Fracture force analysis at the interface of Pd and SrTiO3

The objective of this work is to develop an experimental indentation based method to determine the fracture force at the interface of Pd thin films and SrTiO₃ perovskite substrate. This paper reports on the results obtained for indentation into Pd thin films which were deposited in various thicknesses from 20 nm to 200 nm under vacuum and 300 °C substrate temperature by an electron beam physical vapor deposition. Initially, the relation between grain size, elastic module and hardness was considered as a function of film thickness. Thereafter, in developing new method, oscillating indentation was performed with different applied forces and oscillating times in order to measure the critical fracture force in each thickness. The effect of oscillating time on plastically deformed regions surrounding an indentation was schematically explained in conjunction with variation of oscillating time to determine the interfacial properties of the Pd thin film. Furthermore, the accuracy of the critical fracture force was ensured by applied force versus piling up height plot. The method is validated experimentally for the soft thin films over the hard substrate. However, further study would be essential to measure the film adhesion by means of fracture force at the interface.     

Analysis of the substrate effects of strain-hardening thin films on silicon under nanoindentation

Mechanical properties of thin films on substrates can be evaluated directly through nanoindentation. For a comprehensive study, thin films should be characterized via Young’s modulus, yield stress and strain-hardening exponent at constant temperature. In this paper, we evaluate these effects of thin films on silicon substrate through finite element analysis. Thin films, from soft to hard relative to the silicon substrate, are investigated in three categories: soft films on hard substrates, soft to hard films on no elastic mismatch substrates, and hard films on soft substrates. In addition to examining the load-displacement curve, the normalized hardness versus normalized indentation depth is checked as well to characterize its substrate effect. We found that the intrinsic film hardness can be acquired with indentation depths of less than 12% and 20% of their film thickness for soft films on hard substrates and for soft to hard films on no elastic mismatch substrates, respectively. Nevertheless, nanoindentation of hard films on soft substrates cannot determine the intrinsic film hardness due to the fact that a soft substrate cannot support a hard film. By examining the von Mises stresses, we discovered a significant bending phenomenon in the hard film on the soft substrate. PACS 61.43.Bn; 62.20.-x; 68.03.Hj; 68.05.Cf; 68.08.De     

Regional stretch method to measure the elastic and hyperelastic properties of soft materials

Characterizing the mechanical properties of soft materials and biological tissues is of great significance for understanding their deformation behaviors. In this paper, a regional stretching method is proposed to measure the elastic and hyperelastic properties of a soft material with an adhesive surface or with the aid of glue. Theoretical and dimensional analyses are performed to investigate the regional stretch problem for soft materials that obey the neo-Hookean model, the Mooney-Rivlin model, or the Arruda-Boyce model. Finite element simulations are made to determine the expressions of the dimensionless functions that correlate the stretch response with the constitutive parameters. Thereby, an inverse approach is established to determine the elastic and hyperelastic properties of the tested materials. The regional stretch method is also compared to the indentation technique. Finally, experiments are performed to demonstrate the effectiveness of the proposed method.     

Geometry independence of the normalized relaxation functions of viscoelastic materials in indentation

The normalized relaxation modulus represents a salient feature of viscoelastic materials and its determination is of great significance for various applications. From the normalized relaxation modulus, for instance, one can derive the loss factor of a viscoelastic polymer and judge whether a material is suitable for damping applications or not. By using dimensional analysis and the elastic–viscoelastic correspondence principle, the normalized relaxation function of a linear viscoelastic material obtained from indentation relaxation tests is shown to depend only on the indentation load but not on the indenter geometry and the shape of the indented solid. The result could enable circumvention of the difficulties encountered in the calibration of the indenter geometry and the preparation of indented samples. Numerical simulations are performed on a number of cases of practical interest, including the spherical indentation test of a soft layer lying on a rigid substrate, a flat punch indenter indenting into a soft layer with a rough surface bonded to a rigid substrate, a rigid indenter with irregular shape indenting into a particle, inclined contact of a cylindrical indenter with a cylinder, and indentation of porous substrates. The numerical examples demonstrate that the conclusion from the theoretical analysis is valid for all these situations.     

Scaling relationships in sharp conical indentation of shape memory alloys

Based on dimensional analysis and finite element calculations, several scaling relationships in the indentation of shape memory alloys with a sharp conical indenter were obtained. These scaling relationships illustrate the dependence of the indentation response on the material properties of shape memory alloys, such as phase transition and plastic deformation. It is shown that the yield stress and strain-hardening exponent of transformed martensite play important roles in the indentation response, in addition to the phase transition properties. Additionally, the general relationships between indentation hardness and phase transition stress, maximum transition strain, martensite yield stress and the strain-hardening exponent of shape memory alloys were obtained. The results show that the indentation hardness of shape memory alloys is not proportional to the phase transition stress or to the martensite yield stress, and cannot be used directly to measure the phase transition stress or the yield stress of shape memory alloys.     

Mechanical Characterization of Protein Crystals

The mechanical properties (critical stress intensity factor, hardness and Young's modulus) of 4 crystalline materials (two proteins, lysozyme and glucose isomerase and two non‐proteins, glutamic acid and potassium sulphate) were measured with an indentation technique. It was found that the mechanical properties of lysozyme crystals depend on their state – dried, partly dried and moisture saturated – and their surroundings. The hardness, Young's modulus and the critical stress intensity factor of lysozyme crystals were observed to be much lower than those for the tested non‐proteins, leading to the conclusion that crystalline lysozyme is comparatively more fragile and softer. In combination the mechanical properties of lysozyme and the non‐proteins indicated that these materials were fairly brittle. Mechanical properties for crystals of the other protein, glucose isomerase, could not be quantified by indentation. However, qualitatively crystalline glucose isomerase was found to be more ductile and less fragile than crystalline lysozyme. The experimental findings were interpreted in terms of relative susceptibility to attrition and secondary nucleation in stirred industrial crystallizers.     

应力预释放对单晶硅片的压痕位错滑移的影响

单晶硅片的压痕位错在一定温度下的滑移距离反映了硅片的机械强度. 压痕位错的滑移是受压痕的残余应力驱动的, 因此研究残余应力与位错滑移之间的关系具有重要的意义. 本文首先采用共聚焦显微拉曼术研究了单晶硅片压痕的残余应力经过300或500 ℃ 热处理后的预释放, 然后研究了上述应力预释放对压痕位错在后续较高温度(700–900 ℃)热处理过程中滑移的影响. 在未经应力预释放的情况下, 压痕位错在700–900 ℃热处理2 h后即可滑移至最大距离. 当经过上述预应力释放后, 位错在900 ℃热处理2 h后仍能达到上述最大距离, 但位错滑移速度明显降低; 而在700和800 ℃时热处理2 h后的滑移距离变小, 其减小幅度在预热处理温度为500 ℃时更为显著. 然而, 进一步的研究表明: 即使经过预应力释放, 只要足够地延长700和800 ℃ 的热处理时间, 位错滑移的最大距离几乎与未经预应力释放情形时的一样. 根据以上结果, 可以认为在压痕的残余应力大于位错在某一温度滑移所需临界应力的前提下, 压痕位错在某一温度滑移的最大距离与应力大小无关, 不过达到最大距离所需的时间随应力的减小而显著增长.     

Indentation behaviour of superelastic hard carbon

Superelastic hard carbon particles widely varying in structure and properties have been studied by instrumented microindentation technique. The carbon particles up to 200 μm in size were produced by fullerene collapse upon high-pressure high-temperature treatment of metal–fullerene powder mixture with simultaneous sintering of metal matrix composite materials (CM) reinforced by the particles. The structure and properties of the carbon particles were controlled by changing synthesis parameters and the state (composition and structure) of the parent fullerite crystals. The specific features of the instrumented indentation behaviour of the particles were studied as a function of their hardness. Mechanical properties of the particles tested at loads of up to 1970 mN exhibit an indentation size effect, which becomes more pronounced with increasing hardness of the carbon particles. Upon holding at a constant load, the fullerene-derived carbon particles undergo unrecoverable deformation, and the indentation creep C_IT increases with increasing particle hardness. An increase in hardness of the reinforcing carbon particles substantially improves the wear resistance of the CM and decreases their friction coefficient.     

Theoretical study on nanoindentation hardness measurement of a particle embedded in a matrix

The finite element method was used to simulate indentation tests on a particle embedded in a matrix, to investigate the influence of the properties of the particle and the matrix, and the indentation depth on the measured hardness. The particle’s work-hardening exponent and the mismatch in particle and matrix yield strength have a significant influence on the measured hardness. A particle-dominated indentation depth was identified, within which the measured nanoindentation hardness agrees very well with the true hardness of the particle material. Numerical results from the simulations of a wide range of material properties determined that the measured hardness is within 5% difference of the particle’s true hardness when the indentation depth is less than 13.5% of the particle’s radius. The results can be used in practice as a guideline to measure the hardness of a particle embedded in a matrix and provides the theoretical basis to develop a particle-embedded method to measure the hardness of individual particles.     

Indentation on one-dimensional hexagonal quasicrystals: general theory and complete exact solutions

This paper presents a general account of the indentation responses of a one-dimensional hexagonal quasicrystal half-space pressed by an axisymmetric rigid punch. Based on Green's functions of the half-space subjected to point sources on the surface, the mixed boundary value problem is transformed to integral equations and solved exactly using the results of the potential theory method. Explicit expressions for the generalised pressures and indentation forces are derived for three common indenters (cylinder, cone and approximate sphere) in a systematic manner. For conical and spherical indenters, relations between the contact radius and indentation loads are determined. The coupling phonon–phason fields in the half-space under indentation are accurately expressed in terms of elementary functions. Numerical calculations are performed and discussions on related physical phenomena are given. The present exact solutions can serve as benchmarks for approximate or numerical analyses and can guide the experimental characterisation of material properties of quasicrystals.     

聚氰丙基甲基硅氧烷—聚脲嵌段共聚物的NMR表征及研究

用高分辨NMR对聚甲基硅氧烷-聚脲嵌段共聚物以及聚氰丙基甲基硅氧烷-聚脲嵌段共聚物结构进行表征,对NH形成的各种氢键进行详细的研究,同时观察了氢键在力学性能中的作用,结果发现氢键强烈地影响着力学性能。用固体~1H宽线研究这类材料的相分离状况,并总结影响相分离的因素。保持硬段含量不变,增加软段分子量使相分离程度增加;保持软段分子量不变,增加硬段含量使相分离程度降低。软、硬段之间的相互作用(如氢键)使相分离程度降低。     

Numerical simulation of flat-tip micro-indentation of glassy polymers: Influence of loading speed and thermodynamic state

Flat-tip micro-indentation tests were performed on quenched and annealed polymer glasses at various loading speeds. The results were analyzed using an elasto-viscoplastic constitutive model that captures the intrinsic deformation characteristics of a polymer glass: a strain-rate dependent yield stress, strain softening and strain hardening. The advantage of this model is that changes in yield stress due to physical aging are captured in a single parameter. The two materials studied (polycarbonate (PC) and poly(methyl methacrylate) (PMMA)) were both selected for the specific rate-dependence of the yield stress that they display at room temperature. Within the range of strain rates experimentally covered, the yield stress of PC increases linearly with the logarithm of strain rate, whereas, for PMMA, a characteristic change in slope can be observed at higher strain rates. We demonstrate that, given the proper definition of the viscosity function, the flat-tip indentation response at different indentation speeds can be described accurately for both materials. Moreover, it is shown that the model captures the mechanical response on the microscopic scale (indentation) as well as on the macroscopic scale with the same parameter set. This offers promising possibilities of extracting mechanical properties of polymer glasses directly from indentation experiments.     

聚氰丙基甲基硅氧烷-聚脲嵌段共聚物的NMR表征及研究

用高分辨NMR对聚甲基硅氧烷-聚脲嵌段共聚物以及聚氰丙基甲基硅氧烷-聚脲嵌段共聚物结构进行表征,对NH形成的各种氢键进行详细的研究,同时观察了氢键在力学性能中的作用,结果发现氢键强烈地影响着力学性能。用固体¹H宽线研究这类材料的相分离状况,并总结影响相分离的因素。保持硬段含量不变,增加软段分子量使相分离程度增加;保持软段分子量不变,增加硬段含量使相分离程度降低。软、硬段之间的相互作用(如氢键)使相分离程度降低。     

Measurement of Residual Stresses Using Nanoindentation Method

Instrumented indentation, which is also known as nanoindentation or depth-sensing indentation, is increasingly being used to probe the residual stresses of materials including bulk solids, thin films, and coatings. The residual stresses are proved to have significant effects on various nanoindentation parameters such as hardness, loading curve, unloading curve, pile-up amount around indentation, and true contact area. By analyzing these parameters, numerous methods are developed to evaluate the residual stresses of materials in recent years. This article reviews six commonly used models which determine residual stresses from analyzing load-depth curves, as well as indentation fracture technique which is based on the classical fracture mechanics. Emphasis is placed on the principle, application and limitation of each nanoindentation method.     

Mechanics of plastic flow past a narrow-angle wedge indenter

ABSTRACT

The indentation of a metal specimen by a narrow-angle wedge produces extreme plastic deformation, with an effect akin to cutting into the metal. Simulation of such processes is challenging, and complicated by the need to model material separation along the indentation symmetry axis. Here we use an Arbitrary Lagrangian Eulerian (ALE) framework to enforce the symmetry boundary conditions (bcs) in their original, `strong’ form, as well as conventional Lagrangian FE to impose the bcs in a complementary, `weak’ form. Taken together these two cases, representing perfectly strong and perfectly weak interfaces, produce accurate bounds on the mechanical response for indentation by wedges with semi-apical angles as small as 15 degrees, and encompass intermediate cases that would require complicated models of ductile failure. The method accurately predicts the transition from the cutting pattern to the non-cutting (radially compressive) pattern as the apical angle is increased. In combination with Lagrangian particle tracking, the simulations reveal the deformation pattern as well as strain, strain-rate, and velocity fields in narrow angle indentation at high resolution. Interestingly, the strong form predicts a thin (tens of microns), near-wall layer of intense plastic strain, which has been observed recently in indentation experiments. With the exception of this feature, the strong and weak bc solutions are quite similar. The present approach reveals insights about plastic flow past narrow obstacles in a range of related problems including cone penetration and machining, and suggests using narrow-angle indentation as a way to probe material failure.     

Calculation of the thicknesses and elastic properties of thin-film coatings using atomic-force acoustic microscopy data

The feasibility of applying atomic-force acoustic microscopy to measure the elastic properties of thin-film coatings and their thickness in the range from several to several hundreds of nanometers is studied. In practice, this technique can be used to study diamond-like coatings. The key point of our method is application of “flat” tips, which provide a constant tip-surface contact area and, hence, a constant contact stiffness. The reason for using such tips is that experimental data for thin-film structures gained with standard (rounded) tips cannot be given an adequate quantitative interpretation. Numerical simulation is used to evaluate the thickness and indentation modulus of a coating from contact stiffness k _cont measured by atomic-force acoustic microscopy.     

基于激光技术的压痕应变花及测试应变的原理

介绍了一种用于测试面内三个应变分量的应变测量技术,在试件表面预先压制三个压痕,通过激光照射压痕,经衍射后干涉,产生干涉图。通过分析变形前后干涉斑点的光强值的变化来对待测位置进行应变测量。实验表明该方法对待测试件表面损伤小,且压痕应变花尺寸小,是一种新的光学应变测试技术,不仅可以用来进行普通应变测量,尤其对解决小空间应变测试问题有其独特的优点。     

Indentation of transversely isotropic power-law hardening materials: computational modelling of the forward and reverse problems

Using a combination of dimensional analysis and large deformation finite element simulations of triple indentations of 120 materials, a framework for capturing the indentation response of transversely isotropic materials is developed. By considering 4800 combinations of material properties within the bounds of the original set of 120 materials, forward algorithms that predict the indentation response of materials and reverse algorithms that predict the materials’ elastic and plastic properties from experimentally measured indentation responses are formulated for both longitudinal and transverse indentations. Issues of accuracy, reversibility, uniqueness and sensitivity within the context of the indentation of transversely isotropic materials are addressed carefully. Using 1400 combinations of material properties, it is demonstrated that there is perfect reversibility between the material properties and their indentation responses as predicted by the forward and reverse algorithms. On average, the differences between the results of the finite element analysis and those predicted by the forward algorithms for longitudinal or transverse indentations are less than 1%, thus demonstrating the high accuracy and uniqueness of the forward analysis. For longitudinal and transverse indentations, the reverse algorithms provide accurate results in most cases with an average error of 3 and 6%, respectively. A sensitivity analysis with a ±2% variation in the material properties in the forward algorithm and ±2% variation in the indentation responses in the reverse algorithms demonstrated the robustness of the algorithms developed in the present study, with the longitudinal indentations providing relatively less sensitivity to variability in indentation responses as compared to the transverse indentations.     

Development of an improved energy-based method for residual stress assessment

In this study, an improved energy-based method is proposed to measure the equi-biaxial residual stress of bulk materials using spherical indentation. Through analysis of the load–depth curve and residual indentation profile, two calculation methods of the energy of residual stress are proposed, one of which is determined from the load–depth curve and the other based on the Hertizan theory. Finite element analysis was used to establish their relationship, which is the function of the residual stress and material parameters. According to reverse analysis, the proposed method can be used to quickly and effectively determine residual stress. To verify the model, indentation experiments were performed using a ZHU0.2/Z2.5 testing machine. A comparison with conventional X-ray diffraction results showed that the improved method is suitable for the quantitative assessment of residual stress in industrial facilities.     

Mapping of Two-Dimensional Contact Problems on a Problem with a One-Dimensional Parametrization

We discuss a possible generalization of the ideas of the method of dimensionality reduction (MDR) for the mapping of two-dimensional contact problems (line contacts). The conventional formulation of the MDR is based on the existence and uniqueness of a relation between indentation depth and contact radius. In two-dimensional contact problems, the indentation depth is not defined unambiguously, thus another parametrization is needed. We show here that the Mossakovskii-Jäger procedure of representing a contact as a series of incremental indentations by flat-ended indenters can be carried out in two-dimensions as well. The only available parameter of this process is, however, the normal load (instead of indentation depth as in the case of threedimensional contacts). Using this idea, a complete solution is obtained for arbitrary symmetric two-dimensional contacts with a compact contact area. The solution includes both the relations of force and half-width of the contact and the stress distribution in the contact area. The procedure is generalized for adhesive contacts and is illustrated by solutions of a series of contact problems.