An Investigation of Fatigue Characteristics of Copper Film

Tensile and fatigue behaviors of the copper film coated by tin (Sn) were investigated considering S-N relationships and scanning electron microscope (SEM) observation of fracture surfaces. The fatigue behavior was investigated considering the effect of load ratio, R. The specimen of 2000 μm width, 8000 μm length and 15.26 μm thickness was fabricated by etching process. Tensile properties were measured using the micro-tensile testing system and in-plane electronic speckle pattern interferometric (ESPI) system for measuring the tensile strain during the test. The fatigue tests of the film were carried out in load-control mode with 40 Hz at three different stress ratios of 0.05, 0.3 and 0.5. The S-N curves, including the slope of the curve and fatigue limit, at the respective stress ratios were obtained. These curves were dependent on the load ratio. Empirical relationships indicating the dependency of the fatigue limit and S-N curve on the load ratio were suggested in this study. SEM observation of the tensile fracture surface showed that the cross-sectional area of the testing section was necked in the direction of the film thickness (i.e. parallel to the substrate surface normal) and some ductile dimples in the fracture surface were present. The fracture of the copper film under cyclic loading was progressed in the transgranular fracture mode.     

Deformation measurement of conducting polythiophene thin films by an electronic speckle pattern interferometric method

The deformation measurement of electrosynthesized polythiophene (Pth) thin films is difficult because of the small thickness and high flexibility of the specimen. An electronic speckle pattern interferometry (ESPI) method is used to measure the deformation of Pth films of thicknesses in the range of 4–65 μm. Their stres-strain curve are obtained. It is found that the mechanical properties of Pth films are sensitive to the specimen thickness. The tensile strength increases with decreasing thickness of thin film from 10 μm. The influence of the electrochemical synthesis conditions on the mechanical properties of Pth films is also discussed. Project supported by the Basic-Research Foundation of Tsinghua University (JC2000057), and the Visiting Scholar Foundation of Solid Mechanical Key Lab in Tongji University of the Ministry of Education of China. Received 10 September 2001; revision received 9 November 2001.     

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.     

Electromechanical Characterization of Au Thin Films using Micro-tensile Testing

This paper presents the test technique about measurement of electrical resistance changes of thin films during tensile testing. In this work, we used a real-time digital image correlation strain measurement system coupled with micro-tensile testing unit and voltage/current sourcemeter. This system has the advantage of real time displacement monitoring with a resolution of 50 nm during the micro-tensile testing, with the ability to measure the variation in electrical resistance of the specimen at the same time. We obtained the complete testing data for the stress–strain curve and associated electrical resistance-strain curve for 1 and 2 μm-thick freestanding gold films. Young’s modulus was about 61~69 GPa and 0.2% offset yield strength was about 361~402 MPa. In case of the electrical resistance, rapid change was observed under the elastic regime, while less obvious under the plastic regime. We also conducted finite element analysis, and this result implied that the electrical resistivity would not be constant during micro-tensile testing.     

基于光学和扫描显微平台的微尺度实验力学检测技术和装置研究

本文基于光学和扫描显微平台,介绍了本研究组在微尺度实验力学检测技术和设备方面的最新研究成果。在检测技术方面涉及显微散斑干涉技术、微标记阵列检测技术、晶粒变形分析技术、光学探针动静态变形分析技术;在检测系统和装置方面介绍了新近开发的双视场薄膜检测系统、散斑微干涉系统、微标记检测平台、AFM和SEM单轴拉伸装置、三维微定位与加载系统、微力传感器及其标定装置、微动平台驱动装置等。探讨了微尺度实验力学检测中的问题和新的检测技术,给出了一些典型的应用和相关装置。     

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.     

Evaluation of the Material Properties of an OFHC Copper Film at High Strain Rates Using a Micro-Testing Machine

The material properties of an oxygen-free high thermal conductivity (OFHC) film with a thickness of 0.1 mm were evaluated at strain rates ranging from 10⁻³/s to 10³/s using a high-speed material micro-testing machine (HSMMTM). The high strain-rate material properties of thin films are important especially for an evaluation of the structural reliability of micro-formed parts and MEMS products. The high strain-rate material testing methods of thin films, however, have yet to be established to the point that the testing methods of larger specimens for electronics, auto-body, train, ship, and ocean structures are. For evaluation, a new type of HSMMTM was developed to conduct high-speed tensile tests of thin films. This machine is capable of testing at a sufficiently high tensile speed with an electromagnetic actuator, a novel gripping mechanism, and an accurate load measurement system. The OFHC copper film shows high strain-rate sensitivity in terms of the flow stress, fracture elongation, and strain hardening. These measures increase as the tensile strain rate increases. The rate-dependent material properties of an OFHC copper film are also compared with those of a bulk OFHC copper sheet with a thickness of 1 mm. The flow stress of an OFHC copper film is relatively low compared to that of a bulk OFHC copper sheet in the entire range of strain rates, while the fracture elongation of an OFHC copper film is much larger than that of a bulk OFHC copper sheet. A quantitative comparison would provide material data at high strain rates for the design and analysis of micro-appliances and different types of micro-equipment.     

Distribution of dislocation source length and the size dependent yield strength in freestanding thin films

A method is proposed to estimate the size-dependent yield strength of columnar-grained freestanding thin films. The estimate relies on assuming a distribution of the size of Frank-Read sources, which is then translated into a log-normal distribution of the source strength, depending on film thickness, grain size and theoretical strength of the material, augmented with a single fit parameter. Two-dimensional discrete dislocation plasticity (DDP) simulations are carried out for two sets of Cu films and the fit parameter is determined from independent experiments. Subsequent DDP predictions of the stress-strain curves in comparison with the corresponding experimental data show excellent agreement of initial yield strength and hardening rate for films of varying film thickness and grain size. Having thus demonstrated the power of the proposed strength distribution, it is shown that the mode of this distribution governs the most effective source strength. This is then used to suggest a method to estimate the yield strength of thin films as a function of film thickness and grain size. Simple maps are presented that are in very good agreement with recent experimental results for Cu thin films.     

MEMS材料力学性能的测试技术

微电子机械系统(MEMS)技术的迅速崛起,推动了所用材料微尺度力学性能测试技术的发展.首先按作用方式将实验分成压痕/划痕、弯曲、拉伸、扭转四大类,系统介绍检测MEMS材料微尺度力学性能的微型试样、测试方法及其实验结果.测试材料主要有硅、氧化硅、氮化硅和一些金属.实验结果主要包括基本的力学性能参数如弹性模量、残余应力、屈服强度、断裂强度和疲劳强度等.最后,简要分析了未来的发展需求.      

单纤维微拉伸力学性能测试与分析

针对微尺度材料力学性能测试与尺度效应实验研究的需要,自行研制了一台FMT-I型高精度纤维材料微拉伸力学性能实验装置,并基于LabVIEW软件平台开发了相应的数据采集与控制系统,实现了测试过程的全自动化。该装置的测力传感器由非接触式激光位移传感器和两端固定的薄梁组成,可同时测量试样的拉伸力和上夹持端的位移量,帮助精确地获取试样的载荷-变形曲线。采用该装置对微米级直径的多晶铜丝、316L不锈钢纤维和T300碳纤维进行了拉伸测试。实验结果表明,直径为18～105μm多晶铜丝的拉伸力学行为并无明显的尺度效应;多晶铜丝和316L不锈钢纤维的弹性模量分别在43.9～60.0GPa和102.9～111.5GPa之间,均低于宏观尺度下材料的弹性模量;316L不锈钢纤维的抗拉强度和延伸率随着丝径的减小而降低;T300碳纤维的弹性模量为235.4±12.4GPa,抗拉强度为3238.2±280.8MPa,断裂应变约为1.5%。另外,相同的细铜丝材料的测试结果与Instron5848型商用拉伸试验机的测试结果进行了对比,吻合良好。通过系统的实验分析表明,该装置具有较高的精度和稳定性,适用于各种纤维材料的拉伸力学性能测试。     

Plasticity size effects in free-standing submicron polycrystalline FCC films subjected to pure tension

The membrane deflection experiment developed by Espinosa and co-workers was used to examine size effects on mechanical properties of free-standing polycrystalline FCC thin films. We present stress-strain curves obtained on films 0.2, 0.3, 0.5 and thick including specimen widths of 2.5, 5.0, 10.0 and for each thickness. Elastic modulus was consistently measured in the range of 53- for Au, 125- for Cu and 65- for Al. Several size effects were observed including yield stress variations with membrane width and film thickness in pure tension. The yield stress of the membranes was found to increase as membrane width and thickness decreased. It was also observed that thickness plays a major role in deformation behavior and fracture of polycrystalline FCC metals. A strengthening size scale of one over film thickness was identified. In the case of Au free-standing films, a major transition in the material inelastic response occurs when thickness is changed from 1 to . In this transition, the yield stress more than doubled when film thickness was decreased, with the thick specimen exhibiting a more brittle-like failure and the thick specimen exhibiting a strain softening behavior. Similar plasticity size effects were observed in Cu and Al. Scanning electron microscopy performed on Au films revealed that the number of grains through the thickness essentially halved, from approximately 5 to 2, as thickness decreased. It is postulated that this feature affects the number of dislocations sources, active slip systems, and dislocation motion paths leading to the observed strengthening. This statistical effect is corroborated by the stress-strain data in the sense that data scatter increases with increase in thickness, i.e., plasticity activity.The size effects here reported are the first of their kind in the sense that the measurements were performed on free-standing polycrystalline FCC thin films subjected to macroscopic homogeneous axial deformation, i.e., in the absence of deformation gradients, in contrast to nanoindentation, beam deflection, and torsion, where deformation gradients occur. To the best of our understanding, continuum plasticity models in their current form cannot capture the observed size scale effects.     

Specimen and Grain Size Effects of Al1100 on Strain and Strain Rate Hardening at Various Strain Rates for Al1100

This paper is concerned with comparison of the tensile properties of Al1100 thin film in a micro-scale to that of Al1100 sheet in a macro-scale. The material properties of Al1100 film and sheet with a thickness of 96 μm and 1 mm respectively have been investigated at strain rates ranging from 0.001 to 100 s^?1. The experiments were conducted with Static Micro-Material Testing Machine (SMMTM) and High Speed Micro-Material Testing Machine (HSMMTM) for micro-specimens and with Instron 5583 and high speed material testing machine (HSMTM) for macro-specimens. A reliable jig system for SMMTM and HSMMTM has been newly developed for easy installation of a specimen and accurate alignment between a specimen and the jig system to enhance the reproducibility of tests. The digital image correlation (DIC) method is employed to measure the axial strain of the specimens. In order to obtain a fine speckle pattern for the DIC method, a novel technique is employed to print the speckle pattern with fine particles by blowing sprayed particles before printing. The grain sizes of two Al1100 specimens have been compared and the number of grains in the gauge cross-section has been calculated to obtain the grain number which is related to the specimen size effect. Electron Back Scattered Diffraction (EBSD) images were obtained for both micro-specimens and macro-specimens and analyzed to measure the grain size. The Al1100 film with a smaller average grain size shows larger strain hardening than the Al1100 sheet with a larger average grain size.     

DIC-Based Surface Motion Correction for ESPI Measurements

Electronic Speckle Pattern Interferometry (ESPI) provides a sensitive technique for measuring surface deformations. The technique involves comparison of the speckle phase angles within surface images measured before and after material deformation. This phase angle comparison requires that the speckle positions be consistent in all images. A lateral shift between image sets of just one pixel substantially degrades ESPI measurements, while a shift of two or more pixels typically causes complete decorrelation and compromises the measurement entirely. To prevent such rigid body motions, the specimen and the optical system must be rigidly fixed. This requirement typically impedes use of the ESPI method in applications outside laboratories or where it is necessary to remove the specimen from the optical setup between ESPI measurements. Here, Digital Image Correlation (DIC) is used to track speckle motion caused by specimen displacement between ESPI phase stepped image sets. The measured image set can then be mathematically shifted to restore the original speckle locations, thereby recorrelating the ESPI measurement. Examples are presented where ESPI measurements are successfully made with specimen shifts over 60 pixels.     

Pure-shear Failure of Thin Films by Laser-induced Shear Waves

The measurement of mode-dependent thin film interfacial properties is important in evaluating the quality of the interfaces between thin films and substrates. Previous work has proved that tensile and mixed-mode strength of a thin film/substrate interface can be evaluated using a laser-induced thin film spallation technique. To further examine the application regime of this technique and identify the individual roles of the tensile and shear stress in the resulting interfacial failure, a special sample design is adopted in the current work to realize pure-shear loading at the thin film/substrate interface. Our result demonstrates that for sufficiently high stress amplitude, interfacial failure can be induced solely by the in-plane shear stress and the stress can be quantitatively determined from optical interferometric measurements. Together with the previous tensile and mixed-mode studies, a complete picture of the mode-dependent thin film interfacial strength can now be reliably determined using the laser-induced thin film spallation techniques.     

纳米压痕法测磁控溅射铝薄膜屈服应力

为了在考虑残余应力下测量出磁控溅射铝薄膜的屈服应力,提出了一种实验测量方法,通过曲率测试法和球形压头纳米压痕法测出磁控溅射铝薄膜的屈服应力．建立球形压痕力学模型,并用ANSYS对球形压痕进行力学有限元仿真,利用直流磁控溅射技术在硅基上淀积一层1 μm厚的铝薄膜,首先通过曲率测试法测量膜内等双轴残余应力,再利用最小二乘曲线拟合法从薄膜/基底系统的球形压头纳米压痕实验数据中提取出铝薄膜的屈服应力,测得磁控溅射铝薄膜的屈服应力为371 MPa．该方法也可以用来研究其他材料的薄膜和小体积材料的力学特性．     

Local mechanical properties of the 6061-T6 aluminium weld using micro-traction and instrumented indentation

The local mechanical properties of a weld zone, in a 6061-T6 aluminium alloy subjected to the modified indirect electric arc technique have been studied. The mechanical properties of the base metal, the weld metal and the heat affected zone were determined by means of usual and instrumented indentation testing, as well as micro-traction testing. To analyse the heat input effect resulting from the welding process, the evolution of the weld zone size was evaluated by means of classical indentation under a constant applied load. The results were presented using a Vickers hardness map representation. This allows monitoring exact hardness variation while leading to the identification of the different zones of the welded joint. Instrumented indentation testing was carried out to determine the local mechanical properties, such as the yield stress, the bulk modulus and the strain-hardening exponent. Obtained results are compared to those derived from tensile tests conducted on micro-specimen cuts taken from the weld zone. It was observed that yield stress values are directly comparable for indentation and micro-traction experiments. As for the elastic properties, no comparison was possible since the bulk modulus is measured by indentation, whereas it is the Young’s modulus by tensile test. The micro-traction testing seems to be more sensitive to represent the work hardening of a material since the corresponding exponent is found to be constant by instrumented indentation.     

薄膜应力应变曲线和基本力学性能测试

本文采用白光散斑和数字散斑两种方法测量了厚度在１－６０μｍ）之间康铜孤立膜和其上喷镀ＴｉＯ２后复合膜的应力应变曲线，并成功地利用一种新方法－复合材料分离法由孤立膜和复合膜应力应变曲线分离出ＴｉＯ２膜的应力应变曲线，同时给出了它们的基本力学性能（如（ｅ，ｑｓ，ｑｓ，Ｋ）测量结果表明这一方法对于微电子及其组件中常用的薄膜（１－６０μｍ）及超薄膜（０．１－１μｍ）的应力应变和基本力学性能的测量有普遍意义     

Whole-field strain measurement in a pin-loaded plate by electronic speckle pattern interferometry and the finite element method

The strain field in an epoxy plate loaded in tension through a steel pin is determined using electronic speckle pattern interferometry (ESPI) and the finite element method (FEM). In a dual-beam illumination speckle interferometer, the in-plane component of the displacement at the plate's surface is accurately measured using a four-step phase-shifting algorithm. Digital image processing algorithms have been developed for noise reduction and strain calculation directly in the computer from the phase map with a strain gage length of about 0.4 mm. A whole-field strain map is obtained, as well as distributions of strain concentration factor, in critical regions near the hole of the plate. FEM is used to perform a nonlinear contact analysis accounting for friction effects at the pin/hole interface. The agreement between experimental results and numerical predictions is good. In terms of speed, accuracy and ease of use, dual-beam ESPI appears to be a superior method of whole-field strain analysis.     

Material Characterization at High Strain by Adapted Tensile Tests

The strength of materials at high strain levels has been determined using the so-called Continuous-Bending-under-Tension (CBT) test. This is a modified tensile test where the specimen is subjected to repetitive bending at the same time. This test enables to create high levels of uniform strain. A wide variety of materials has been tested this way. The strength of the material after CBT testing has been measured in different ways: by secondary tensile tests, by interrupted CBT tests, and directly from the fracture in the CBT test. All methods yield similar results: the strength is largely unaffected by the cyclic pre-deformation and mainly depends on the overall increase in length. Only for multi-phase materials the strength shows a minor influence of CBT test conditions. The hardening follows the extrapolated hardening observed in a conventional tensile test, except for brass. This test method can potentially be used for measuring hardening curves at high strain levels.     

Strain Localization in Mild (Low Carbon) Steel Observed by Acoustic Emission - ESPI Coupling during Tensile Test

Two strain localization modes: the Piobert-Lüders band propagation and the development of necking, were investigated in uniaxial tensile tests for a low alloyed and low carbon steel. These two macroscopic localization phenomena were simultaneously monitored by speckle interferometry (ESPI) and acoustic emission (AE). The coupling of these two experimental techniques gives complementary information about strain localization features and mechanisms. For Lüders bands, it was found that the acoustic activity heard during the travel of the Piobert-Lüders band varies in closely correlated to the tensile force fluctuations, the relations between strain rate, band velocity, band width and plastic strain were investigated. Although the strain rate in the wake of the wave front is not always zero, the acoustic activity remains concentrated in the wave front itself. For necking, the acoustic activity is found to decrease regularly through the homogeneous plasticity stage and the diffuse necking stage and then increases when the localized necking starts, while ESPI patterns show a gradual strain concentration.