In-situ tensile testing of nano-scale specimens in SEM and TEM

We present a new experimental method for the mechanical characterization of freestanding thin films with thickness on the order of nanometers to micrometers. The method allows, for the first time, in-situ SEM and TEM observation of materials response under uniaxial tension, with measurements of both stresses and strains under a wide variety of environmental conditions such as temperature and humidity. The materials that can be tested include metals, dielectrics, and multi-layer composites that can be deposited/grown on a silicon substrate. The method involves lithography and bulk micromachining techniques to pattern the specimen of desired geometry, release the specimen from the substrate, and co-fabricate a force sensor with the specimen. Co-fabrication provides perfect alignment and gripping. The tensile testing fits an existing TEM straining stage, and a SEM stage. We demonstrate the proposed methodology by fabricating a 200 nm thick, 23.5 μm wide, and 185 μm long freestanding sputter deposited aluminum specimen. The testing was done in-situ inside an environmental SEM chamber. The stress-strain diagram of the specimen shows a linear elastic regime up to the yield stress σ _y MPa, with an elastic modulusE=74.6 GPa.     

A review of MEMS-based microscale and nanoscale tensile and bending testing

Thin films at the micrometer and submicrometer scales exhibit mechanical properties that are different than those of bulk polycrystals. Industrial application of these materials requires accurate mechanical characterization. Also, a fundamental understanding of the deformation processes at smaller length scales is required to exploit the size and interface effects to develop new and technologically attractive materials. Specimen fabrication, small-scale force and displacement generation, and high resolution in the measurements are generic challenges in microscale and nanoscale mechanical testing. In this paper, we review small-scale materials testing techniques with special focus on the application of microelectromechanical systems (MEMS). Small size and high force and displacement resolution make MEMS suitable for small-scale mechanical testing. We discuss the development of tensile and bending testing techniques using MEMS, along with the experimental results on nanoscale aluminum specimens.     

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.     

A Measuring System for Bulk and Shear Characterization of Polymers

This paper describes a novel measuring system for investigating the influence of pressure and temperature on the mechanical properties of time-dependent polymer materials. The system can measure the volume and the shear relaxation moduli of solid polymer specimens simultaneously subjected to temperatures from −50 to +120°C with a precision of ±0.01°C, and pressures from atmospheric to 500 MPa with a precision of ±0.1 MPa. The paper demonstrates the measuring capabilities of the apparatus. For poly(vinyl) acetate (PVAc) are presented sample measurements of the shear relaxation modulus as function of time, pressure and temperature; specific volume; the bulk creep compliance; the coefficient of thermal expansion; the bulk modulus; and the pressure drop experiments which simulate conditions to which a material is exposed during the injection molding process. The shear moduli may be measured in the range from 1 to 4,000 MPa with the relative error of 3%.The error of volumetric measurements is 0.05%, which corresponds to 0.00005 cm³/g. In all cases results are shown as measured, no additional smoothing or filtering was employed. This paper is dedicated to Professor Nicholas W. Tschoegl on the occasion of his 87th birthday, for his contributions to the field of time-dependent bulk properties of polymeric materials.     

Predictions of nonlinear viscoelastic behavior using a hybrid approach

An approach for nonlinear viscoelastic characterization is presented which uses the combined measurements from creep and dynamic mechanical tests. Although the methodology should extend to several materials and geometries, this research concentrates on thin film polymers used in the manufacture of high altitude scientific balloons. Typically, the constitutive behavior of these materials is characterized through the use of linear viscoelastic techniques. Although this linear approach provides an accurate model for small strains or loads, these materials have been shown to be highly stress dependent and, consequently, it is necessary to identify this nonlinear behavior. Traditional creep measurements require extensive laboratory test times, yet the results obtained from dynamic mechanical analysis provide the capability to predict long term material performance without a lengthy experimentation program. However, dynamic mechanical methods are currently limited to linear response; thus, an approach is presented in which the stress-dependent behavior is derived from short-term creep measurements in a manner analogous to time-temperature superposition. Predictions of material response using linear and nonlinear approaches are compared with experimental results obtained from traditional long-term creep tests. Although linear pre-dictions deteriorate for large stresses, excellent agreement is shown for the nonlinear model.     

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.     

Design of Inserts for Split-Hopkinson Pressure Bar Testing of Low Strain-to-Failure Materials

In the present study a new insert design is presented and validated to enable reliable dynamic mechanical characterization of low strain-to-failure materials using the Split-Hopkinson Pressure Bar (SHPB) apparatus. Finite element-based simulations are conducted to better understand the effects of stress concentrations on the dynamic behavior of LM-1, a Zr-based bulk metallic glass (BMG), using the conventional SHPB setup with cylindrical inserts, and two modified setups—one utilizing conical inserts and the other utilizing a “dogbone” shaped specimen. Based on the results of these computational experiments the ends of the dogbone specimen are replaced with high-strength maraging steel inserts. This new insert-specimen configuration is expected to prevent specimen failure outside the specimen gage section. Simulations are then performed to validate the new insert design. Moreover, high strain-rate uniaxial compression tests are conducted on LM-1 using the modified SHPB with the new inserts. An ultra-high-speed camera is employed to investigate the changes in failure behavior of the specimens. Additional experiments are conducted with strain gages directly attached to the gage section of the specimens to determine accurately their dynamic stress–strain behavior.     

Temperature dependent bulge test for elastomers

The bulge test is a particularly convenient testing method for characterizing elastomers under biaxial loading. In addition, it is convenient to utilize this test for validating material models in simulation due to the heterogeneous strain field induced during inflation. During the bulge test the strain field for elastomers covers uniaxial tension at the border to pure shear and equibiaxial tension at the pole. Elastomeric materials exhibit a hyperelastic material behavior, with a dependency on temperature and loading rate. The temperature effect on the mechanical behavior during biaxial loading is considered in the present study. A bulge test setup combined with a temperature chamber is developed in order to characterize this effect, and an exemplary temperature dependent characterization of a poly(norbornene) elastomer is performed with this setup. The equibiaxial stress–strain curves measured at 60 °C, 20 °C and −20 °C are presented.     

Experimental Results of a Damage Detection Methodology using Variations in Modal Parameters

The present paper reports the results obtained by a methodology of damage detection in which combined EMA and FEM data are used to localise the damage on mechanical components. The utilized method uses the eigenvalues and eigenvectors obtained from FE modelling, compared with the eigenvalues obtained experimentally on damaged specimens. The method assumes a linear behaviour of the materials. Firstly it is applied to rectangular plates in order to test its reliability in discovering the damage located on very simply shaped specimens that are made of homogeneous and isotropic material. The methodology was subsequently applied to mechanical components of complex shape, allowing the location of the damage to be accurately identified.     

Neighborhood Relationships of Widely Distributed and Irregularly Shaped Particles in Partially Dewatered Filter Cakes

A more thorough understanding of the properties of bulk material structures in solid–liquid separation processes is essential to understand better and optimize industrially established processes, such as cake filtration, whose process outcome is mainly dependent on the properties of the bulk material structure. Here, changes of bulk properties like porosity and permeability can originate from local variations in particle size, especially for non-spherical particles. In this study, we mix self-similar fractions of crushed, irregularly shaped Al₂O₃ particles (20 to 90 µm and 55 to 300 µm) to bimodal distributions. These mixtures vary in volume fraction of fines (0, 20, 30, 40, 50, 60 and 100 vol.%). The self-similarity of both systems serves the improved parameter correlation in the case of multimodal distributed particle systems. We use nondestructive 3D X-ray microscopy to capture the filter cake microstructure directly after mechanical dewatering, whereby we give particular attention to packing structure and particle–particle relationships (porosity, coordination number, particle size and corresponding hydraulic isolated liquid areas). Our results reveal widely varying distributions of local porosity and particle contact points. An average coordination number (here 5.84 to 6.04) is no longer a sufficient measure to describe the significant bulk porosity variation (in our case, 40 and 49%). Therefore, the explanation of the correlation is provided on a discrete particle level. While individual particles?<?90 µm had only two or three contacts, others?>?100 µm took up to 25. Due to this higher local coordination number, the liquid load of corresponding particles (liquid volume/particle volume) after mechanical dewatering increases from 0.48 to 1.47.

     

Measurement of Local Thermal Deformations in Heterogeneous Microstructures via SEM Imaging with Digital Image Correlation

It is challenging to measure accurately and with high spatial resolution the local thermal strains in heterogeneous microstructures due of the complex nature of the thermal deformations and local boundary conditions. In the enclosed study, a digital image correlation (DIC) based, thermal strain mapping technique is described that is able to probe thermal deformations with sub-micron spatial resolution and sub-nanometer displacement accuracy for both homogeneous and heterogeneous materials, including cross-sections of IC packages. The full-field thermal deformation maps of different materials within a nanostructured IC chip cross-section are established from room temperature up to 160 °C, uncovering the heterogeneous nature of the specimen while accurately measuring the highly non-uniform displacement and strain fields across the multiple material constituents. As described in this work, the DIC-enabled technique is capable of high resolution mapping of local thermo-mechanical deformations in heterogeneous materials, providing a methodology that can improve our understanding of complex material systems under controlled thermal-environmental conditions.     

Adiabatic shear banding in plane strain tensile deformations of 11 thermoelastoviscoplastic materials with finite thermal wave speed

We study the initiation and propagation of adiabatic shear bands (ASBs) in 11 homogeneous materials each modeled as microporous, isotropic and thermoelastoviscoplastic, and deformed in plane strain tension. The heat conduction in each material is assumed to be governed by a hyperbolic heat equation; thus thermal and mechanical waves propagate with finite speeds. The decrease in the thermophysical parameters due to the increase in porosity is considered. An ASB is assumed to initiate at a material point when the maximum shear stress there has dropped to 80% of its peak value for that material point and it is deforming plastically. An approximate solution of the coupled nonlinear partial differential equations subject to suitable initial and boundary conditions is found by the finite element method (FEM). In contrast to the Considerè and the Hart criterion, it is found that an ASB initiates when the axial load drops rapidly and not when it peaks. The refinement of the 40 × 40 uniform FE mesh to 120 × 120 uniform elements decreased the ASB initiation time by 2.1% while increasing the CPU time by a factor of ∼26. By locating points where the ASB has initiated we find its current length, width and speed. The 11 materials are ranked according to the time of initiation of an ASB under otherwise identical geometric and loading conditions with the same initial nonuniform porosity distribution. This ranking of materials is found to differ somewhat from that ascertained by Batra and Kim (1992) who studied simple shearing deformations, and by Batra et al. (1995) who analyzed three-dimensional torsional deformations of thin-walled tubular specimens. The average axial strain determined from the maximum axial load condition differs noticeably from that when an ASB initiates.     

An empirical methodlogy to estimate a local yield stress in work-hardened surface layers

A methodology is proposed for estimating the local yield stress in work-hardened surface layers. It is based on the concept of in-depth normalized variation of hardness and x-ray diffraction peak width, both of which measure the strain-hardening attained by the materials' surface-treated layers due to, for example, shot-peening. Its principle is directly founded on the classical hardness theory. To study the evolution of those values with plastic deformation, specimens of five steels with different mechanical properties were subjected to interrupted tensile tests. The tests were performed at successive increments of plastic strain, until fracture occurred. The specimens were loaded and unloaded in increments of about 2% true strain. After each plastic strain increment, hardness and diffraction peak width were measured. It was observed that the variations of diffraction peak width and hardness are related to the material's strain-hardening, and their normalized variations can be considered proportional to the normalized variation of the material's yield stress. Thus, where the yield stress of the bulk material, its hardness or a characteristic diffraction peak width value, and their relative variations along the hardened layers, are known, an empirical expression could be used to estimate the local yield stress as a function of the treated depth.     

Influence of geometry on stress state in bulk characterization tests

This paper is concerned with the selection of the geometries of test specimens for bulk metal characterization tests. Simulations of characterization tests on cylindrical, notched, and shear specimens were conducted to allow for the analysis of stress state evolution during the tests and to evidence the impact of geometry on stress state. Both stress triaxiality and Lode parameter were considered for selecting representative specimens. Three choice criterions were regarded: the diversification of stress states as well as the constancy and the nearness of stress state indicators to the theoretical values along the deformation.     

Determination of mechanical properties of non-linear coatings from measurements with coated beams

Coatings are applied to structural components for several various reasons, such to protect against erosion or corrosion, as thermal barrier coatings, or to increase the energy dissipation. As determining the material properties of such coatings from homogeneous specimens is often difficult, it is sometimes necessary to conduct testing on coated specimens, with the properties of the coating then to be extracted from the results of testing. A methodology for doing this is given here. While applicable to other materials, the properties of such coatings as ceramics, metallics, or compounds to be applied to rotating and static components of gas turbines are of special interest. Such materials present a special challenge as the mechanical properties have generally been found to display a strong dependence on the amplitude of cyclic strain. Application of the methodology requires careful measurement of specimen dimensions, weights, natural frequencies, and system loss factors before and after coating. From these, the storage (Young’s) modulus, the loss modulus, and the loss factor can be extracted. The methodology is demonstrated through the use of data taken on flat specimens of titanium with plasma-sprayed coatings of NiCrAlY and a titania–alumina blend ceramic, vibrating in a cantilever mode.     

Murray lecture tensile testing at the micrometer scale: Opportunities in experimental mechanics

The measurement of mechanical properties using specimens whose minimum dimensions are of the order of micrometers is an important new area of experimental solid mechanics. One obvious application is in the area of micro-electromechanical systems (MEMS) where the final product is on the millimeter or micrometer scale. This paper describes techniques developed at Johns Hopkins University for tensile testing of materials used in MEMS. Polycrystalline silicon is currently the most widely used material; its modulus has been measured as 158±10 GPa, and its Poisson's ratio as 0.22±0.01, with fracture strengths ranging from 1.2 to 3.0 GPa depending upon the manufacturer. The properties of silicon nitride, silicon carbide, and electroplated nickel have also been measured and are presented. In addition to the quasi-static tensile tests, new techniques and procedures for measuring strengths at stress concentrations in brittle thin-film materials, fatique testing, and high-temperature testing are described.     

On the Measurement of two Independent Viscoelastic Functions with Instrumented Indentation Tests

In the present paper, a methodology for complete characterization of linear isotropic viscoelastic material with spherical instrumented indentation test is proposed. The developed method allows for measuring two independent viscoelastic functions, shear relaxation modulus and time-dependent Poisson’s ratio, from the indentation test data obtained at non-decreasing loading, but otherwise arbitrary. Finite element modelling (FEM) is relied upon for validating the proposed methodology and for quantifying the influence of experimental variables on the measurements accuracy. Spherical indentation experiments are performed on several viscoelastic materials: polyoxymethylene, bitumen and bitumen-filler mastics. The viscoelastic material functions obtained with the indentation tests are compared with the corresponding results from the standard mechanical tests. Numerical and experimental results presented indicate that the methodology proposed allows mitigating the machine compliance and loading rate effects on the accuracy of the viscoelastic indentation tests.     

A General Methodology for Full-Field Plastic Strain Measurements Using X-ray Absorption Tomography and Internal Markers

Probing the strain locally and throughout the bulk of various materials has long been of interest in Materials Science. This article presents a general methodology for assessing the plastic strain in terms of the displacement gradient tensor throughout the bulk of opaque samples. The method relies on a homogenous distribution of marker particles throughout the bulk of a sample, markers which are detected through the application of synchrotron X-ray tomography. Making use of the morphology of individual markers, motion of individual markers is tracked during deformation allowing the local displacement field to be determined throughout the bulk. The local displacement gradient tensor is derived from the displacement field. Spatial resolution is directly related to marker particle density in the sample, here 30 μm. The accuracy of the displacement gradient tensor calculation is dependent on the accuracy with which each marker position is determined and is shown to be in the range from 0.005 to 0.012. The software implementation of the procedures and algorithms presented in this work has been collected to form the “3Dstrain” program package which is intended to be free for use by the scientific community. It is available at under GNU General Public License.     

Numerical-graphical method for determining characteristics of damaged viscoelastic materials

A method for determining the material functions of nonlinear endochronic theory of aging viscoelastic materials (NETAVEM) with preliminary mechanical damage was developed. The proposed method is based on an analysis of the differences between two graphs of the stress dependence on time obtained in tension with the same constant speed of two specimens made of the same filled polymer material. One of the specimens was not preloaded, and the other was preloaded. The reduced time [1] contained in the NETAVEM constitutive relations and its dependence on the actual time are determined by the distances from the stress axis to two points corresponding to the same stress value and lying on the graphs for the damaged and undamaged specimens. The relaxation kernel is determined in the experiment with the undamaged specimen. These two material functions and the curve obtained for the damaged specimen are used to obtain the NETAVEM aging function, and then the function of viscosity can be calculated. As a result, all characteristics of the damaged material become known, and the strength of structures made of this material can be calculated.