Patric A. Gruber

Tensile testing of ultrathin polycrystalline films: A synchrotron-based technique

The mechanical properties of metallic thin films on the nanoscale acquire increasingly more importance as applications in microelectromechanical systems/NEMS as well as microelectronics have reached this size scale. Here, we present a synchrotron x-ray diffraction technique by which it is possible to characterize the evolution of mechanical stress in a metallic film thinner than 100 nm at measurement times shorter than 60 s per data point. This high data acquisition rate is achieved because no relative motions or tilting of specimen, x-ray source and detector (a large-area charge coupled device camera) are required. The technique comprises an initial “sin2 ψ” measurement to establish the absolute stress values followed by periodic “sin2 φ” measurements during straining to determine stress increments. We describe an experimental setup established at the synchrotron radiation source ANKA (Karlsruhe, Germany) which is specifically suited for monitoring the stress evolution during in situ tensile tests on thi...

Strain bursts in plastically deforming molybdenum micro- and nanopillars

Plastic deformation of micron and sub-micron scale specimens is characterized by intermittent sequences of large strain bursts (dislocation avalanches) which are separated by regions of near-elastic loading. In the present investigation we perform a statistical characterization of strain bursts observed in stress-controlled compressive deformation of monocrystalline molybdenum micropillars. We characterize the bursts in terms of the associated elongation increments and peak deformation rates, and demonstrate that these quantities follow power-law distributions that do not depend on specimen orientation or stress rate. We also investigate the statistics of stress increments in between the bursts, which are found to be Weibull distributed and exhibit a characteristic size effect. We discuss our findings in view of observations of deformation bursts in other materials, such as face-centred cubic and hexagonal metals.

Effect of pre-straining on the size effect in molybdenum pillars

The effect of prior deformation on mechanical behavior as a function of size is investigated for body-centered cubic (bcc) molybdenum (Mo) pillars. Experiments were performed using focused ion beam (FIB) manufactured [0 0 1] and [2 3 5] Mo micro/nanopillars, which were compressed, re-FIB machined, and compressed again. Unlike in bulk materials, pre-straining has a negligible effect on stress–strain behavior of the pillars, suggesting that dislocation storage does not occur in small-scale bcc specimens. The prevailing mechanism behind the size effect is attributed to dislocation nucleation mechanisms.

Deformation-induced grain growth and twinning in nanocrystalline palladium thin films

Summary The microstructure and mechanical properties of nanocrystalline Pd films prepared by magnetron sputtering have been investigated as a function of strain. The films were deposited onto polyimide substrates and tested in tensile mode. In order to follow the deformation processes in the material, several samples were strained to defined straining states, up to a maximum engineering strain of 10%, and prepared for post-mortem analysis. The nanocrystalline structure was investigated by quantitative automated crystal orientation mapping (ACOM) in a transmission electron microscope (TEM), identifying grain growth and twinning/detwinning resulting from dislocation activity as two of the mechanisms contributing to the macroscopic deformation. Depending on the initial twin density, the samples behaved differently. For low initial twin densities, an increasing twin density was found during straining. On the other hand, starting from a higher twin density, the twins were depleted with increasing strain. The findings from ACOM-TEM were confirmed by results from molecular dynamics (MD) simulations and from conventional and in-situ synchrotron X-ray diffraction (CXRD, SXRD) experiments.

Temperature dependence of mechanical properties in ultrathin Au films with and without passivation

Temperature and film thickness are expected to have an influence on the mechanical properties of thin films. However, mechanical testing of ultrathin metallic films at elevated temperatures is difficult, and few experiments have been conducted to date. Here, we present a systematic study of the mechanical properties of 80–500-nm-thick polycrystalline Au films with and without SiN x passivation layers in the temperature range from 123 to 473 K. The films were tested by a novel synchrotron-based tensile testing technique. Pure Au films showed strong temperature dependence above 373 K, which may be explained by diffusional creep. In contrast, passivated samples appeared to deform by thermally activated dislocation glide. The observed activation energies for both mechanisms are considerably lower than those for the bulk material, indicating that concomitant stress relaxation mechanisms are more pronounced in the thin film geometry.

Size Effect on Crack Formation in Cu/Ta and Ta/Cu/Ta Thin Film Systems

Layered structures of Cu and Ta thin films on silicon are well established for many technological applications in microelectronics. Electronic circuits used for flexible displays or wearable electronics are becoming increasingly popular. For such applications, the Cu/Ta system must be transferred to flexible substrates, incorporating a design rule for several percent of total strain. We have investigated the deformation behaviour of different Cu/Ta and Ta/Cu/Ta thin film systems on a flexible polyimide substrate subjected to total strains of more than 5%. A novel synchrotron X-ray diffraction technique allowed us to characterize the evolution of mechanical stress in very thin metallic films during isothermal tensile tests. We found that samples with a Cu film thickness below 300 nm showed a sudden stress decrease at a total strain of about 2.5%. This stress drop was attributed to fracture of the entire film system, initiated by cracks in the Ta layers.

Improving mechanical fatigue resistance by optimizing the nanoporous structure of inkjet-printed Ag electrodes for flexible devices

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.

The effect of solute segregation on strain localization in nanocrystalline thin films: Dislocation glide vs. grain-boundary mediated plasticity

Deformation mechanisms of nanocrystalline Au and AuCu thin films on compliant substrates were investigated by synchrotron-based in situ tensile testing and Automated Crystal Orientation Mapping using transmission electron microscopy. The results demonstrate that intragranular dislocation plasticity, inferred from evolution of deformation texture, is responsible for the formation of periodic and ordered shear bands in AuCu films. In contrast, pure Au films deform homogeneously without shear band formation and without evolution of deformation texture. Cu solutes are deemed to pin grain boundaries thereby enforce dislocation glide, while in pure Au, plasticity is carried by grain boundary shear and grain boundary migration.

Anatomizing deformation mechanisms in nanocrystalline Pd90Au10

Abstract We utilized synchrotron-based in-situ diffraction and dominant shear deformation to identify, dissect, and quantify the relevant deformation mechanisms in nanocrystalline Pd 90 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  ≈ 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  ≈ 1.4 GPa and contributes a share of  ≈ 10% to overall strain. Appreciable dislocation activity begins at a stress value of  ≈ 0.9 GPa to then increase and eventually propagate a maximal share of  ≈ 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.

Temperature-dependent strain localization and texture evolution of highly nanotwinned Cu

Strong differences in the plastic strain and texture development in high purity nanotwinned copper foils deformed to failure in tension at ambient and liquid nitrogen (LN) temperatures have been observed. High energy microdiffraction patterns for the room temperature (RT) sample showed two distinct deformation regions relative to its fracture surface: d   500 μm; while for the sample deformed at 77 K, three distinct regions were observed: d   1550 μm. The localized plastic deformation in the RT tensile test and the increased ductile deformation at LN temperature are discussed in terms of the dualistic nanotwins plus micro-scale columnar grain structure.