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.     

利用纳米硬度试验法确定Cr/Cu梯度材料的变形特性

利用纳米硬度仪研究了在Cu基底上的Cu／Cr梯度膜的机械性能。梯度膜是通过将Cu靶和Cr靶同时溅射到Cu基底材料上，但两个靶的相对溅射功率随溅射时间变化而制备。利用Oliver and Pharr方法得到了膜随其厚度变化的硬度和弹性模量。然后利用加载／卸载／再加载的方法得到了在不同深度(即膜的厚度)压头平均压力与相对压人深度之间的关系曲线，在此曲线上可以明显反映出材料的屈服特性。     

Size-dependent response of ultra-thin films with surface effects

A modified continuum model of elastic films with nano-scale thickness is proposed by incorporating surface elasticity into the conventional nonlinear Von Karman plate theory. By using Hamilton’s principle, the governing equations and boundary conditions of the ultra-thin film including surface effects are derived within the Kirchhoff’s assumption, where the effects of non-zero normal stress and large deflection are taken into account simultaneously. The present model is then applied to studying the bending, buckling and free vibration of simply supported micro/nano-scale thin films in-plane strains and explicit exact solutions can be obtained for these three cases. The size-dependent mechanical behavior of the thin film due to surface effects is well elucidated in the obtained solutions.     

Measurement of Mechanical Properties of Thin Film by Membrane Deflection Test

Micro-tensile properties of Au thin films were measured using a membrane deflection testing system. During the membrane deflection test, the deflection of the film was measured by an out-of-plane electronic speckle pattern interferometric (ESPI) system. From the measurement, the tensile loads and strains exerted on the membrane film during the deflection of the film could be determined. Quantitative analysis of the phase maps of the ESPI speckle patterns corresponding to the respective different deflection levels provided the deflection distribution along the testing section of the film. Test pieces were fabricated by electromachining process using 0.5 and 1. 0 μm thick Au films which were deposited on the silicon wafer by sputtering technique. Tensile properties, including elastic modulus, yield and tensile strength, were evaluated in the tensile stress-strain curve determined from the load-deflection relation. These properties were compared to those obtained from the micro-tensile tests. It was found that the yield and tensile strengths obtained from the deflection tests were lesser than those from the micro-tensile tests. Furthermore, the thickness effect, showing the increasing tendency of yield strength with decreasing thickness, was experimentally examined.     

Mechanical properties of ultrananocrystalline diamond thin films relevant to MEMS/NEMS devices

The mechanical properties of ultrananocrystalline diamond (UNCD) thin films were measured using microcantilever deflection and membrane deflection techniques. Bending tests on several free-standing UNCD cantilevers, 0.5 μm thick, 20 μm wide and 80 μm long, yielded elastic modulus values of 916–959 GPa. The tests showed good reproducibility by repeated testing on the same cantilever and by testing several cantilevers of different lengths. The largest source of error in the method was accurate measurement of film thickness. Elastic modulus measurements performed with the novel membrane deflection experiment (MDE), developed by Espinosa and co-workers, gave results similar to those from the microcantilever-based tests. Tests were performed on UNCD specimens grown by both micro and nano wafer-seeding techniques. The elastic modulus was measured to be between 930–970 GPa for the microseeding and between 945–963 GPa for the nanoseeding technique. The MDE test also provided the fracture strength, which for UNCD was found to vary from 0.89 to 2.42 GPa for the microseeded samples and from 3.95 to 5.03 for the nanoseeded samples. The narrowing of the elastic modulus variation and major increase in fracture strength is believed to result from a reduction in surface roughness, less stress concentration, when employing the nanoseeding technique. Although both methods yielded reliable values of elastic modulus, the MDE was found to be more versatile since it yielded additional information about the structure and material properties, such as strength and initial stress state.     

Nanomechanical Property and Nanowear Measurements for Sub-10-nm Thick Films in Magnetic Storage

In the magnetic storage industry, thin film carbon overcoats play a critical role in reducing magnetic and physical spacing between the recording slider and the rotating disk so that the information stored per unit area is maximized. Thin film carbon overcoats have been improved such that they exhibit higher hardness with lower thickness of few nanometers and still being able to perform reliably. In this paper, nanoindentation and nanoscratch techniques to measure nanomechanical properties, namely hardness, elastic modulus and shear strength of thin solid films were presented along with a recently developed high resolution force transducer. Nanowear behavior characterization techniques were also examined and were applied to commercially available magnetic disks to characterize their wear behavior. It was shown that the properties and wear behavior of sub-10-nm thick film carbon overcoats were reliably measured. These techniques could be applied to different thin solid films on substrates, and they are not restricted to magnetic storage systems.     

A continuum model for size-dependent deformation of elastic films of nano-scale thickness

Ultra-thin elastic films of nano-scale thickness with an arbitrary geometry and edge boundary conditions are analyzed. An analytical model is proposed to study the size-dependent mechanical response of the film based on continuum surface elasticity. By using the transfer-matrix method along with an asymptotic expansion technique of small parameter, closed-form solutions for the mechanical field in the film is presented in terms of the displacements on the mid-plane. The asymptotic expansion terminates after a few terms and exact solutions are obtained. The mid-plane displacements are governed by three two-dimensional equations, and the associated edge boundary conditions can be prescribed on average. Solving the two-dimensional boundary value problem yields the three-dimensional response of the film. The solution is exact throughout the interior of the film with the exception of a thin boundary layer having an order of thickness as the film in accordance with the Saint-Venant’s principle.     

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。     

Experimental Investigation of Strain Rate Dependence of Nanocrystalline Pt Films

A new microscale uniaxial tension experimental method was developed to investigate the strain rate dependent mechanical behavior of freestanding metallic thin films for MEMS. The method allows for highly repeatable mechanical testing of thin films for over eight orders of magnitude of strain rate. Its repeatability stems from the direct and full-field displacement measurements obtained from optical images with at least 25 nm displacement resolution. The method is demonstrated with micron-scale, 400-nm thick, freestanding nanocrystalline Pt specimens, with 25 nm grain size. The experiments were conducted in situ under an optical microscope, equipped with a digital high-speed camera, in the nominal strain rate range 10⁻⁶–10¹ s⁻¹. Full field displacements were computed by digital image correlation using a random speckle pattern generated onto the freestanding specimens. The elastic modulus of Pt, E = 182 ± 8 GPa, derived from uniaxial stress vs. strain curves, was independent of strain rate, while its Poisson’s ratio was v = 0.41 ± 0.01. Although the nanocrystalline Pt films had the elastic properties of bulk Pt, their inelastic property values were much higher than bulk and were rate-sensitive over the range of loading rates. For example, the elastic limit increased by more than 110% with increasing strain rate, and was 2–5 times higher than bulk Pt reaching 1.37 GPa at 10¹ s⁻¹.     

氧化铝多孔膜振动性能的实验研究

电化学氧化法制备的氧化铝多孔膜有六角规则密排的纳米孔,其优良的结构特点使其具有良好的用途,可应用于微粒物质分离,氧化剂的载体,微电子机械系统的组件和纳米器件等。在前期研究了这种氧化铝膜的力学性能如拉伸性能和弯曲性能的基础上,本文实验研究了这种氧化铝多孔膜的振动特性即共振频率特性和振动模态,估算了该氧化铝多孔膜的相当弹性模量,与其他方法测得的相当弹性模量基本一致。     

Gripless nanotension test for determination of nano-scale properties

This paper proposes a novel material testing method, gripless nanotension technique (GNT), to assess the basic mechanical properties of nano-scale structures in top-down processes. The GNT exhibits prominent advantages over conventional methods, i.e., use of a nanoindenter as a reliable and simple testing device, high-quality nano-scale metallic specimen with negligible residual stress, and tensile testing possible in the through-thickness direction. Using the proposed method, nano-scale polycrystalline specimens obtained from a nickel film were tested. Through the experiment, well-defined values of material properties with extraordinary phenomenal findings, i.e., strikingly reduced elastic modulus, yield strength and tensile strength of much higher values could be reliably observed and determined at the nano-scale.     

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 Discontinuous Elastic Interface Transfer Model of Thin Film Nanoindentation

A new model of thin film indentation that accounted for an apparent discontinuity in elastic strain transfer at the film/substrate interface was developed. Finite element analysis suggested that numerical values of strain were not directly continuous across the interface; the values in the film were higher when a soft film was deposited on a hard substrate. The new model was constructed based on this discontinuity; whereby, separate weighting factors were applied to account for the influence of the substrate in strain developed in the film and vice-versa. By comparing the model to experimental data from thirteen different amorphous thin film materials on a silicon substrate, constants in each weighting factor were found to have physical significance in being numerically similar to the bulk scale Poisson’s ratios of the materials involved. When employing these material properties in the new model it was found to provide an improved match to the experimental data over the existing Doerner and Nix and Gao models. Finally, the model was found to be capable of assessing the Young’s modulus of thin films that do not exhibit a flat region as long as the bulk Poisson’s ratio is known.     

考虑膜厚影响薄膜磁致伸缩系数、泊松比和杨氏模量的同时测量

基于经典层合板理论,建立了一个能同时测量薄膜-基底系统中薄膜的磁致伸缩系数、杨氏模量和泊松比的板模型.以前的研究计算薄膜磁致伸缩系数时,大多假设薄膜的弹性属性与相应的块材一致,由此导致的磁致伸缩系数计算是不准确的.在目前大多数方法中仅仅在使用一个单一的弹性各向同性基底中能够避免这个问题.该文模型在各向异性基底下同样适用,并且不要求薄膜的厚度远远小于基底厚度,因此也能够用来计算磁致伸缩应变和设计微电机械系统和生物微电机械系统.对已有的铁基非晶薄膜的实验数据,在不同磁场强度下,磁致伸缩系数的计算结果与已有模型进行了比较,它们之间的差异得到了解释.同时,还可以得到薄膜的弹性常数.     

激光冲击对氧化石墨烯薄膜的结构及力电性能影响

采用激光烧蚀氧化石墨烯薄膜,可实现其微尺度图案化加工,以应用于微纳米电子器件。但激光冲击下氧化石墨烯薄膜的结构及力、电性能变化直接影响了器件稳定性和可靠性。为研究超高应变率加载对氧化石墨烯薄膜的结构及性能的影响,采用不同功率激光冲击氧化石墨烯薄膜,通过对其表面形貌、化学成分表征揭示薄膜结构的改变机理,通过对薄膜冲击前后的硬度、弹性模量、导电率测试探索合理的激光加工参数。结果表明:在1.14 W功率的二氧化碳激光冲击下,可实现加工区氧化石墨烯薄膜的还原且不造成薄膜烧蚀断裂,其电导率可达到1.727×103 S/m,弹性模量为49.97 GPa,硬度为5.71 GPa。     

Micron-scale channel formation by the release and bond-back of pre-stressed thin films: A finite element analysis

Buckling of thin films on a rigid substrate during use or fabrication is a well-known but unwanted phenomenon. However, this phenomenon can also be exploited to generate well-controlled patterns at the micro and nano-scale. These patterned surfaces find various technological applications such as optical gratings or micro/nano-fluidic channels. In this article, we present a numerical model that accounts for the buckling-up of pre-strained thin films by a reduction of the interface toughness and the subsequent bond-back. Channels are formed whose dimensions can be controlled by tuning the film dimensions, film thickness and stiffness, the eigenstrain in the film and the cohesive interface energy between the film and the substrate. We will show how the buckling-up and draping back processes can be captured in terms of a limited set of dimensionless parameters, providing quantitative insight on how these parameters should be tuned to generate a specified channel geometry.     

Nanoindentation of polymeric thin films with an interfacial force microscope

The mechanical properties of interphase regions at bi-material interfaces can be quite different from the surrounding bulk materials. For composite materials, this interphase region is usually thin but plays an important role in their overall mechanical properties. Nanoindentation has become a commonly used experimental technique for measuring the mechanical properties of materials, especially when one of the dimensions is small. However, the extraction of reduced elastic modulus from the nanoindentation of thin films on substrates can pose challenges due to the influence of the substrate. In this study, the nanoindentation of thin films on substrates has been examined with a view to extracting the reduced modulus of thin polymer films.Thin films of (3-aminopropyl)triethoxysilane (C₉H₂₃NO₃Si, γ-APS) were deposited on silicon. An interfacial force microscope (IFM) was used to indent the γ-APS films. The effect of the substrate was studied by considering two very different thicknesses ( and ). The nanoindentation data were analyzed via contact mechanics theories and a finite element analysis that incorporated surface interactions. The analyses showed that nanoindentation experiments can provide reliable values of film modulus when the film is very different from the substrate. It was found that the commonly used rule of thumb that the indentation depth should be less than 10% of the thickness did not eliminate substrate effects for a wide range of material combinations. Instead, it is proposed that the contact radius should be less than 10% of the thickness so that contact mechanics theories for monolithic materials can be used without considering the presence of the substrate. The modulus of γ-APS polymer films and the surface energy between the tungsten tip of the IFM and γ-APS films were extracted and were related to their cure. A completely cured thick γ-APS film had a reduced modulus of . This value falls in the usual range for polymers due to the amorphous nature of the γ-APS films.     

Bulge Testing Transparent Thin Films with Moiré Deflectometry

The problem that is addressed here is the measurement of the mechanical properties of very thin, transparent films using bulge tests. All existing techniques make use of reflection from the film surface, but they can be difficult or impossible to apply to very thin, transparent films. Consequently, a novel approach based on the formation of a lens structure and using transmitted light is developed. In this technique, the focal length of the lens structure formed by the bulged film and the pressurizing medium is determined by moiré deflectometry with a corrected governing equation. The resulting curvature of the bulge film is used in the stress analysis of the bulge-test. By combining circular and rectangular configurations, the Young’s modulus and Poisson’s ratio of a 3 μm PET film were 4.65 ± 0.11 GPa and 0.34 ± 0.01, respectively. Consistent residual stresses were obtained from both configurations.     

Multi-layer thin films/substrate system subjected to non-uniform misfit strains

Current methodologies used for the inference of thin film stress through curvature measurement are strictly restricted to stress and curvature states that are assumed to remain uniform over the entire film/substrate system. These methodologies have recently been extended to a single layer of thin film deposited on a substrate subjected to the non-uniform misfit strain in the thin film. Such methodologies are further extended to multi-layer thin films deposited on a substrate in the present study. Each thin film may have its own non-uniform misfit strain. We derive relations between the stresses in each thin film and the change of system curvatures due to the deposition of each thin film. The interface shear stresses between the adjacent films and between the thin film and the substrate are also obtained from the system curvatures. This provides the basis for the experimental determination of thin film stresses in multi-layer thin films on a substrate.