The mechanisms of plastic deformation are investigated using different characterization tools as scanning electron microscopy (SEM), transmission electron microscopy, or synchrotron‐based X‐ray techniques like Laue microdiffraction (μLaue). However, structural information can be limited to the specimen surface (SEM), to extremely thin samples (TEM), or depth averaging (μLaue). Until today, a nondestructive in situ investigation of a dislocation population, and de facto, the determination of the local stress tensor in bulk samples, remain challenging. To decompose the depth‐integrated μLaue signals, the so‐called “differential aperture X‐ray microscopy” (DAXM), allowing the 3D determination of the local structural crystal properties, is used. Using this approach, the local crystallographic phase, orientation, and the elastic strain tensor are obtained with 1 μm3 voxel size. In order to accomplish the experiment, a protocol and a new combined in situ mechanical testing rig with a DAXM microscope is created. The experiment is conducted on a severely bent focused ion beam copper single‐crystal microcantilever (10 × 10 × 25 μm3). The local deviatoric strain tensor and the local lattice curvature in the deformed sample are analyzed in 3D. The advantages and resolution limits of the technique are discussed in detail.
A series of Al and Al/Al2O3thin‐film multilayer structures on flexible polymer substrates are fabricated with a unique deposition chamber combining magnetron sputtering (Al) and atomic layer deposition (ALD, Al2O3, nominal thickness 2.4–9.4 nm) without breaking vacuum and thoroughly characterized using transmission electron microscopy (TEM). The electromechanical behavior of the multilayers and Al reference films is investigated in tension with in situ X‐ray diffraction (XRD) and four‐point probe resistance measurements. All films exhibit excellent interfacial adhesion, with no delamination in the investigated strain range (12%). For the first time, an adhesion‐promoting naturally forming amorphous interlayer is confirmed for thin films sputter deposited onto polymers under laboratory conditions. The evolution of Al film stresses and electrical resistance reveal changes in the deformation behavior as a function of oxide thickness. Strengthening of Al is observed with increasing oxide thickness. Significant embrittlement can be avoided for oxide layer thicknesses ≤2.4 nm.
Microwires have become of increasing interest for the miniaturization of structural components. A profound understanding of the deformation behavior of microwires is important for the assessment of their applicability and lifetime in specific components. In particular, the deformation behavior under torsional loading and the associated microstructure evolution are of interest. The exact involvement of individual slip systems and their activities in the complex stress field under torsional loading are mostly unknown. In this paper, the microstructure evolution of single crystalline gold microwires under torsion have been analyzed for the high-symmetry crystal orientations 〈100〉, 〈110〉, and 〈111〉 using simulation and experimental results. It is shown that a classification of the slip systems can be derived a priori by theoretical considerations. It is found, that the slip system activity, stress relaxation mechanism, as well as screw and edge composition of the piled-up dislocation density depends on specific slip system groups. Furthermore, the misorientation and its rotational axes including the identification of the slip system activities are discussed.
Complex stress states due to torsion lead to dislocation structures characteristic for the chosen torsion axis. The formation mechanism of these structures and the link to the overall plastic deformation are unclear. Experiments allow the analysis of cross sections only ex situ or are limited in spacial resolution which prohibits the identification of the substructures which form within the volume. Discrete dislocation dynamics simulations give full access to the dislocation structure and their evolution in time. By combining both approaches and comparing similar measures the dislocation structure formation in torsion loading of micro wires is explained. For the ⟨100⟩ torsion axis, slip traces spanning the entire sample in both simulation and experiment are observed. They are caused by collective motion of dislocations on adjacent slip planes. Thus these slip traces are not atomically sharp. Torsion loading around a ⟨111⟩ axis favors plasticity on the primary slip planes perpendicular to the torsion axis and dislocation storage through cross-slip and subsequent collinear junction formation. Resulting hexagonal dislocation networks patches are small angle grain boundaries. Both, experiments and discrete dislocation simulations show that dislocations cross the neutral fiber. This feature is discussed in light of the limits of continuum descriptions of plasticity.
Many different methods, such as screen printing, gravure, flexography, inkjet etc., have been employed to print electronic devices. Depending on the type and performance of the devices, processing is done at low or high temperature using precursor- or particle-based inks. As a result of the processing details, devices can be fabricated on flexible or non-flexible substrates, depending on their temperature stability. Furthermore, in order to reduce the operating voltage, printed devices rely on high-capacitance electrolytes rather than on dielectrics. The printing resolution and speed are two of the major challenging parameters for printed electronics. High-resolution printing produces small-size printed devices and high-integration densities with minimum materials consumption. However, most printing methods have resolutions between 20 and 50 μm. Printing resolutions close to 1 μm have also been achieved with optimized process conditions and better printing technology.
Printed and flexible metal‐oxide transistor technology has recently demonstrated great promise due to its high performance and robust mechanical stability. Herein, fully printed inverter structures using electrolyte‐gated oxide transistors on a flexible polyimide (PI) substrate are discussed in detail. Conductive graphene ink is printed as the passive structures and interconnects. The additive printed transistors on PI substrates show an ratio of and show mobilities similar to the state‐of‐the‐art printed transistors on rigid substrates. Printed meander structures of graphene are used as pull‐up resistances in a transistor–resistor logic to create fully printed inverters. The printed and flexible inverters show a signal gain of 3.5 and a propagation delay of 30 ms. These printed inverters are able to withstand a tensile strain of 1.5% following more than 200 cycles of mechanical bending. The stability of the electrical direct current (DC) properties has been observed over a period of 5 weeks. These oxide transistor‐based fully printed inverters are relevant for digital printing methods which could be implemented into roll‐to‐roll processes.
The microstructure contribution to the very low fracture toughness of freestanding metallic thin films was investigated by bulge fracture tests on 200-nm-thick {100} single-crystalline and polycrystalline silver films. The single-crystalline films exhibited a significantly lower fracture toughness value (KIC = 0.88 MPa m1/2) than their polycrystalline counterparts (KIC = 1.45 MPa m1/2), which was rationalized by the observation of an unusual crack initiation behavior-characterized by twinning in front of the notch tip-during in situ testing in the atomic force microscope. Twinning was also observed as a dominant deformation mechanism in atomistic simulations. This twinning tendency is explained by comparing the resolved shear stresses acting on the leading partial dislocation and the full dislocation, which allows to develop a size- and orientation-dependent twinning criterion. The fracture toughness of polycrystalline samples was found to be higher because of the energy dissipation associated with full dislocation plasticity and because of crack meandering along grain boundaries.
With progressing miniaturization of modern electronic devices, interconnects become increasingly smaller. Additionally, as electronic devices move away from rigid substrates toward flexible ones, understanding their mechanical and structural stability is becoming crucial. In this work, a thorough mechanical characterization of copper thin films deposited on flexible substrates was performed with two techniques, namely well-established synchrotron X-ray diffraction (sXRD) and the rather new usage of reflectance anisotropy spectroscopy (RAS) for mechanical characterization of thin films. The comparison of these two techniques shows that RAS can be reliably used for the accurate and prompt yield stress measurements. The acquisition time of RAS is much faster than that of sXRD: 1 second per data point compared to several seconds per data point for sXRD experiments. Moreover, the signal-to-noise ratio of the RAS data is much higher than that of the sXRD. Our results show that yield stress of Cu films increases with the decrease in the film thickness, going from 352 MPa for a 500 nm films to 793 MPa for a 50 nm thick film. Microstructure analyses of the films by electron microscopy allowed correlation of the mechanical behavior of the films to their grain morphologies. We have shown that RAS can supplement sXRD measurements due to a faster acquisition rate which allowed us to analyze the creep behavior of our copper thin film at different strain rates.
We present all-solution processed, indium tin oxide-free organic solar cells on mechanically flexible polyethylene terephthalate (PET) substrates with power conversion efficiencies up to 4.8%. The mechanical properties of the devices are dictated by the electrodes from either metal-organic silver inks or a combination of poly(3,4-ethylenedioxythiophene):poly(4-styrenesulfonate) and silver nanowires. Both electrodes can sustain high tensile strains. The influence of mechanical strain on the solar cell performance was experimentally studied in situ by measuring the J–V curves of elongated samples under illumination. At a strain of 14%, we still observed 90% of the initial device power output. At higher strain, crack formation within the electrodes was identified as the origin for device failure.
We utilized synchrotron-based in-situ diffraction and dominant shear deformation to identify, dissect, and quantify the relevant deformation mechanisms in nanocrystalline $\mathrm{Pd}_{90}\mathrm{Au}_{10}$ in the limiting case of grain sizes at or below 10 nm. We could identify lattice and grain boundary elasticity, shear shuffling operating in the core region of grain boundaries, stress driven grain boundary migration, and dislocation shear along lattice planes to contribute, however, with significantly different and nontrivial stress-dependent shares to overall deformation. Regarding lattice elasticity, we find that Hookean linear elasticity prevailed up to the maximal stress value of $\approx$ 1.6 GPa. Shear shuffling that propagates strain at/along grain boundaries increases progressively with increasing load to carry about two thirds of the overall strain in the regime of macroplasticity. Stress driven grain boundary migration requires overcoming a threshold stress slightly below the yield stress of $\approx$ 1.4 GPa and contributes a share of $\approx$ 10% to overall strain. Appreciable dislocation activity begins at a stress value of $\approx$ 0.9 GPa to then increase and eventually propagate a maximal share of $\approx$ 15% to overall strain. In the stress regime below 0.9 GPa, which is characterized by a markedly decreasing tangent modulus, shear shuffling and lattice- and grain boundary elasticity operate exclusively. The material response in this regime seems indicative of nonlinear viscous behavior rather than being correlated with work- or strain hardening as observed in conventional fcc metals.
The thickness dependence of the electrical stability under monotonic and cyclic tensile loading is investigated for Cu films on polymer substrates. As for monotonic tensile deformation, thicker films show better stability than thinner films due to their higher ductility and the larger capability of strain accommodation. For the fatigue resistance, however, a more complex behavior was observed depending on the amount of the applied strain. For low strain amplitude in the high cycle fatigue (HCF) regime, thinner films exhibit longer fatigue life because the larger strength of thinner films suppresses dislocation movement and damage nucleation. However, for high strain amplitudes in the low cycle fatigue (LCF) regime, the fatigue life for thinner films is drastically reduced compared to thicker films. It is shown that fatigue coefficients in the LCF regime can be obtained when applying the Coffin–Manson relationship.
Fatigue behavior of 100nm and 1.0µm thick Cu films with 10nm Ta passivation layers has been studied using cyclic tensile testing. The results show that Ta capping-layer has influences on fatigue damage by suppression of extrusion formation and, thereby, improved the fatigue life dramatically in the 1.0µm thick Cu film, but does not change the fatigue life of 100nm thick Cu film for which crack formation is the dominant damage mechanism.
The development of highly conductive metallic electrodes with long-term reliability is in great demand for real industrialization of flexible electronics, which undergo repeated mechanical deformation during service. In the case of vacuum-deposited metallic electrodes, adequate conductivity is provided, but it degrades gradually during cyclic mechanical deformation. Here, we demonstrate a long-term reliable Ag electrode by inkjet printing. The electrical conductivity and the mechanical reliability during cyclic bending are investigated with respect to the nanoporous microstructure caused by post heat treatment, and are compared to those of evaporated Ag films of the same thickness. It is shown that there is an optimized nanoporous microstructure for inkjet-printed Ag films, which provides a high conductivity and improved reliability. It is argued that the nanoporous microstructure ensures connectivity within the particle network and at the same time reduces plastic deformation and the formation of fatigue damage. This concept provides a new guideline to develop an efficient method for highly conductive and reliable metallic electrodes for flexible electronics.
Nanocrystalline thin films on compliant substrates become increasingly important for the development of flexible electronic devices. In this study, nanocrystalline AuCu thin films on polyimide substrate were tested in tension while using a synchrotron-based in situ testing technique. Analysis of X-ray diffraction profiles allowed identifying the underlying deformation mechanisms. Initially, elastic and microplastic deformation is observed, followed by dislocation-mediated shear band formation, and eventually macroscopic crack formation. Particularly the influence of alloy composition, heat-treatment, and test temperature were investigated. Generally, a highly ductile behavior is observed. However, high Cu concentrations, annealing, and/or large plastic strains lead to localized deformation and hence reduced ductility. On the other hand, enhanced test temperature allows for a delocalized deformation and extended ductility.
We utilized synchrotron-based in-situ diffraction and dominant shear deformation to identify, dissect, and quantify the relevant deformation mechanisms in nanocrystalline $\mathrm{Pd}_{90}\mathrm{Au}_{10}$ in the limiting case of grain sizes at or below 10 nm. We could identify lattice and grain boundary elasticity, shear shuffling operating in the core region of grain boundaries, stress driven grain boundary migration, and dislocation shear along lattice planes to contribute, however, with significantly different and nontrivial stress-dependent shares to overall deformation. Regarding lattice elasticity, we find that Hookean linear elasticity prevailed up to the maximal stress value of $\approx$ 1.6 GPa. Shear shuffling that propagates strain at/along grain boundaries increases progressively with increasing load to carry about two thirds of the overall strain in the regime of macroplasticity. Stress driven grain boundary migration requires overcoming a threshold stress slightly below the yield stress of $\approx$ 1.4 GPa and contributes a share of $\approx$ 10% to overall strain. Appreciable dislocation activity begins at a stress value of $\approx$ 0.9 GPa to then increase and eventually propagate a maximal share of $\approx$ 15% to overall strain. In the stress regime below 0.9 GPa, which is characterized by a markedly decreasing tangent modulus, shear shuffling and lattice- and grain boundary elasticity operate exclusively. The material response in this regime seems indicative of nonlinear viscous behavior rather than being correlated with work- or strain hardening as observed in conventional fcc metals.
By use of X-ray diffraction, the load-bearing contributions of nanometer-thick Cu and Nb layers in Cu/Nb multilayer composites are isolated. The Cu bears higher stresses at failure and the Nb bears lower stresses at failure with decreasing Cu layer thickness. The Cu and Nb layers appear to have independent deformation mechanisms.
Nanocrystalline (nc) materials possess unique mechanical properties, such as very high strength. However, an understanding of the deformation mechanisms and the succession of related microscopic processes that occur during deformation is still incomplete. We used synchrotron-based in situ compression testing to investigate the sequence of deformation mechanisms emerging in bulk nc nickel with a grain size of 30nm. The study was accompanied by high-resolution grain size analysis and crystal orientation mapping using transmission electron microscopy. Regardless of the initial microstructure, the deformation behavior of electrodeposited nc Ni is initiated by inhomogeneous elastic lattice straining and its accommodation within the grain boundary network, followed by the onset of dislocation plasticity, which was inferred from texture evolution, and stress-driven grain growth. This observation indicates that deformation in nc metals is governed by a succession of different, partly overlapping mechanisms. It is estimated that intragranular dislocation plasticity contributes only about 40% to the overall deformation.