Demonstrating the potential of Accurate Absolute Cross-grain Stress and Orientation correlation using Electron Backscatter Diffraction

We report a first exploration of High-angular-Resolution Electron Backscatter Diffraction, without using simulated Electron Backscatter Diffraction patterns as a reference, for absolute stress and orientation measurements in polycrystalline materials. By co-correlating the pattern center and fully exploiting crystal symmetry and plane-stress, simultaneous correlation of all overlapping regions of interest in multiple direct-electron-detector, energy-filtered Electron Backscatter Diffraction patterns is achieved. The potential for highly accurate measurement of absolute stress, crystal orientation and pattern center is demonstrated on a virtual polycrystalline case-study, showing errors respectively below 20 MPa (or 1e-4 in strain), 7e-5 rad and 0.06 pixels.Comment: Manuscript as accepted for publication in Scripta Materiali

Cool, Dry, Nano-scale DIC Patterning of Delicate, Heterogeneous, Non-planar Specimens by Micro-mist Nebulization

Background: Application of patterns to enable high-resolution Digital Image Correlation (DIC) at the small scale (μm/nm) is known to be very challenging as techniques developed for the macro- and mesoscale, such as spray painting, cannot be scaled down directly. Moreover, existing nano-patterning techniques all rely on harsh processing steps, based on high temperature, chemicals, physical contact, liquids, and/or high vacuum, that can easily damage fragile, small-scale, free-standing and/or hygro-sensitive specimens, such as MEMS or biological samples. Objective: To present a straightforward, inexpensive technique specially designed for nano-patterning highly delicate specimens for high-resolution DIC. Methods: The technique consists in a well-controlled nebulized micro-mist, containing predominantly no more than one nanoparticle per mist droplet. The micro-mist is subsequently dried, resulting in a flow of individual nanoparticles that are deposited on the specimen surface at near-room temperature. By having single nanoparticles falling on the specimen surface, the notoriously challenging task of controlling nanoparticle-nanoparticle and nanoparticle-surface interactions as a result of the complex droplet drying dynamics, e.g., in drop-casting, is circumvented. Results: High-quality patterns are demonstrated for a number of challenging cases of physically and chemically sensitive specimens with nanoparticles from 1 μm down to 50 nm in diameter. It is shown that the pattern can easily be scaled within (and probably beyond) this range, which is of special interest for micromechanical testing using in-situ microscopic imaging techniques, such as high-magnification optical microscopy, optical profilometry, atomic force microscopy, and scanning electron microscopy, etc. Conclusions: Delicate specimens can conveniently be patterned at near-room temperature (∼ 37 ∘C), without exposure to chemicals, physical contact or vacuum, while the pattern density and speckle size can be easily tuned.</p

One‐step deposition of nano‐to‐micron‐scalable, high‐quality digital image correlation patterns for high‐strain in‐situ multi‐microscopy testing

Digital image correlation (DIC) is of vital importance in the field of experimental mechanics, yet producing suitable DIC patterns for demanding in-situ (micro)mechanical tests remains challenging, especially for ultrafine patterns, despite the large number of patterning techniques reported in the literature. Therefore, we propose a simple, flexible, one-step technique (only requiring a conventional physical vapour deposition machine) to obtain scalable, high-quality, robust DIC patterns, suitable for a range of microscopic techniques, by deposition of a low-melting temperature solder alloy in the so-called island growth mode, without elevating the substrate temperature. Proof of principle is shown by (near-)room temperature deposition of InSn patterns, yielding highly dense, homogeneous DIC patterns over large areas with a feature size that can be tuned from as small as ~10 nm to ~2 μm and with control over the feature shape and density by changing the deposition parameters. Pattern optimisation, in terms of feature size, density, and contrast, is demonstrated for imaging with atomic force microscopy, scanning electron microscopy, optical profilometry, and optical microscopy. Moreover, the performance of the InSn DIC patterns and their robustness to large deformations is validated in two challenging case studies of in-situ micromechanical testing: (a) self-adaptive isogeometric digital height correlation of optical surface height profiles of a coarse, bimodal InSn pattern providing microscopic 3D deformation fields (illustrated for delamination of Al stretchable interconnects on a PI substrate) and (b) DIC on scanning electron microscopy images of a much finer InSn pattern allowing quantification of high strains near fracture locations (illustrated for rupture of a polycrystalline Fe foil). As such, the high controllability, performance, and scalability of the DIC patterns, created by island growth of a solder alloy, offer a promising step towards more routine DIC-based in-situ micromechanical testing.</p

Effect of restrained versus free drying on hygro-expansion of hardwood and softwood fibers and paper handsheet

Earlier work on the hygro-expansion of paper states that the larger hygro-expansivity of freely compared to restrained dried handsheets is due to structural differences between the fibers inside the handsheet. To study this hypothesis, first, the hygro-expansion of freely and restrained dried, hardwood and softwood handsheets has been characterized. Subsequently, the transient full-field hygro-expansion (longitudinal, transverse, and shear strain) of fibers extracted from these handsheets was measured using global digital height correlation, from which the micro-fibril angle was deduced. The hygro-expansivity of each individual fiber was tested before and after a wetting period, during which the fiber’s moisture content is maximized, to analyze if a restrained dried fiber can “transform” into a freely dried fiber. It was found that the longitudinal hygro-expansion of the freely dried fibers is significantly larger than the restrained dried fibers, consistent with the sheet-scale differences. The difference in micro-fibril angle between the freely and restrained dried fibers is a possible explanation for this difference, but merely for the hardwood fibers, which are able to “transform” to freely dried fibers after being soaked in water. In contrast, this “transformation” does not happen in softwood fibers, even after full immersion in water for a day. Various mechanisms have been studied to explain the observations on freely and restrained dried hardwood and softwood, fiber and handsheets including analysis of the fibers’ lumen and cross-sectional shape. The presented results and discussion deepens the understanding of the differences between freely and restrained dried handsheets.</p

Effect of restrained versus free drying on hygro-expansion of hardwood and softwood fibers and paper handsheet

Earlier work on the hygro-expansion of paper states that the larger hygro-expansivity of freely compared to restrained dried handsheets is due to structural differences between the fibers inside the handsheet. To study this hypothesis, first, the hygro-expansion of freely and restrained dried, hardwood and softwood handsheets has been characterized. Subsequently, the transient full-field hygro-expansion (longitudinal, transverse, and shear strain) of fibers extracted from these handsheets was measured using global digital height correlation, from which the micro-fibril angle was deduced. The hygro-expansivity of each individual fiber was tested before and after a wetting period, during which the fiber’s moisture content is maximized, to analyze if a restrained dried fiber can “transform” into a freely dried fiber. It was found that the longitudinal hygro-expansion of the freely dried fibers is significantly larger than the restrained dried fibers, consistent with the sheet-scale differences. The difference in micro-fibril angle between the freely and restrained dried fibers is a possible explanation for this difference, but merely for the hardwood fibers, which are able to “transform” to freely dried fibers after being soaked in water. In contrast, this “transformation” does not happen in softwood fibers, even after full immersion in water for a day. Various mechanisms have been studied to explain the observations on freely and restrained dried hardwood and softwood, fiber and handsheets including analysis of the fibers’ lumen and cross-sectional shape. The presented results and discussion deepens the understanding of the differences between freely and restrained dried handsheets.</p

Full-field hygroscopic characterization of paper inter-fiber bonds and the implications on network hygro-expansivity

The state-of-the-art in paper micro-mechanics calls for novel experimental data covering the full-field hygro-expansion of inter-fiber bonds, i.e., the 3D morphological changes and inter-fiber interactions. Therefore, a recently developed full-field single fiber hygro-expansion measurement methodology based on global digital height correlation is extended to orthogonal inter-fiber bonds, to investigate their full-field quasi-3D hygroscopic behavior. A sample holder has been developed which enables the quasi-3D characterization of the initial geometry of individual inter-fiber bonds, including the fiber thickness and width along the length of the fibers as well as the degree of wrap around and contact area of the bond, which are vital for understanding the inter-fiber bond hygro-mechanics. Full-field hygroscopic testing reveals the inter-fiber interactions: (i) the transverse hygro-expansion of each fiber strongly reduces when approaching the bonded area, due to the significantly lower longitudinal hygro-expansion of the other bonded fiber. (ii) The relatively large transverse strain of one fiber stretches the other crossing fiber in its longitudinal direction, thereby significantly contributing to the sheet scale hygro-expansion. (iii) Out-of-plane bending is observed in the bonded region which is driven by the significant difference in transverse and longitudinal hygro-expansion of, respectively, the top and bottom fiber constituting the bond. A bi-layer laminate model is employed to rationalize the bending deformation and an adequate match is found with the experimental data. Under the assumption of zero bending, which represents constrained inter-fiber bonds inside a paper sheet, the model can predict the contribution of the transverse strain in the bonded regions to the sheet-scale hygro-expansion.</p

Ultra-Stretchable Interconnects for High-Density Stretchable Electronics

The exciting field of stretchable electronics (SE) promises numerous novel applications, particularly in-body and medical diagnostics devices. However, future advanced SE miniature devices will require high-density, extremely stretchable interconnects with micron-scale footprints, which calls for proven standardized (complementary metal-oxide semiconductor (CMOS)-type) process recipes using bulk integrated circuit (IC) microfabrication tools and fine-pitch photolithography patterning. Here, we address this combined challenge of microfabrication with extreme stretchability for high-density SE devices by introducing CMOS-enabled, free-standing, miniaturized interconnect structures that fully exploit their 3D kinematic freedom through an interplay of buckling, torsion, and bending to maximize stretchability. Integration with standard CMOS-type batch processing is assured by utilizing the Flex-to-Rigid (F2R) post-processing technology to make the back-end-of-line interconnect structures free-standing, thus enabling the routine microfabrication of highly-stretchable interconnects. The performance and reproducibility of these free-standing structures is promising: an elastic stretch beyond 2000% and ultimate (plastic) stretch beyond 3000%, with 10 million cycles at 1000% stretch with <1% resistance change. This generic technology provides a new route to exciting highly-stretchable miniature devices.Comment: 13 pages, 5 figure, journal publicatio

Experimental characterisation of the local mechanical behaviour of cellulose fibres: an in‑situ micro‑profilometry approach

The accurate mechanical characterisation of fibres of micrometric length is a challenging task, especially in the case of organically-formed fibres that naturally exhibit considerable irregularities along the longitudinal fibre direction. The present paper proposes a novel experimental methodology for the evaluation of the local mechanical behaviour of organically-formed (aged and unaged) and regenerated cellulose fibres, which is based on in-situ micro-tensile testing combined with optical profilometry. In order to accurately determine the cross-sectional area profile of a cellulose fibre specimen, optical profilometry is performed both at the top and bottom surfaces of the fibre. The evolution of the local stress at specific fibre locations is next determined from the force value recorded during the tensile test and the local cross-sectional area. An accurate measurement of the corresponding local strain is obtained by using Global Digital Height Correlation (GDHC), thus resulting in multiple, local stress--strain curves per fibre, from which local tensile strengths, elastic moduli, and strains at fracture can be deduced. Since the variations in the geometrical and material properties within an individual fibre are comparable to those observed across fibres, the proposed methodology is able to attain statistically representative measurement data from just one, or a small number of fibre samples. This makes the experimental methodology very suitable for the mechanical analysis of fibres taken from valuable and historical objects, for which typically a limited number of samples is available. It is further demonstrated that the accuracy of the measurement data obtained by the present, local measuring technique may be significantly higher than for a common, global measuring technique since possible errors induced by fibre slip at the grip surfaces are avoided

A bulge test based methodology for characterizing ultra-thin buckled membranes

Buckled membranes become ever more important with further miniaturization and development of ultra-thin film based systems. It is well established that the bulge test method, generally considered the gold standard for characterizing freestanding thin films, is unsuited to characterize buckled membranes, because of compressive residual stresses and a negligible out-of-plane bending stiffness. When pressurized, buckled membranes immediately start entering the ripple regime, but they typically plastically deform or fracture before reaching the cylindrical regime. In this paper the bulge test method is extended to enable characterization of buckled freestanding ultra-thin membranes in the ripple regime. In a combined experimental-numerical approach, the advanced technique of digital height correlation was first extended towards the sub-micron scale, to enable measurement of the highly varying local 3D strain and curvature fields on top of a single ripple in a total region of interest as small as approximately 25 microns. Subsequently, a finite element (FE) model was set up to analyze the post-buckled membrane under pressure loading. In the seemingly complex ripple configuration, a suitable combination of local region of interest and pressure range was identified for which the stress-strain state can be extracted from the local strain and curvature fields. This enables the extraction of both the Young's modulus and Poisson's ratio from a single bulge sample, contrary to the conventional bulge test method. Virtual experiments demonstrate the feasibility of the approach, while real proof of principle of the method was demonstrated for fragile specimens with rather narrow ( approximately 25 microns) ripples