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. (c) 2006 Elsevier Ltd. All rights reserved.

宏观深度测量压入仪器的研制

基于深度测量压入方法,以材料试验机Instron 5848 Microtester作为加载平台,外接高分辨力位移传感器,设计专用夹具,开发出该材料试验机的宏观压入功能.研究发现:对于机架柔度,无需再进行修正;对于压针接触面积,可用相关的方法计算.采用Oliver-Pharr方法处理测试数据,可获得材料的硬度和弹性模量.为了验证试验的可靠性,选用5种典型金属材料,将宏观压入测试结果与MTS Nano Indenter(R) XP测试结果进行对比,二者基本一致,其分散性均在10%以内.显示了开发传统材料试验机宏观压入测试功能的可行性

微桥结构Ni膜杨氏模量和残余应力研究

采用MEMS(MicroelectromechanicalSystems)技术研制了镍(Ni)膜微桥结构试样,应用陶瓷压条为承力单元,与纳米压痕仪XP系统的Berkovich三棱锥压头相结合,解决了较宽Ni膜微桥加载问题。测量了微桥载荷与位移的关系,并结合微桥力学理论模型得到了Ni膜微桥的杨氏模量及残余应力,其值分别为190.5GPa和146MPa,与应用纳米压痕仪直接测得的带有Si基底的Ni膜杨氏模量186.8±7.34GPa相吻合。

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=O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≠O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．

微桥结构铜膜杨氏模量和残余应力研究

采用MEMS(MicroelectromechanicalSystems)技术研制了铜 (Cu)膜微桥结构试样 ,应用陶瓷压条为承力单元 ,并与纳米压痕仪XP系统的Berkovich三棱锥压头相结合 ,解决了较宽Cu膜微桥加载问题。测量了微桥载荷与位移的关系 ,并结合微桥力学理论模型得到了Cu膜微桥的杨氏模量及残余应力 ,其值分别为 115 .2GPa和 19.3MPa ,与应用纳米压痕仪直接测得的带有Si基底的Cu膜杨氏模量 110± 1.6 7GPa相吻合。

Methods of Obtaining Instantaneous Modulus of Viscoelastic Solids Using Displacement-Controlled Instrumented Indentation with Axisymmetric Indenters of Arbitrary Smooth Profiles

We derive a relationship between the initial unloading slope, contact depth, and the instantaneous relaxation modulus for displacement-controlled indentation in linear viscoelastic solids by a rigid indenter with an arbitrary axisymmetric smooth profile. While the same expression is well known for indentation in elastic and in elastic-plastic solids, we show that it is also true for indentation in linear viscoelastic solids, provided that the unloading rate is sufficiently fast. When the unloading rate is slow, a "hold" period between loading and unloading can be used to provide a correction term for the initial unloading slope equation. Finite element calculations are used to illustrate the methods of fast unloading and "hold-at-the-maximum-indenter-displacement" for determining the instantaneous modulus using spherical indenters.

CHARACTERIZATION OF SHEAR BANDS IN TWO BULK METALLIC GLASSES WITH DIFFERENT INHERENT PLASTICITY

Shear banding characterization of Zr64.13Cu15.75Ni10.12Al10 and Zr65Cu15Ni10Al10 bulk metallic glasses (BMGs) with significant difference in inherent plasticity and quite similar chemical composition was studied by depth sensitive macroindentaion tests with conical indenter. Well-developed shear band pattern can be found for both BMGs after indentation. Distinct difference in the shear band spacing, scale of plastic deformation region and the shear band branching in the two BMGs account for the different plasticity.

The effects of capillary force in micro or nano-indentation

Models describing wet adhesion between indenters and substrates joined by liquid bridges are investigated. The influences of indenter shapes and various parameters of structures on capillary force are focused. In the former, we consider several shapes, such as conical, spherical and truncated conical indenter with a spherical end. In the latter, the effects of the contact angle, the environmental humidity, the gap between the indenter and the substrate, etc. are included. Different dependences of the capillary force on the indenter shapes and the geometric parameters are observed. Most interesting finding is that applying the present results to micro- and nano-indentation experiments shows the size effect in indentation hardness not produced but underestimated by the effects of capillary force.(4 refs)

Analysis of micro-indentation problem of a soft film on a hard substrate

Two stages have been observed in micro-indentation experiment of a soft film on a hard substrate. In the first stage, the hardness of the thin film decreases with increasing depth of indentation when indentation is shallow; and in the second stage, the hardness of the film increases with increasing depth of indentation when the indenter tip approaches the hard substrate. In this paper, the new strain gradient theory is used to analyze the micro-indentation behavior of a soft film on a hard substrate. Meanwhile, the classic plastic theory is also applied to investigating the problem. Comparing two theoretical results with the experiment data, one can find that the strain gradient theory can describe the experiment data at both the shallow and deep indentation depths quite well, while the classic theory can't explain the experiment results.

微尺度压痕实验的数值模拟及相关问题研究

目前国际上占主导地位的纳米压痕技术是由Oliver与Pharr提出并发展,目前的纳米压痕可以给出整个加、卸载过程的载荷—位移曲线以及硬度与弹性模量随压痕深度变化的曲线,从而提供了丰富的、比较精确的信息,为利用它探索材料比较完整的力学特性提供了可能.为达到该目的,就必须对压痕实验的加、卸过程进行较为深入的研究.作为主要的研究工具,有限元方法模拟微压痕过程在探讨通过实验数据得到更多、更准确的材料表层力学性能参数以及解释实验现象等方面发挥着重要作用.基于计算机速度与容量的原因,较早进行微压痕过程有限元模拟的BhattacharyaandNix、LaursenandSino都使用圆锥压头模拟维氏显微硬度标准正四棱锥Vicker压头与纳米压痕仪标准正三棱锥Berkovich压头,因为圆锥压头具有旋转对称性,可用二维旋转对称单元(二维实体单元)进行计算从而降低计算规模.即便如此,以当时大型计算机的水平,对规模为400~2000个四节点矩形单元的有限元模型进行一次完整的加、卸载过程也需要1~2天.到目前为止,微尺度压痕实验的数值模拟沿用二维模型.事实上,由于加工工艺的限制,微尺度压痕仪的压头如Berkovich与Vicker压头均不个旋转对称性;就微观尺度而言,实际的表层材料都是非均匀的.这些特征均不能由二维模拟体现,所以该文首先建立三维有限元模型,模拟带滑动接触的微尺度压痕加、卸载过程.在此基础上重点讨论了压头几何效应的问题,如二维模拟与三维模拟的关系、显微硬度与纳米的压痕硬度的关系、不同压头下材料的应力应变场、压痕间距与压痕边界的效应等,最后针对微尺度压痕实验中出现的压痕硬度随压痕深度减小而升高的现象,讨论了影响不同压痕深度硬度值的因素.

Characterization Of Shear Bands In Two Bulk Metallic Glasses With Different Inherent Plasticity

Shear banding characterization of Zr64.13Cu15.75Ni10.12Al10 and Zr65Cu15Ni10Al10 bulk metallic glasses (BMGs) with significant difference in inherent plasticity and quite similar chemical composition was studied by depth sensitive macroindentaion tests with conical indenter. Well-developed shear band pattern can be found for both BMGs after indentation. Distinct difference in the shear band spacing, scale of plastic deformation region and the shear band branching in the two BMGs account for the different plasticity.

The elastic-plastic indentation response of a columnar thermal barrier coating

Thermal barrier coatings with a columnar microstructure are prone to erosion damage by a mechanism of surface cracking upon impact by small foreign particles. In order to explore this erosion mechanism, the elastic indentation and the elastic-plastic indentation responses of a columnar thermal barrier coating to a spherical indenter were determined by the finite element method and by analytical models. It was shown that the indentation response is intermediate between that of a homogeneous half-space and that given by an elastic-plastic mattress model (with the columns behaving as independent non-linear springs). The sensitivity of the indentation behaviour to geometry and to the material parameters was explored: the diameter of the columns, the gap width between columns, the coefficient of Coulomb friction between columns and the layer height of the thermal barrier coating. The calculations revealed that the level of induced tensile stress is sufficient to lead to cracking of the columns at a depth of about the column radius. It was also demonstrated that the underlying soft bond coat can undergo plastic indentation when the coating comprises parallel columns, but this is less likely for the more realistic case of a random arrangement of tapered columns. © 2009 Elsevier B.V.

Estimating material elasticity by spherical indentation load-relaxation tests on viscoelastic samples of finite thickness

A two-step viscoelastic spherical indentation method is proposed to compensate for 1) material relaxation and 2) sample thickness. In the first step, the indenter is moved at a constant speed and the reaction force is measured. In the second step, the indenter is held at a constant position and the relaxation response of the material is measured. Then the relaxation response is fit with a multi-exponential function which corresponds to a three-branch general Maxwell model. The relaxation modulus is derived by correcting the finite ramp time introduced in the first step. The proposed model takes into account the sample thickness, which is important for applications in which the sample thickness is less than ten times the indenter radius. The model is validated numerically by finite element simulations. Experiments are carried out on a 10% gelatin phantom and a chicken breast sample with the proposed method. The results for both the gelatin phantom and the chicken breast sample agree with the results obtained from a surface wave method. Both the finite element simulations and experimental results show improved elasticity estimations by incorporating the sample thickness into the model. The measured shear elasticities of the 10% gelatin sample are 6.79 and 6.93 kPa by the proposed finite indentation method at sample thickness of 40 and 20 mm, respectively. The elasticity of the same sample is estimated to be 6.53 kPa by the surface wave method. For the chicken breast sample, the shear elasticity is measured to be 4.51 and 5.17 kPa by the proposed indentation method at sample thickness of 40 and 20 mm, respectively. Its elasticity is measured by the surface wave method to be 4.14 kPa. © 2011 IEEE.

Size effects in the conical indentation of an elasto-plastic solid

The size effect in conical indentation of an elasto-plastic solid is predicted via the Fleck and Willis formulation of strain gradient plasticity (Fleck, N.A. and Willis, J.R., 2009, A mathematical basis for strain gradient plasticity theory. Part II: tensorial plastic multiplier, J. Mech. Phys. Solids, 57, 1045-1057). The rate-dependent formulation is implemented numerically and the full-field indentation problem is analyzed via finite element calculations, for both ideally plastic behavior and dissipative hardening. The isotropic strain-gradient theory involves three material length scales, and the relative significance of these length scales upon the degree of size effect is assessed. Indentation maps are generated to summarize the sensitivity of indentation hardness to indent size, indenter geometry and material properties (such as yield strain and strain hardening index). The finite element model is also used to evaluate the pertinence of the Johnson cavity expansion model and of the Nix-Gao model, which have been extensively used to predict size effects in indentation hardness. © 2012 Elsevier Ltd.

Multi-scale permeability of murine bone measured by nanoindentation

The determination of lacunar-canalicular permeability is essential to understand the mechano-transduction mechanism of bone. Murine models are widely used to investigate skeletal growth and regulation, but the value of lacunar-canalicular permeability is still unclear. To address this question, a poroelastic analysis based on nanoindentation data was used to calculate the lacunar-canalicular permeability of wild type C57BL/6 mice of 12 months. Cross-sections of three tibiae were indented using spherical fluid cell indenter tips of two sizes. Results suggest that the value of lacunar-canalicular intrinsic permeability of B6 female murine tibia is in the order of 10 -24 m2. The distribution of the values of intrinsic permeability suggests that with larger contact sizes, nanoindentation alone is capable of capturing the multi-scale permeability of bone. Multi-scale permeability of bone measured by nanoindentation will lead to a better understanding of the role of fluid flow in mechano-transduction. © 2013 American Society of Civil Engineers.