Novel Microtensile Method for Monotonic and Cyclic Testing of Freestanding Copper Thin Films

This paper presents the results of new microtensile tests conducted to investigate the mechanical properties of submicron-thick freestanding copper films. The method, used in this study, allows the observation of materials response under uniaxial tensile loads with measurements of stress at strain rates up to 5.5 × 10⁻⁴/s. It also facilitates tension–tension fatigue experiments under a variety of mean stress conditions at cyclic loading frequencies to 20 Hz. The sample processes involve fabrication of a supporting frame with springs and alignment beams all made of electroplated nickel. Electroplating took place on top of a previously deposited sample rather than creating a structure by subtractive fabrication. Tensile sample loading is applied using a piezoelectric actuator. Load was measured using a capacitance gap sensor with a novel mechanical coupling to the sample. Tension–tension fatigue experiments were carried out with feedback to give load control. Fatigue tests were conducted on sputter-deposited 500 and 900 nm copper films with grain sizes ∼50 nm. Fatigue life reached 10⁵ cycles at low mean load, which decreased with an increase in the mean load. The results indicate decreasing plasticity with increasing mean load.     

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.     

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.     

Effects of coincidence window and measuring volume size on laser Doppler velocimetry measurement of turbulence

The effects of coincidence window and measuring volume size on two-component laser velocimeter measurement of turbulence in an isothermal liquid flow through a concentric annular channel were studied. Three different coincidence windows (100–500 μs) and three different measuring volume sizes (diameter, 5–9 wall units; spanwise length, 24–91 wall units) were used in a flow of Reynolds number 31,500 and data density spanning the high end of intermediate to the low end of high (3–6). While no significant effects of the coincidence window and measuring volume size were found on the time-mean velocity and turbulence intensities, the streamwise Reynolds shear stress measured near a wall was found to be markedly affected by both. The smallest feasible measuring volume along with an appropriate coincidence window provides good measurement of the shear stress. Received: 8 September 1999/Accepted: 11 July 2000     

Tensile and Tensile-Mode Fatigue Testing of Microscale Specimens in Constant Humidity Environment

A tensile and tensile-mode-fatigue tester has been developed for testing microscale specimens in high humidity environments in order to investigate the fracture mechanisms of microelectromechanical materials. A humidity control system was installed on a tensile-mode fatigue tester equipped with an electrostatic force grip. A specimen and a griping device were inserted into a small chamber and the humidity was controlled by air flow from a temperature and humidity chamber. The humidity stability was within ±2%RH for humidities in the range 25–90%RH for eight hours of testing. Fatigue tests were performed on single-crystal silicon (SCS) specimens in constant humidity environments and laboratory air for up to 10⁶ cycles. The gauge length, width, and thickness of the SCS specimens were 100 or 500 μm, 13.0 μm, and 3.3 μm, respectively. The average tensile strength was 3.68 GPa in laboratory air; this value decreased in high humidity environments. Fatigue failure was observed during cyclic loading at stresses lower than the average strength. A reduction in the fatigue strength was observed at high relative humidities. Different fracture origins and fracture behaviors were observed in tensile tests and fatigue tests, which indicates that the water vapor in air affects the fatigue properties of SCS specimens.     

A high-resolution laser Doppler anemometer: design, qualification, and uncertainty

A new high-resolution laser Doppler anemometer (LDA) has been developed with a working distance of 350 mm, allowing operation in lab-scale wind tunnels. The measurement volume size is 35 μm in diameter by 60 μm in length, allowing resolution of the smallest turbulence scales even at fairly high Reynolds numbers. The controversial question of velocity and validation bias in LDA data is resolved with an experimental method for measuring and removing those effects. Uncertainty estimates are also derived for all the mean and Reynolds stress measurements. Received: 27 June 1999/Accepted: 30 August 2000     

Experimental study of microhole growth and coalescence in ductile materials

The growth and coalescence of two microholes in copper foil were studied experimentally byin situ tensile tests under a scanning electronic microscope. Two microholes of 15–35 μm in diameter were arranged in different distances and orientations. It was found that the mechanisms of microhole evolution were represented by slipping band creation, and then crack initiation and propagation along the slipping bands in ligament. The process of microhole growth and coalescence was influenced by the inter-center distance and orientation of microholes. The critical surface of microholes at coalescence is about 2–2.5 times that of the initial one. The variation of both the inter-center distance and orientation depends on the initial angle.     

Micro-scale behavior of granular materials during cyclic loading

This study presents the micro-scale behavior of granular materials under biaxial cyclic loading for different confining pressures using the two-dimensional (2D) discrete element method (DEM). Initially, 8450 ovals were generated in a rectangular frame without any overlap. Four dense samples having confining pressures of 15, 25, 50, and 100 kPa were prepared from the initially generated sparse sample. Numerical simulations were performed under biaxial cyclic loading using these isotropically compressed dense samples. The numerical results depict stress–strain–dilatancy behavior that was similar to that observed in experimental studies. The relationship between the stress ratio and dilatancy rate is almost independent of confining pressures during loading but significantly dependent on the confining pressures during unloading. The evolution of the coordination number, effective coordination number and slip coordination number depends on both the confining pressures and cyclic loading. The cyclic loading significantly affects the microtopology of the granular assembly. The contact fabric and the fabric-related anisotropy are reported, as well. A strong correlation between the stress ratio and the fabric related to contact normals is observed during cyclic loading, irrespective of confining pressures.     

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.     

Stiffening and Contraction Induced by Dexamethasone in Alveolar Epithelial Cells

Background  The structural integrity of the alveolar monolayer, which is compromised during lung inflammation, is determined by the balance between cell–cell and cell-matrix tethering forces and the centripetal forces owing to cell viscoelasticity and contraction. Dexamethasone is an anti-inflammatory glucocorticoid with protective effects in lung injury. Aim  To determine the effects of Dexamethasone on the stiffness and contractility of alveolar epithelial cells. Methods  Cell stiffness (G′) and average traction exerted by the cell (T) were measured by magnetic twisting cytometry and by traction microscopy, respectively. A549 cells were treated 24 h with Dexamethasone (1 μM) or vehicle (control). G′ and T were measured before and 5 min after challenge with the inflammatory mediator Thrombin (0.5 U/ml). Changes induced by Dexamethasone in actin cytoskeleton polymerization were assessed by the fluorescent ratio between F-actin and G-actin obtained by staining cells with phalloidin and DNase I. Results  Dexamethasone significantly increased G′ and T by 56% (n = 11; p < 0.01) and by 80% (n = 17; p < 0.05), respectively. Dexamethasone also increased F/G-actin ratio from 2.68 ± 0.07 to 2.96 ± 0.09 (n = 10; p < 0.05). The relative increase in stiffness and contraction induced by Thrombin in control cells was significantly (p < 0.05) reduced by Dexamethasone treatment: from 190 to 98% in G′ and from 318 to 105% in T. Conclusion  The cytoskeleton remodelling and the increase in cell stiffness and contraction induced by Dexamethasone could account for its protective effect in the alveolar epithelium when subjected to inflammatory challenge.     

Study of high Deborah number flow of polyisobutylene in square die

A large capacity RAM extruder was designed which provides the opportunity to study high Deborah number (D) flows, with D < 1,000. A modified version of particle image velocimetry was developed to enable the measurement of the velocity field in dies of arbitrary cross section. During the measurement process, tracer particles were simultaneously illuminated by both a focused laser beam locally and a lamp globally. Only those particles that passed through the laser beam were taken into account. The beam was scanned to achieve full field measurements. This method of measurement allowed us to find the location of a particle in the direction of the optical axis of the lens, i.e. that which makes the particle image on the CCD detector of the video camera. A device employing this method was designed and used to measure velocity profiles. The results of these measurements in two cross sections of the square die, at three values of pressure, are presented. The velocity was defined as the ratio of displacement to the elapsed time during which this displacement occurred. Errors in measurements of the coordinates and the observation time of particles were estimated as ±20 μm and less than 0.1%, respectively. A large plateau in the axial velocity profile was found at relatively small Deborah numbers, e.g. D ≈ 28. In flows with higher Deborah numbers, e.g. D ≈ 766, an almost flat velocity profile was detected. Two components of velocity, one longitudinal and one transversal, were measured simultaneously. However, the transversal component appeared to be less than the error of measurements and less than 1% of the axial velocity. Received: 4 August 1998 Accepted: 5 April 1999     

Heat transfer measurements in fully turbulent flows: basic investigations with an advanced thin foil triple sensor

In a former article in this journal a double layer hot film with two 10 μm nickel foils, separated by a 25 μm polyimide foil was introduced as a multi-purpose sensor. Each foil can be operated as a (calibrated) temperature sensor in its passive mode by imposing an electric current small enough to avoid heating by dissipation of electrical energy. Alternatively, however, each foil can also serve as a heater in an active mode with electric currents high enough to cause Joule heating. This double foil sensor can be used as a conventional heat flux sensor in its passive mode when mounted on an externally heated surface. In fully turbulent flows it alternatively can be operated in an active mode on a cold, i.e. not externally heated surface. Then, by heating the upper foil, a local heat transfer is initiated from which the local heat transfer coefficient h can be determined, once the lower foil is heated to the same temperature as the upper one, thus acting as a counter-heater. For further investigations with respect to the underlying sensor concept a triple sensor has been built which consists of three double layer film sensors very close to each other. Various aspects of heat transfer measurements in active modes can be addressed by this sensor.     

Transient elongational viscosities of aqueous polyacrylamide solutions measured with an optical rheometer

An anionic polyacrylamide solution was characterized in elongational flow by combining laser-Doppler velocimetry to determine the strain rate in the flow direction and the two-color flow-induced birefringence method to measure the first normal stress difference along the axial centerline of a hyperbolic die. The elongational rate was constant along the axial centerline of the planar hyperbolic die as long as vortices at the die entrance did not occur. The transient elongational viscosity μ ⁺ was determined as a function of the elongational rate. The parameters varied are the Hencky strain rate and the polymer concentration. μ ⁺ showed a pronounced increase over the linear viscoelastic behavior above critical Hencky strains of 1.2 to 1.5; that is, a significant strain hardening could be observed for polyacrylamide solutions. This strain hardening is stronger the higher the elongational rate. A slight enhancement of strain hardening was found by increasing the concentration from 0.5 to 1 g/l. The stress optical coefficient was determined as 1.8 × 10⁻⁷ Pa⁻¹ (0.5 g/l) and 1.2 × 10⁻⁷ Pa⁻¹ (1 g/l).

Squeezing flow of semi liquid foods between parallel Teflon coated plates

Samples of commercial tomato paste, low fat mayonnaise and mustard about 6–8 mm thick were squeezed to 0.8 mm at various speeds between 5 mm min⁻¹ and 25 mm min⁻¹ between Teflon-coated parallel plates 127 mm in diameter using an Instron UTM Model 5542. All the log force vs log height relationships had a clearly identified linear region. This indicated that a dominant squeezing flow regime was achieved at about 3 mm height, and that the machine has the proper stiffness to perform the tests. The stress level at a pre-selected height in this region is a measure of consistency, sensitive enough to distinguish between products of different brands. The residual stress after relaxation for about 2 min was on order of 10–50% of the initial stress, an indication that all three foods have a considerable structural integrity. In all three products there was a considerable discrepancy between the observed rate effects and predictions based on a pseudoplastic (power law) model. It could be described by the empirical relation (F_v1 − F_R)/(F_v2 − F_R)=(V₁/V₂)^m where F_v1 and F_v2 are the forces at the given displacement reached at speeds v₁ and v₂ respectively, F_R is the residual force after relaxation (found to be practically rate independent), and m is a constant of the order of 0.15–0.33, independent of the compression velocities ratio but characteristic of the food and brand. The calculated elongational viscosity was not a unique function of biaxial strain rate. To a certain extent, this was probably due to imperfect lubrication. But it was also a manifestation of these products considerable structural integrity which cannot be accounted for by models developed for ideal liquids. Received: 1 November 1999 Accepted: 2 May 2000     

Strain hardening in bent copper foils

A series of systematic tensile and microbend tests were conducted on copper foil specimens with different thicknesses. The specimens were made of a copper foil having almost unidirectional crystal orientations that was considered to be nearly single-crystal. In order to investigate the effects of slip system interactions, two different crystal orientations relative to the tensile direction were considered in the tests: one is close to coplanar double-slip orientation, and the other is close to the ideal cube orientation (the tensile direction nearly coincides to [0 0 1]) that yields multi-planar multi-slip deformation. We extended the microbend test method to include the reversal of bending, and we attempted to divide the total amount of strain-hardening into isotropic and kinematic hardening components. In the tensile tests, no systematic tendency of size dependence was observed. In the microbend tests, size-dependent kinematic hardening behavior was observed for both the crystal orientations, while size dependence of isotropic hardening was observed only for the multi-planar multi-slip case. We introduce an extended crystal plasticity model that accounts for the effects of the geometrically necessary dislocations (GNDs), which correspond to the spatial gradients of crystallographic slips. Through numerical simulations performed using the model, the origin of the size-dependent behavior observed in the microbend tests is discussed.     

Lattice orientation effects on void growth and coalescence in fcc single crystals

Void growth and coalescence in fcc single crystals were studied using crystal plasticity under uniaxial and biaxial loading conditions and various orientations of the crystalline lattice. A 2D plane strain unit cell with one and two cylindrical voids was employed using three-dimensional 12 potentially active slip systems. The results were compared to five representative orientations of the tensile axis on the stereographic triangle. For uniaxial tension conditions, the void volume fraction increase under the applied load is strongly dependent on the crystallographic orientation with respect to the tensile axis. For some orientations of the tensile axis, such as [1 0 0] or [1 1 0], the voids exhibited a growth rate twice as fast compared with other orientations ([1 0 0], [2 1 1]). Void growth and coalescence simulations under uniaxial loading indicated that during deformation along some orientations with asymmetry of the slip systems, the voids experienced rotation and shape distortion, due mainly to lattice reorientation. Coalescence effects are shown to diminish the influence of lattice orientation on the void volume fraction increase, but noteworthy differences are still present. Under biaxial loading conditions, practically all differences in the void volume fraction for different orientations of the tensile axes during void growth vanish. These results lead to the conclusion that at microstructural length scales in regions under intense biaxiality/triaxiality conditions, such as crack tip or notched regions, the plastic anisotropy due to the initial lattice orientation has only a minor role in influencing the void growth rate. In such situations, void growth and coalescence are mainly determined by the stress triaxiality, the magnitude of accumulated strain, and the spatial localization of such plastic strains.     

Three-dimensional micro-PTV using deconvolution microscopy

A three-dimensional micro-particle tracking velocimetry (micro-PTV) scheme is presented using a single camera with deconvolution microscopy. This method devises tracking of the line-of-sight (z) flow vectors by correlating the diffraction pattern ring size variations with the defocusing distances of small particle locations. The working principle is based on optical serial sectioning microscopy, or equivalently deconvolution microscopy, that records images of an infinitesimally small particle, and generates a point-spread function of the three-dimensional diffraction patterns. A new image-processing algorithm has also been developed to digitally identify the center locations and measure the radii of the diffraction rings, which allows simultaneous tracking of all three-vector components. The developed PTV technique uses a 40×, 0.75 NA dry objective lens with 500-nm fluorescent seeding particles of SG=1.05, and successfully measures the fully three-dimensional fields flowing over a spherical obstacle snuggly fitted inside a 100 μm × 100 μm micro-channel. The volumetric measurement resolution of the present system is equivalent to a 5.16 μm × 5.16 μm × 5.16 μm cube, and the overall measurement uncertainty for single-point velocity vector detection is estimated to ±7.58%.

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The effect of mixing particles of different size on the electrorheological response under steady shear flow

 The effect of mixing particles of different sizes on the electrorheological response of suspensions under steady shear flow was investigated. Two sizes, 15 μm and 50 μm, of monodisperse spherical sulfonated poly(styrene-co-divinylbenzene) particles were used. Several electrorheological fluids were made containing different proportions of small and large particles dispersed in silicone oil, but with constant overall particulate concentration. It was found that the mixed size system produced the highest electrorheological response under the shear rates used (10 s⁻¹ to 500 s⁻¹), which is the opposite trend to previous studies of bimodal systems with larger size ratios. Received: 21 December 2000 Accepted: 29 March 2001     

Bentonite slurries—zeta potential,yield stress,adsorbed additive and time-dependent behaviour

Bentonite clay is a vital ingredient of drilling mud. The time-dependent and high shear thinning yield stress behaviour of drilling mud is essential for maintaining wellbore stability and to remove cuttings, cool and clean the drill bit of debris. As-prepared 3, 5 and 7 wt.% bentonite clay slurries displayed time-dependent behaviour where the yield stress (measured after quick stirring) decreased with time of rest. An equilibrium value is reached after 24 h. Despite the low solids concentration, the yield stress is already relatively high and is displayed at all pH level. The yield stress is maximum at pH 2 and minimum at pH ∼ 7. This yield stress is due to the formation of gel structure by the swelling clay particles. However the addition of phosphate additives such as (PO₃)^19 −, (P₃O₁₀)^5 − and (P₂O₇)^4 − completely dispersed the clay slurries at pH above 6. At pH below 6, yield stress is still present but is 3-folds smaller than that of the pure bentonite slurry. With phosphate additives, the magnitude of the critical zeta potential at the complete dispersion pH is ca 48 mV. However for the pure bentonite, the slurry remained flocculated at zeta potential of >50 mV in magnitude. Interestingly, (P₂O₇)^4 − anions is more effective than the other two phosphate additives in reducing the yield stress at low pH, ∼ 2.0.