A central focus in high strain rate research is understanding the dynamic behavior of materials at strain rates where a strength upturn is observed. While strength upturns at strain rates of 10^3 to 10^4 s^-1 have been widely reported in the literature, their occurrence in certain materials remains controversial, and the underlying physics driving this phenomenon is not yet fully understood. Current mechanical testing methods are limited, as no single technique spans the full strain rate range of 10^1 to 10^5 s^-1 where this phenomenon is expected, and a unified technique would enable consistent post-deformation characterization with minimal error. To address this, we developed a customized piezoelectric in situ nanomechanical test setup, enabling constant indentation strain rates up to 10^5 s^-1 for the first time. Using this system, we examined rate-dependent hardness in single-crystalline molybdenum, nanocrystalline nickel, and amorphous fused silica over strain rates from 10^1 to 10^5 s^-1, remarkably revealing a hardness upturn in all three materials. Further, post-deformation analysis of single-crystalline molybdenum revealed that the hardness upturn was primarily driven by increased dislocation density, with phonon drag – traditionally considered a dominant contributor – playing a minimal role.

To study the size and strain rate dependency of copper polycrystalline microstructures, a multi-layered copper/Al2O3 thin film was deposited on a Si substrate using a hybrid deposition system (combining physical vapour and atomic layer deposition). High temperature treatment was applied on the “As Deposited” material with ultrafine-grained structure to increase the average grain size, resulting in a “Heat Treated” state with microcrystalline structure. Focused ion beam milling was employed to create square shaped micropillars with two different sizes, that were subjected to compressive loading at various (0.001/s – 1000/s) strain rates. Differences in the strain rate sensitivity behavior manifesting at low and high strain rates are discussed in the context of the pillar diameters and the grain size of the deformed samples. The Al2O3 interlayer studied by transmission electron microscopy showed excellent thermal stability and grain boundary pinning by precipitation, also resulting in the homogeneous deformation of the pillars and preventing shear localization. Geometrically necessary dislocation densities estimated by high (angular) resolution electron backscatter diffraction presented inhomogeneous dislocation distribution within the deformed pillar volumes, that is attributed to the proximity of the sample edges. Finally, the Al2O3 interlayers successfully suppressed any possible recrystallization processes, contributing to the excellent film stability, that makes the proposed coating ideal to be operating under extreme conditions.

The Co–Cr–Cu–Fe–Ni–Zn compositional library was studied on a combinatorial high-entropy alloy thin film processed on a silicon substrate by magnetron sputtering technique. The thickness of the coating was between 2 and 3 μm while the lateral dimension was 10 cm. The chemical composition in the layer depended on the location and for each constituent element the concentration varied between 5 and 42 at.%. The phase composition and the microstructure were mapped using synchrotron X-ray diffraction, and the crystallite size as well as the density of lattice defects (dislocations and twin faults) were determined by diffraction line profile profile analysis. In addition, selected locations were studied by transmission electron microscopy. The influence of the chemical composition on the microstructure and the mechanical behavior was revealed. The mechanical performance was characterized by nanoindentation mapping which determined the hardness and the elastic modulus versus the element concentrations. It was found that the coating contains single phase face-centered cubic (FCC) and body-centered cubic (BCC) regions as well as an intermediate two-phase area. In the whole combinatorial sample, the microstructure consisted of nanocrystalline columns growing perpendicular to the coating surface and having pores between them. Due to the porosity, the hardness and the elastic modulus were relatively low despite the nanostructure and the very high defect density. The highest hardness (3.4 GPa) and elastic modulus (119 GPa) were measured in the BCC region with the chemical composition of 10%Co–38%Cr–13%Cu–27%Fe–5%Ni–7%Zn (at.%).

We report detailed diffraction peak analysis and parameters indicative of the transition between fully amorphous microstructures and nanocrystal formation in sputter deposited thin film metallic glasses. Specifically, we fabricated ternary CuZrAg alloy films (2µm thickness) with a large compositional gradient on flexible, X-ray transparent polymer substrates in high vacuum conditions. The combinatorial libraries were subjected to point-by-point structural (XRD synchrotron radiation) and chemical (X-ray fluorescence spectroscopy) analysis, characterizing roughly 172 alloys. A strong correlation was found between peak symmetry and width, and early stages of crystalline phase formation. These nanocrystals are difficult to detect from the evolution of the peak position. In view of current literature, our data questions the recently claimed universality of the peak width as indicator of high glass forming ability. The addition of Ag significantly improves the poor glass formation of binary CuZr (36 alloys) under identical deposition conditions, as fully amorphous alloys are found for the majority of the investigated composition space. A thorough understanding of the microstructure of CuZrAg alloys on flexible substrates is highly relevant in view of favourable antibacterial properties and potential application as coatings for biomedical surfaces.

The endothelium of blood vessels is a vital organ that reacts differently to subtle changes in stiffness and mechanical forces exerted on its environment (extracellular matrix (ECM)). Upon alteration of these biomechanical cues, endothelial cells initiate signaling pathways that govern vascular remodeling. The emerging organs-on-chip technologies allow the mimicking of complex microvasculature networks, identifying the combined or singular effects of these biomechanical or biochemical stimuli. Here, we present a microvasculature-on-chip model to investigate the singular effect of ECM stiffness and mechanical cyclic stretch on vascular development. Following two different approaches for vascular growth, the effect of ECM stiffness on sprouting angiogenesis and the effect of cyclic stretch on endothelial vasculogenesis are studied. Our results indicate that ECM hydrogel stiffness controls the size of the patterned vasculature and the density of sprouting angiogenesis. RNA sequencing shows that the cellular response to stretching is characterized by the upregulation of certain genes such as ANGPTL4+5, PDE1A, and PLEC.

The combination of conventional physical vapor deposition and a gas aggregation nanoparticle source enabled the study of model systems of unique material combinations and dimensions. Zr50Cu45Ag5 thin film metallic glasses with varying contents of single-crystalline 5 nm tungsten nanoparticles were synthesized using this technique. This approach provides precise control over nanoparticle shape, size, distribution, and concentration. The films were later annealed at 150 degrees C, 250 degrees C, 350 degrees C, and 450 degrees C. At room temperature inclusion of 0.01 vol% tungsten nanoparticles caused a 15% increase in the nano-indentation hardness of a thin film metallic glass, while having no significant effect on pop-in length or frequency, as seen in the loading curves. Even more remarkably, at 450 degrees C a control film containing no nanoparticles experienced significant segregation and subsequent crystallization, whereas this effect was repressed in the tungsten nanoparticle composite thin film metallic glass. Unobstructed by nanoparticles, at high temperatures zirconium diffused to the surface of the film, forming a crystalline layer of up to 80 nm. In contrast, this layer is kept to below 30 nm when the nanoparticles are present. The stabilization of the microstructure is also clear from indentation results, while the hardness of the reference sample changes significantly due to the undesired crystallization, the hardness of the composite remains constant.

Measuring strain accurately at small length scales poses a significant challenge, making it difficult to obtain precise elastic properties of small materials. This becomes particularly pronounced for test geometries beyond micro-pillars and for materials with high elastic limits and high Peierls stresses. This study investigates the elastic strain limits and strain distribution in micro double shear tests conducted on single-crystalline silicon with different crystallographic orientations. In situ scanning electron microscopy images were used to obtain full-field strain maps using digital image correlation. This local strain analysis approach revealed that the shear zones of the test geometry are not solely under pure shear conditions, but also experience superimposed bending. The local strain analysis approach increases the precision of measured elastic properties to ±15% of the literature value compared to deviations of 75-80% using the traditional global strain analysis approach. This study highlights the limitations of the global strain analysis approach in complex specimen geometries and demonstrates the effectiveness of digital image correlation in accurately determining elastic strain at the small length scale. Furthermore, both the low defect density in the samples as well as the small length scales allow for the exploration of orientation dependent strength levels close to the theoretical limit.

The increasing use of oxide glasses in high-tech applications illustrates the demand of novel engineering techniques on nano- and microscale. Due to the high viscosity of oxide glasses at room temperature, shaping operations are usually performed at temperatures close or beyond the point of glass transition Tg . Those treatments, however, are global and affect the whole component. It is known from the literature that electron irradiation facilitates the viscous flow of amorphous silica near room temperature for nanoscale components. At the micrometer scale, however, a comprehensive study on this topic is still pending. In the present study, electron irradiation inducing viscous flow at room temperature is observed using a micropillar compression approach and amorphous silica as a model system. A comparison to high temperature yielding up to a temperature of 1100 °C demonstrates that even moderate electron irradiation resembles the mechanical response of 600 °C and beyond. As an extreme case, a yield strength as low as 300 MPa is observed with a viscosity indicating that Tg has been passed. Those results show that electron irradiation-facilitated viscous flow is not limited to the nanoscale which offers great potential for local microengineering.

Diffusion is one of the most important phenomena studied in science ranging from physics to biology and, in abstract form, even in social sciences. In the field of materials science, diffusion in crystalline solids is of particular interest as it plays a pivotal role in materials synthesis, processing and applications. While this subject has been studied extensively for a long time there are still some fundamental knowledge gaps to be filled. In particular, atomic scale observations of thermally stimulated volume diffusion and its mechanisms are still lacking. In addition, the mechanisms and kinetics of diffusion along defects such as grain boundaries are not yet fully understood. In this work we show volume diffusion processes of tungsten atoms in a metal matrix on the atomic scale. Using in situ high resolution scanning transmission electron microscopy we are able to follow the random movement of single atoms within a lattice at elevated temperatures. The direct observation allows us to confirm random walk processes, quantify diffusion kinetics and distinctly separate diffusion in the volume from diffusion along defects. This work solidifies and refines our knowledge of the broadly essential mechanism of volume diffusion.

The creation of hollow nanomaterials based on metal oxides has become an important research topic, as they show potential in a broad range of technical applications. However, the controlled synthesis of long and at the same time thin nanotubes is still challenging. Here we present a universal approach to create ultrathin aluminum oxide nanotubes with a length/diameter ratio of >1200 and minimum wall thickness of ≤4 nm. We use a facile process based on defined heat treatment of specific core-shell nanowires. The metal nanowires act as a template, which is thermally removed during heat treatment until an empty tube is created. The core-shell nanowires are produced by Physical Vapour Deposition (PVD) with a subsequent coating via Atomic Layer Deposition (ALD). The custom-built PVD-ALD system enables a direct sample transfer without breaking the vacuum, which allows determining the effect of a native oxide layer on the metal-ALD bonding. In combination with correlative ex situ observations, in situ Transmission Electron Microscopy (TEM) heating experiments unravel the dynamical processes going on at small scales. Based on the microscopic analysis, the energetics of the core material is analyzed, giving insights about heat induced effects as well as the phase transition from the amorphous to the crystalline state.

A unique deposition approach combining atomic layer deposition (ALD) and magnetron sputtering was used to fabricate a series of thin film multilayer structures of Al (50 nm) and Al2O3 (ALD, 2.4-9.4 nm) on flexible polymer substrates without breaking vacuum. The multilayers together with 50 nm and 150 nm Al reference films were analyzed by cross-sectional TEM analysis and experimentally strained in biaxial tension to investigate their deformation behavior. Al film stresses and peak widths, measured in situ with Synchrotron X-ray diffraction, are in good agreement with post-mortem surface SEM and through-thickness FIB analysis of the multilayers. It was revealed that brittle cracking of the multilayer can be avoided, and that the lateral and through-thickness crack resistance improve as a function of decreasing oxide layer thickness. An attempt to model the full biaxial yield surface of the multilayers, which remains experimentally challenging, appears to be valid up to 2.4 nm oxide thickness. Model predictions are further compared to compression data, obtained from the unloading segments of the tensile tests. Describing the mechanical behaviour under multiaxial stress conditions is of utmost importance for a diverse understanding of these multilayers across a variety of potential carrier systems and loading cases.& COPY; 2023 The Author(s). Published by Elsevier Ltd. This is an open access article under the CC BY license (http://creativecommons.org/licenses/by/4.0/).

The ability to predict the micro-scale strength and plasticity of fused-silica micro-components is crucial as their miniaturization and applications in harsh environments advance. This study focusses on the micro-mechanical behavior of fused silica micropillars at high temperatures and variable strain rates. 160 micropillars with a diameter of 1.6 µm have been tested at temperatures between −120 °C and 600 °C and strain rates between 10-3 s−1 and 1 s−1, which are to date unexplored conditions. Between −120 °C and 300 °C, the yield strengths (6–8 GPa) and strain rate sensitivities (≤0.03) vary only marginally. However, at 600 °C, a significant decrease in yield strength by more than 50 % (2.5–4.5 GPa) and an increase in strain rate sensitivity by a factor of 3 (0.09) is observed. Post-compression synchrotron-based ptychographic X-ray computed tomography (PXCT) on plastically deformed micropillars revealed a transition in deformation mechanisms: Shear-localization and shear-promoted densification at 25 °C; homogeneous shear-flow and densification limited by radial cracking at 300 °C; and unconstrained shear-flow and limited densification due to weak confinement strength at 600 °C. FEM results support these observations while separating geometric from material-intrinsic effects. These results suggest that the classification of fused silica as a glass that deforms predominantly through densification should be challenged – at least under unconstrained compression, which is the predominant mode of loading in applications.

Journal Article In situ TEM Study to Unravel Dynamic Processes and Phase Transition During the Synthesis of Ultrathin Crystalline ALD Nanotubes Get access LM Vogl, LM Vogl Laboratory for Mechanics of Materials and Nanostructures, EMPA– Swiss Federal Laboratories for Materials Science and Technology, Thun, Switzerland Corresponding author: Lilian.Vogl@empa.ch Search for other works by this author on: Oxford Academic Google Scholar P Schweizer, P Schweizer Laboratory for Mechanics of Materials and Nanostructures, EMPA– Swiss Federal Laboratories for Materials Science and Technology, Thun, Switzerland Search for other works by this author on: Oxford Academic Google Scholar L Pethö, L Pethö Laboratory for Mechanics of Materials and Nanostructures, EMPA– Swiss Federal Laboratories for Materials Science and Technology, Thun, Switzerland Search for other works by this author on: Oxford Academic Google Scholar A Sharma, A Sharma Laboratory for Mechanics of Materials and Nanostructures, EMPA– Swiss Federal Laboratories for Materials Science and Technology, Thun, Switzerland Search for other works by this author on: Oxford Academic Google Scholar E Spiecker, E Spiecker Institute of Micro-and Nanostructure Research, Friedrich-Alexander University Erlangen-Nürnberg Search for other works by this author on: Oxford Academic Google Scholar I Utke, I Utke Laboratory for Mechanics of Materials and Nanostructures, EMPA– Swiss Federal Laboratories for Materials Science and Technology, Thun, Switzerland Search for other works by this author on: Oxford Academic Google Scholar J Michler J Michler Laboratory for Mechanics of Materials and Nanostructures, EMPA– Swiss Federal Laboratories for Materials Science and Technology, Thun, Switzerland Search for other works by this author on: Oxford Academic Google Scholar Microscopy and Microanalysis, Volume 28, Issue S1, 1 August 2022, Pages 2316–2318, https://doi.org/10.1017/S143192762200890X Published: 01 August 2022

We report for the first-time combinatorial synthesis of thin film metallic glass libraries via magnetron co-sputtering at the limit of crystallinity. Special care was taken to prepare extremely pure CuZr films (1–2 µm thickness) with large compositional gradients (Cu18.2Zr81.8 to Cu74.8Zr25.2) on X-ray transparent polymer substrates in high-vacuum conditions. Combined mapping of atomic structure (synchrotron radiation) and chemical composition (X-ray fluorescence spectroscopy) revealed that over the entire composition range, covering multiple renowned glass formers, two phases are present in the film. Our high-resolution Synchrotron approach identified the two phases as: untextured amorphous Cu51Zr14 (cluster size 1.3 nm) and textured, nanocrystalline α-Zr (grain size 1–5 nm). Real space HR-STEM analyses of a representative composition substantiate our XRD results. Determined cluster and grain sizes are below the resolution limit of conventional laboratory-scale X-ray diffractometers. The presented phase mixture is not permitted in the Cu-Zr phase diagram and contrary to existing literature. The phase ratio follows a linear trend with amorphous films on the Cu-rich side and increasing amounts of α-Zr with increasing Zr content. While cluster size and composition of the amorphous phase remain constant thorough the compositional gradient, crystallite size and texture of the nanocrystalline α-Zr change as a function of Zr content.

Nanocrystalline and nanotwinned materials achieve exceptional strengths through small grain sizes. Due to large areas of crystal interfaces, they are highly susceptible to grain growth and creep deformation, even at ambient temperatures. Here, ultrahigh strength nanotwinned copper microstructures have been stabilized against high temperature exposure while largely retaining electrical conductivity. By incorporating less than 1 vol% insoluble tungsten nanoparticles by a novel hybrid deposition method, both the ease of formation and the high temperature stability of nanotwins are dramatically enhanced up to at least 400 °C. By avoiding grain coarsening, improved high temperature creep properties arise as the coherent twin boundaries are poor diffusion paths, while some size-based nanotwin strengthening is retained. Such microstructures hold promise for more robust microchip interconnects and stronger electric motor components.

A novel artificial intelligence-assisted evaluation of the X-ray diffraction (XRD) peak profiles was elaborated for the characterization of the nanocrystallite microstructure in a combinatorial Co-Cr-Fe-Ni compositionally complex alloy (CCA) film. The layer was produced by a multiple beam sputtering physical vapor deposition (PVD) technique on a Si single crystal substrate with the diameter of about 10 cm. This new processing technique is able to produce combinatorial CCA films where the elemental concentrations vary in a wide range on the disk surface. The most important benefit of the combinatorial sample is that it can be used for the study of the correlation between the chemical composition and the microstructure on a single specimen. The microstructure can be characterized quickly in many points on the disk surface using synchrotron XRD. However, the evaluation of the diffraction patterns for the crystallite size and the density of lattice defects (e.g., dislocations and twin faults) using X-ray line profile analysis (XLPA) is not possible in a reasonable amount of time due to the large number (hundreds) of XRD patterns. In the present study, a machine learning-based X-ray line profile analysis (ML-XLPA) was developed and tested on the combinatorial Co-Cr-Fe-Ni film. The new method is able to produce maps of the characteristic parameters of the nanostructure (crystallite size, defect densities) on the disk surface very quickly. Since the novel technique was developed and tested only for face-centered cubic (FCC) structures, additional work is required for the extension of its applicability to other materials. Nevertheless, to the knowledge of the authors, this is the first ML-XLPA evaluation method in the literature, which can pave the way for further development of this methodology.

A combinatorial Co-Cr-Fe-Ni compositional complex alloy (CCA) thin film disk with a thickness of 1 µm and a diameter of 10 cm was processed by multiple-beam-sputtering physical vapor deposition (PVD) using four pure metal sources. The chemical composition of the four constituent elements varied between 4 and 64 at.% in the film, depending on the distance from the four PVD sources. The crystal structure, the crystallite size, the density of lattice defects (e.g., dislocations and twin faults) and the crystallographic texture were studied as a function of the chemical composition. It was found that in a wide range of elemental concentrations a face-centered cubic (fcc) structure with {111} crystallographic texture formed during PVD. Considering the equilibrium phase diagrams, it can be concluded that mostly the phase composition of the PVD layer is far from the equilibrium. Body-centered cubic (bcc) and hexagonal-close packed (hcp) structures formed only in the parts of the film close to Co-Fe and Co-Cr sources, respectively. A nanocrystalline microstructure with the grain size of 10–20 nm was developed in the whole layer, irrespective of the chemical composition. Transmission electron microscopy indicated a columnar growth of the film during PVD. The density of as-grown dislocations and twin faults was very high, as obtained by synchrotron X-ray diffraction peak profile analysis. The nanohardness and the elastic modulus were determined by indentation for the different chemical compositions on the combinatorial PVD film. This study is the continuation of a former research published recently in Nagy et al., Materials 14 (2021) 3357. In the previous work, only the fcc part of the sample was investigated. In the present paper, the study was extended to the bcc, hcp and multiphase regions.

Physical vapour deposition combined with atomic layer deposition was exploited to design a model sys-tem of UFG aluminium with a narrow grain size and shape distribution, including two types of inter-faces (Al-Al & Al-Al2O3), with Al-Al grain boundary orientations exclusively parallel to the loading axis. This enabled isolated study of the strengthening mechanisms that ultrathin oxide layers would provide in a metal multilayer structure. The Al/Al2O3 crystalline/amorphous multilayers with 240 nm metal lay-ers and oxide thicknesses in the range < 1 nm-12 nm (i.e. to below the natural oxidation thickness), were microcompressed, yielding a pseudo-macroscopic yield strength of 532 MPa - over 100 MPa higher than the literature-conforming oxide-free reference. The homogenous co-deformation of the structure, with barrelling of the individual metal layers at the micropillar edges, results from the high bonding strength of the metal with its native oxide, meaning no failure or sliding at the interface, unlike previ-ous Al/ceramic multilayer studies. Only the thicker ( >= 5 nm) oxide layers fractured in-plane: at locations coincident with vertical Al-Al grain boundaries. An analysis of contributions to the strength of these crys-talline/amorphous metal/ceramic hybrid multilayers is carried out, identifying the Al-Al2O3 interface to be the crucial factor, rather than the in-plane tensile stiffness and considerable plasticity of ALD Al2O3 itself. The strengthening effect of the oxide layer was effective down to a layer thickness of just 0.5 nm. (c) 2022 The Author(s). Published by Elsevier Ltd on behalf of Acta Materialia Inc. This is an open access article under the CC BY license ( http://creativecommons.org/licenses/by/4.0/ )

The increasing demand for functional materials and an efficient use of sustainable resources makes the search for new material systems an ever growing endeavor. With this respect, architected (meta-)materials attract considerable interest. Their fabrication at the micro- and nanoscale, however, remains a challenge, especially for composites with highly different phases and unmodified reinforcement fillers. This study demonstrates that it is possible to create a non-cytotoxic nanocomposite ink reinforced by a sustainable phase, cellulose nanocrystals (CNCs), to print and tune complex 3D architectures using two-photon polymerization, thus, advancing the state of knowledge toward the microscale. Micro-compression, high-res scanning electron microscopy, (polarised) Raman spectroscopy, and composite modeling are used to study the structure-property relationships. A 100% stiffness increase is observed already at 4.5 wt% CNC while reaching a high photo-polymerization degree of ≈80% for both neat polymers and CNC-composites. Polarized Raman and the Halpin-Tsai composite-model suggest a random CNC orientation within the polymer matrix. The microscale approach can be used to tune arbitrary small scale CNC-reinforced polymer-composites with comparable feature sizes. The new insights pave the way for future applications where the 3D printing of small structures is essential to improve performances of tissue-scaffolds, extend bio-electronics applications or tailor microscale energy-absorption devices.