test has been extensively applied to study the mechanical properties such as elastic modulus of different materials. The Oliver–Pharr method to measure the elastic modulus from an indentation test was originally developed for single phase materials. During a spherical indentation test on shape memory alloys (SMAs), both austenite and martensite phases exist and evolve in the specimen due to stress-induced phase transformation. The question, “What is the measured indentation modulus by using the Oliver–Pharr method from a spherical indentation test on SMAs?” is answered in this paper. The finite element method, combined with dimensional analysis, was applied to simulate a series of spherical indentation tests on SMAs. Our numerical results indicate that the measured indentation modulus strongly depends on the elastic moduli of the two phases, the indentation depth, the forward transformation stress, the transformation hardening coefficient and the maximum transformation strain. Furthermore, a method based on theoretical analysis and numerical simulation was established to determine the elastic moduli of austenite and martensite by using the spherical indentation test and the Oliver–Pharr method. Our numerical experiments confirmed that the proposed method can be applied in practice with satisfactory accuracy. The research approach and findings can also be applied to the indentation of other types of phase transformable materials.     

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.     

基于微米力学实验的页岩I型断裂韧度表征

页岩断裂韧度($K_{IC})$是页岩气储层水力压裂设计的基础参数之一,由于组成的非均质性,常规宏观力学测量方法存在制样困难、力学解释参数不连续、精度偏低等问题. 如何及时获取页岩的断裂特性,确保安全高效的工程施工,是当前面临的一大问题. 因此,提出了基于微米力学实验的页岩Ⅰ型断裂韧度分析方法,可用于页岩微裂纹起裂、发育直至形成宏观裂纹的机理研究,进行页岩宏观Ⅰ型断裂韧度预测. 基于页岩多尺度组成分析,开展了维氏压头和玻氏压头的页岩微米力学实验,分析了页岩残余压痕与压头间的相似关系、有效测试载荷以及压头参数的优化与选择. 分析了不同压入载荷下的页岩细观断裂韧度分布特征,开展了宏观巴西圆盘实验,验证页岩微米力学测试方法的适用性. 研究结果表明,在有效载荷范围内的页岩细观Ⅰ型断裂韧度波动性较小,当压入载荷过大时,由于岩样压痕区域出现局部剥落导致断裂韧度测量值偏小. 与宏观实验的比对分析显示,微米力学实验的$K_{IC}$平均值为0.86 MPa$\cdot \sqrt{m}$,直槽切缝巴西圆盘实验得到的$K_{IC}$平均值为0.92 MPa$\cdot \sqrt{m}$,两类方法的统计平均值较为接近,页岩局部组成的非均质性使得微米力学测量结果较宏观测试更为分散. 研究结果可用于页岩宏观Ⅰ型断裂韧度预测,为有效解决页岩气储层水力压裂参数评价提供新的思路和方法.      

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.     

Mechanics of indentation of plastically graded materials—II: Experiments on nanocrystalline alloys with grain size gradients

A systematic study of depth-sensing indentation was performed on nanocrystalline (nc) Ni-W alloys specially synthesized with controlled unidirectional gradients in plastic properties. A yield strength gradient and a roughly constant Young's modulus were achieved in the nc alloys, using electrodeposition techniques. The force vs. displacement response from instrumented indentation experiments matched very well with that predicted from the analysis of Part I of this paper. The experiments also revealed that the pile-up of the graded alloy around the indenter is noticeably higher than that for the two homogeneous reference alloys that constitute the bounding conditions for the graded material. These trends are also consistent with the predictions of the indentation analysis.     

Evaluation of the stress–strain curve of metallic materials by spherical indentation

A method for deducing the stress–strain uniaxial properties of metallic materials from instrumented spherical indentation is presented along with an experimental verification.An extensive finite element parametric analysis of the spherical indentation was performed in order to generate a database of load vs. depth of penetration curves for classes of materials selected in order to represent the metals commonly employed in structural applications. The stress–strain curves of the materials were represented with three parameters: the Young modulus for the elastic regime, the stress of proportionality limit and the strain-hardening coefficient for the elastic–plastic regime.The indentation curves simulated by the finite element analyses were fitted in order to obtain a continuous function which can produce accurate load vs. depth curves for any combination of the constitutive elastic–plastic parameters. On the basis of this continuous function, an optimization algorithm was then employed to deduce the material elastic–plastic parameters and the related stress–strain curve when the measured load vs. depth curve is available by an instrumented spherical indentation test.The proposed method was verified by comparing the predicted stress–strain curves with those directly measured for several metallic alloys having different mechanical properties.This result confirms the possibility to deduce the complete stress–strain curve of a metal alloy with good accuracy by a properly conducted instrumented spherical indentation test and a suitable interpretation technique of the measured quantities.     

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.     

Effect of Varying Test Parameters on Elastic–plastic Properties Extracted by Nanoindentation Tests

A systematic experiment was performed in an effort to investigate how the levels of certain test parameters affect the values of elastic modulus, hardness, yield stress, and strain hardening constant obtained using nanoindentation test. Maximum applied load, loading (unloading) rate, and hold time at maximum load were varied at three levels. The effects of these testing parameters were investigated through a three-level, full factorial design of experiment. The experiments were conducted on ultrafine Al-Mg specimens that were mechanically extruded. Both longitudinal and transverse extrusion directions were examined to investigate effects of anisotropy on mechanical properties and evaluate the persistence of observed variations due to test parameters on different materials orientations. An indentation size effect (ISE) was observed demonstrating that maximum load—and thereby maximum indentation depth—can have a significant effect on values of hardness and elastic modulus. Hardness values decreased with higher loading rates, and higher rates of unloading resulted in higher values of elastic modulus (5–10 GPa increases). Strain-hardening exponent showed a decreasing trend with increasing loading rate while yield stress exhibited a consistent correlation to hardness across all studied parameters. The material exhibited very little creep during the hold period, and values of the calculated properties were not significantly altered by varying the length of the hold time. Anisotropy effect was observed, particularly in the values of yield strength. This is attributed to the preferred grain orientation due to extrusion.     

Viscoelastic solutions for conical indentation

The aim of indentation analysis is to link indentation data, typically an indentation force vs. indentation depth curve, P–h, to meaningful mechanical properties of the indented material. While well established for time independent behavior, the presence of a time dependent behavior can strongly affect both the loading and the unloading responses. The paper presents a framework of viscoelastic indentation analysis based on the method of functional equations, developed by Lee and Radok [1960, The contact problem for viscoelastic bodies, J. Appl. Mech. 27, 438–444]. While the method is restricted to monotonically increasing contact areas, we show that it remains valid at the very beginning of the unloading phase as well. Based on this result, it is possible to derive closed form solutions following the classical procedure of functional formulations of viscoelasticity: (1) the identification of the indentation creep function, which is the indentation response to a Heaviside load; and (2) a convolution integral of the load history over the indentation creep function. This is shown here for a trapezoidal loading by a conical indenter on three linear isotropic viscoelastic materials with deviator creep: the 3-parameter Maxwell model, the 4-parameter Kelvin–Voigt model and the 5-parameter combined Kelvin–Voigt–Maxwell model. For these models, we derive closed form solutions that can be employed for the back-analysis of indentation results from the loading and holding period and for the definition of unloading time criteria that ensure that viscous effects are negligible in the unloading response.     

The Modified Rockwell Test: A New Probe for Mechanical Properties of Metals

In the present work a novel methodology is proposed, based on the combination of the Rockwell and the Vickers tests, to provide estimates of the mechanical properties of metal substrates. The analysis is based on some novel invariants obtained from the finite element solution of the Vickers indentation (the imprint diagonal relates to the maximum indentation depth and the residual indentation depth with the average pressure and the elastic modulus). Several other useful results are discussed and experiments are performed with a modified Rockwell apparatus on steel and aluminium alloys. The results are important for the interpretation of micro indentation tests. Inverting the indentation data, reasonably accurate results can be obtained for strain hardening properties for “power law” behaviour, whereas more complex strain hardening would require further investigation.     

Determination of mechanical properties by instrumented indentation

The paper reviews the current state of the depth-sensing indentation (sometimes called nanoindentation), where the information on material behaviour and properties is obtained from the indenter load and depth, measured continuously during loading and unloading. It is shown how the contact parameters and principal characteristics are determined using pointed or spherical indenters. Indentation tests can be used for the measurement of hardness and elastic modulus, and also of the yield stress and for the construction of stress–strain diagrams, for the determination of the work of indentation and its components. Most devices use monotonic loading and unloading, but some also enable measurement under a small harmonic signal added to the basic monotonously increasing load. This makes possible continuous measurement of contact stiffness and the study of dynamic properties and the determination of properties of coatings. One section is devoted to the measurement on viscoelastic-plastic materials, where the delayed deforming must be considered during the measurement as well as in data evaluation. Instrumented indentation can also be used for the study of creep under high temperatures. The paper also discusses the errors arising in depth-sensing measurements and informs briefly about some other possibilities of the method.