基于原子力显微镜的薄膜原位压痕力学性能研究

基于原子力显微镜(AFM)和扫描电子显微镜(SEM)建立了一套原位纳米压痕测试系统。该系统可以实现控制带有金刚石(Cube corner)压头的AFM微悬臂梁对样品进行压入实验,并得到载荷-位移曲线,同时可以对压痕过程进行原位SEM实时观察。发展了一种基于AFM微悬臂梁加载和原位SEM压痕图像分析的力学性能测试方法,通过测量压入最大载荷和原位SEM测量压痕残余面积得到塑性薄膜的硬度和弹性模量。利用此方法对磁控溅射硅衬底上纳米晶银薄膜进行了压痕实验,并与Nanoindenter G200型纳米压痕仪实验进行对比研究。结果表明,原位AFM压痕方法具有高的载荷和位移分辨率,可以实现纳牛至微牛级的压痕实验,通过测量压痕面积得到塑性薄膜的硬度值,减小了使用Oliver-pharr方法中软膜硬基底上凸起(Pile-up)效应的影响,计算结果也具有好的测试精度和可靠性。     

Effects of the substrate on the determination of thin film mechanical properties by nanoindentation

We examine the effects of the substrate on the determination of mechanical properties of thin films by nanoindentation. The properties of aluminum and tungsten films on the following substrates have been studied: aluminum, glass, silicon and sapphire. By studying both soft films on hard substrates and hard films on soft substrates we are able to assess the effects of elastic and plastic inhomogeneity, as well as material pile-up, on the nanoindentation response. The data set includes Al/glass and W/sapphire, with the film and substrate having nearly the same elastic properties. These systems permit the true contact area and true hardness of the film to be determined from the measured contact stiffness, irrespective of the effects of pile-up or sink-in. Knowledge of the true hardness of the film permits a study of the effects of the elastic modulus mismatch on the nanoindentation properties, using the measured contact stiffness as a function of depth of indentation.     

On the determination of residual stress and strain fields by sharp indentation testing.: Part II: experimental investigation

An experimental investigation has been carried out in order to study how residual stress and strain fields can be determined by sharp indentation testing. Aiming at a thorough understanding of the influence from general residual surface stress and strain fields on global indentation parameters, i.e. hardness and contact area, Vickers indentation tests have been performed on specimens first exposed to standard four-point bend (4PB) or single edge notch bend (SEN(B)) loading. The experimental results have been evaluated based on the findings in a parallel theoretical/numerical investigation and are compared with finite element simulations as well as with corresponding results taken from the literature. Good agreement between experiments and numerical results has been found, particularly in a situation with no or little plastic deformation due to preloading.     

Investigation of residual stress by the indentation method with the flat cylindrical indenter

Experiments and numerical simulations have been carried out to study residual stress of copper specimens by the identation method with a flat cylindrical indenter. Copper specimens were annealed at different temperatures for 35 min to obtain different residual stress levels. The experiments carried out on these specimens demonstrated the influence of residual stress on indentation behavior. The influence of annealing temperature on the elastic-plastic transition region is quite obvious. A method has been presented to determine material properties, such as elastic modulus and Poisson ratio. This method can also be applied to determine residual stress with the assumption of knowing the yield stress in advance. The advantage of this method is that it can avoid calculating the contact area. In the finite element modeling (FEM), residual stresses on copper specimens are simulated by preapplying stresses. The influence of residual stress on the indentation load-depth curves has been studied by FEM. There is good agreement between experimental and FEM numerical results. A numerical method has also been presented to determine residual stress. In addition, Mises stress and plastic distribution ahead of the indenter have also been studied to help us further understand the influence of residual stress.     

纳米压痕技术及其在薄膜/涂层体系中的应用

综述了纳米压痕技术的发展历程及其在薄膜领域的应用。介绍了当前实验室条件下主要采用的电磁驱动式纳米压痕仪的构造和工作过程。为了保证测试结果的准确性,要在合适的温度、湿度下进行压入实验,借助保载来消除一些可以避免的误差。阐述了压头的分类和选择原则,玻氏压头相比于维氏压头具有更小的中心线与棱面夹角,避免了尖端横刃对于压入结果准确性的影响,因此最常用的压头为玻氏压头;表征断裂韧性最合适的压头为立方角压头;表征微机电系统的弯曲采用楔形压头。总结了通过最大载荷和压入面积得到涂层力学参量的分析流程。归纳了将纳米压痕法应用于表征薄膜涂层的硬度和弹性模量、室温下蠕变性能、断裂韧性、残余应力、塑性性能等力学量的研究,如表征硬度和弹性模量的Oliver-Pharr法的应用,识别蠕变柔量的Lee-Radok模型的应用,分析断裂韧性的Lawn-Evans-Marshall模型的应用。在涂层制备过程中,制备参数的改变可以使得涂层具有不同的力学性能,涂层厚度远小于表面尺寸,硬度和弹性模量仍然存在各向异性,非晶态结构涂层具有更高的硬度和弹性模量。采用碳纳米管强化可以提高涂层的断裂韧性,涂层内存在适量的残余应力数值和合...     

Determination and Relaxation of Residual Stress in 2024 Al-30 vol.% Magnesium Borate Whisker Composites

Residual stresses in 30 vol.% magnesium borate whisker-reinforced 2024 aluminum matrix composites have been determined by a nanoindentation method which takes into consideration pile-up and sink-in effects on indentation contact depth. Owing to the thermal mismatch and the large difference in elasticity modulus between the Al matrix and MBO whiskers, tensile residual stress was introduced to Al matrix material during fabrication. It was found that the solution treatment reduced the tensile residual stress by producing interfacial component and dislocations in the composites. Cryogenic cooling released the stress via reversing the tensile residual stress to compression in the matrix, which was more effective than solution treatment to release the tension stress in the composites. The combination of the solution treatment and the cryogenic cooling provided the most effective procedure to release the residual stress in the composites, which reduced the tensile residual stress from 232.6 to 56.5 MPa, i.e., 76% reduction. Meanwhile, no cracks were observed in the composite when processed with such sudden thermal shocking.     

TA15钛合金中纳米压痕附近残余应力-应变场及几何必须位错密度的分布

结合纳米压痕及高分辨电子背散射衍射技术(EBSD)测定了TA15钛合金中α及β相的弹性模量和纳米硬度,揭示了纳米压痕附近应力-应变场及几何必须位错(GND)密度的非均匀分布情况.利用高分辨EBSD测试过程中同步保存的背散射电子衍射花样,并基于cross-correlation的处理方法,计算得出了纳米压痕附近区域的残余弹性应力-应变场分布.结合应变梯度场理论,计算分析了纳米压痕附近区域的几何必须位错密度分布,进而对合金的微观塑性变形机制进行了讨论与分析.结果表明,α相的弹性模量及纳米硬度分别为129.05 GPa和6.44GPa,而β相的相应值为109.80 GPa和4.29 GPa.纳米压痕附近区域的残余Mises应力呈现明显的非均匀分布并受到相邻较软β相的显著影响.压痕附近的低残余应力区域伴随有显著较高的<α>形和柱面型几何必须位错密度分布.     

On the effect of a general residual stress state on indentation and hardness testing

During indentation experiments, residual stresses are superimposed on the applied indentation stress field and influence the measurement of the volume of interest. The residual stress state can vary in magnitude and biaxiality, and the resultant error in the measured hardness is difficult to estimate. A prediction of the effect in the contact pressure with and without residual stresses is carried out by a new model that accounts for nonlinearities caused by the von Mises’ flow rule. The model can also be used for the correction of the effect of a general residual stress state on any further analysis of mechanical properties and stress–strain behaviour from the measured indentation data. The model provides an estimation of the measurement uncertainty when the stress ratio or the strength of the material is unknown – a situation that is a commonly encountered with hardness testing of thin films and welded materials.     

Indentation size effect on mechanical properties of HVOF sprayed WC based cermet coatings for a roller cylinder

The present paper concerns the determination of mechanical properties such as hardness, elastic modulus and yield strength of WC-based cermet coatings for a roller cylinder. With this regard, Co and Ni containing WC-based coatings were sprayed on Ni-Al deposited 316 L stainless steel substrates by using High Velocity Oxygen Fuel (HVOF) technique. These HVOF sprayed coatings were analyzed by Scanning Electron Microscopy (SEM) with an Energy Dispersive Spectroscopy (EDS) system attachment. Mechanical properties of the coatings were examined by Shimadzu Dynamic Ultra-micro hardness test machine in order to determine the Young's modulus through load-unload sensing analysis. In addition to mechanical investigation, hardness-depth and hardness-force curves of WC-based coatings were investigated. It was found that both of these characteristics exhibit significant peak load dependency. Experimental indentation studies were carried out to determine load-unload curves of WC-Co and WC-Ni based coatings under 300 mN, 350 mN, 400 mN and 450 mN applied peak loads. Hardness and Young's modulus of WC-based coatings were calculated from experimental indentation test data of samples. It has been observed that the hardness and Young's modulus of the coating depends on the contact area and indentation size. The originality of this study is to determine the indentation size effect and contact area variations on mechanical properties of HVOF sprayed WC-based coatings.     

低模量Ti6Al4V表面Ti(Al/Pt)N薄膜强化改性

为解决硬质薄膜因与软基体硬度和模量差较大导致的薄膜失效问题,提高硬质薄膜在Ti6Al4V(TC4)钛合金基体上的适应性,使用掺杂氮化钛（TiN）陶瓷薄膜对低模量Ti6Al4V合金表面强化。采用热丝增强等离子体磁控溅射技术在Ti6Al4V合金表面制备Ti(Al/Pt)N薄膜：包括本征TiN、Al&Pt掺杂TiAlN和TiAl(Pt)N薄膜。采用扫描电子显微镜、X-射线衍射仪、纳米压痕仪、洛氏硬度计和摩擦磨损测试仪分别表征三种薄膜组织形貌、能谱分析、相结构和内应力、纳米硬度和模量及耐磨性。结果表明：Al元素掺杂使TiN薄膜柱状晶细化,截面形貌柱状晶更致密;同时微量Pt掺杂后,截面断口呈韧性撕裂。本征TiN和TiAlN薄膜衍射峰图谱呈现TiN(111)取向,TiAl(Pt)N薄膜的衍射峰呈TiN(200)主峰位。Al元素掺杂使TiN薄膜晶格畸变增多,内应力从-13 MPa增大到-115 MPa,导致膜-基结合力恶化,洛氏压痕和摩擦磨损实验中均出现薄膜剥落。Pt掺杂后薄膜内应力降低到-66 MPa,在洛氏压痕试验中TiAl(Pt)N薄膜与基体结合良好,仅有少许环形裂纹。摩擦磨损试验中本...     

Indentation modulus and hardness of polyaniline thin films by atomic force microscopy

Polyaniline (PANI) thin films with different thicknesses have been deposited on indium tin oxide (ITO) coated glass substrates by electrochemical polymerization of the aniline monomer in H₂SO₄ aqueous solution. By using the tip of an atomic force microscopy (AFM) apparatus as an indenter, cantilever deflection versus sample vertical displacement curves have been acquired and analyzed for evaluating the contact stiffness, by using an approach analogous to that developed for standard depth sensing indentation (DSI) tests. After the calibration performed using a set of polymeric reference materials, indentation modulus and hardness of PANI films have been deduced as a function of the reached maximum penetration depth. By using a model originally proposed for the analysis of standard DSI measurements, indentation modulus and hardness values of only PANI are finally deduced from the corresponding apparent values measured for the film-substrate systems, although they have to be considered as semi-quantitative estimations, since the roughness of the films does not allow a certain determination of the local thickness in correspondence of the probed points.     

A critical assessment of indentation-based ductile damage quantification

This paper scrutinizes the reliability of indentation-based damage quantification, frequently used by many industrial and academic researchers. In this methodology, damage evolution parameters for continuum damage models are experimentally measured by probing the deformation-induced degradation of either hardness or indentation modulus. In this critical assessment the damage evolution in different sheet metals was investigated using this indentation approach, whereby the obtained results were verified by other experimental techniques (scanning electron microscopy, X-ray microtomography and highly sensitive density measurements), and by finite element simulations. This extensive experimental–numerical assessment reveals that the damage-induced degradation of both hardness and modulus is at least partially, but most likely completely, masked by other deformation-induced microstructural mechanisms (e.g. grain shape change, strain hardening, texture development, residual stresses and indentation pile-up). It is therefore concluded that hardness-based or modulus-based damage quantification methods are intrinsically flawed and should not be used for the determination of a damage parameter.     

WC-17Co粉末密度对涂层力学性能及残余应力的影响

选取3种不同密度的WC-17Co粉末,采用超音速火焰喷涂法制备厚度为0.3 mm的涂层。通过扫描电镜观察分析了3种涂层的孔隙率,采用压痕法测量了涂层的努氏硬度与弹性模量,同时采用剥层法对不同密度粉末制备的WC-17Co涂层残余应力进行了测试与计算。结果表明,涂层孔隙率随WC-17Co粉末密度的增大而增大,涂层的努氏硬度、弹性模量均随WC-17Co粉末密度的增大而减小。WC-17Co涂层内部存在的残余应力表现为压应力,且应力值随涂层厚度的增大而增加,在临近涂层-基体界面处迅速减小。涂层残余压应力最大值随WC-17Co粉末密度的增大而增加：粉末密度为11.52、12.86、13.49 g·cm^-3所制备的涂层残余应力最大值分别为-798、 -986和-1120 MPa。     

On the determination of residual stress and strain fields by sharp indentation testing.: Part I: theoretical and numerical analysis

Sharp indentation tests, presently represented by cone and Vickers indenters, are analysed theoretically and numerically in order to explore how equi-biaxial residual stress and strain fields can be determined from the global properties, i.e. the size of the contact area between indenter and material and the hardness, given by such tests. It is shown that the residual strain fields can be accurately correlated with the hardness value while residual stresses are related to the size of the contact area. The latter feature is explained by the fact that the size of the contact area is sensitive to elastic effects. The results are summarized in simple closed form relations, well-suited to be used in an experimental situation, and the range of validity for the resulting formulae is discussed. The predictions are compared with corresponding results taken from the literature and good agreement is found. An experimental scheme for determination of residual fields by indentation is also suggested.     

Thermomechanical properties of aluminum alkoxide (alucone) films created using molecular layer deposition

Nanometer-scale-thick, polymer-like coatings deposited using the molecular layer deposition (MLD) technique constitute a new class of materials. The modulus and hardness of aluminum alkoxide (“alucone”) films grown using either homobifunctional or heterobifunctional reactants were measured using nanoindentation. Because the coatings are brittle and possess a significant tensile film stress immediately after deposition, the influence of film stress on the indentation measurements was quantified using a numerical analysis protocol. The film stress and coefficient of thermal expansion for alucone were determined using the wafer curvature method. Film stress was found to stabilize within the first thermal cycle, demonstrating a repeatable hysteresis thereafter. Curvature/time measurements on coated microcantilever beams indicated that the most significant evolution in film stress for alucone occurred during the initial 2 weeks of storage in the ambient environment. The temporal behavior is attributed to the change in thickness and/or modulus of alucone, and is consistent with the film stress becoming more compressive over time. An encapsulating alumina film, coated using the atomic layer deposition technique, was found to suppress the evolution of stress within alucone. The studies here suggest that the alucones have a greater elastic modulus than traditional polymers, are at present quite brittle and are prone to environmental influence. The MLD technique, however, possesses a rich wealth of options that enable the modulus, adhesion and chemical stability of the coatings to be tailored.     

Numerical analysis of the contact stresses developed during the indentation of coated systems with substrates with orthotropic properties

Many works in the literature have analyzed the contact stresses developed during the indentation of coated systems. In general, the damage observed in systems with soft substrates is characterized by circular cone cracks that propagate at the edge of the indentations. In systems with soft substrates, recent works have also shown that the amount of substrate indentation pile-up presents direct relationship with a peak in radial stresses at film surface and, consequently, with the amount of indentation circular cracks.In this work, a series of finite element analyses was conducted to simulate the indentation of systems with an elastic film and an elastic-plastic substrate. Two values of film thickness were selected and, in each simulation, substrates were divided into two layers with different plastic properties. The layer on the bottom was considered isotropic and the layer attached to the film presented plastic properties along the loading direction (z) that were different from the plastic properties along the radial and tangential directions. Different ratios between axial and radial/tangential properties were considered.Results indicated that the amount of substrate pile-up and, consequently, the peak in radial stresses at film surface, could be significantly reduced in coated systems with substrates with orthotropic plastic properties.     

Deformation in a Zr57Ti5Cu20Ni8Al10 bulk metallic glass during nanoindentation

Nanoindentation experiments of a Zr₅₇Ti₅Cu₂₀Ni₈Al₁₀ bulk metallic glass were performed with indentation loads ranging from 200 to 2000 μN. Both the indentation hardness and the reduced contact modulus decreased with the increase in the indentation load due to the propagation of shear bands underneath the indenter – the occurrence of a softening effect. The ratio of the indentation hardness to the reduced contact stiffness was a function of the reciprocal of the indentation depth. Based on the concept of diffusion-induced stresses, a one-dimensional constitutive relation between the change of the excessive free volume and the flow stress was proposed. The indentation-size effect as observed in the indentation tests was explained through the consideration of the contribution of the strain gradient in the constitutive relation.     

20CrMnMo钢不同渗碳淬硬层深度的组织与应力分布

以三种渗碳淬硬层深度不同的20CrMnMo齿轮钢试样为研究对象,对其显微组织和硬度梯度进行检测,采用电化学剥层技术,借助X-350A型X射线应力仪,测量各试样深层渗碳淬硬层的残余应力及其分布,将硬度梯度与残余应力的分布进行对照,认为20CrMnMo钢渗碳淬硬层硬度小于400 HV1,均为残余压应力,之后才转换为残余拉应力,这一结果为确保齿面具有可靠的抗接触疲劳性能,合理地确定重载大模数齿轮有效硬化层深度提供技术支撑。     

Determination of tensile properties by instrumented indentation technique: Representative stress and strain approach

Tensile properties can be evaluated by defining representative stress and strain with the parameters obtained from instrumented indentation tests using a spherical indenter. The accuracy of this approach depends strongly on how the contact depth is analyzed and how the representative stress and strain are defined. The primary factors influencing the determination of contact depth, pile-up/sink-in and elastic deflection, were quantified by analyzing indentation morphology by finite element simulation; then plastic pile-up/sink-in behavior was formulated in terms of the strain-hardening exponent and the ratio of indentation depth to indenter radius. For the representative strain, the definition by tangent function was determined to be more appropriate for assessing tensile properties based on derived behaviors of the strain-hardening exponent. This approach was experimentally verified by comparing tensile properties of 10 metallic materials from uniaxial tensile tests and instrumented indentation tests.     

A new method for evaluating the plastic properties of materials through instrumented frictional sliding tests

Frictional normal contact probing methods involving instrumented, depth-sensing indentation can be used to estimate the mechanical properties of small-volume structures and materials such as thin films and components of micro-electro-mechanical systems. This paper describes a new method for estimating the plastic properties, i.e. the yield strength and strain hardening exponent, of ductile materials from the topography of scratches formed by a conical tip during an instrumented, depth-sensing frictional sliding test. The proposed reverse analysis (or inverse analysis) uses dimensionless functions derived from computational simulations to extract plastic properties from an instrumented scratch response performed on a standard, commercially available instrument. Sensitivity analysis indicates that an experimental error of 5% in the scratch hardness or the pile-up height induces an error of <22% in the estimated strain hardening exponent. Laboratory experiments illustrate how two aluminum alloy tempers of the same indentation hardness have significantly different pile-up as a result of different strain hardening. Comparative results between the frictional sliding test and traditional tensile tests showed reasonable agreement for a total of 11 metallic alloys evaluated. These results confirm the potential usefulness of the proposed method as an engineering tool to probe plastic properties of small-volume materials and confined structures where it is difficult to obtain reliable estimates of mechanical properties by other means.