Atomic scale volume and grain boundary diffusion elucidated by in situ STEM.

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.

From metal nanowires to ultrathin crystalline ALD nanotubes: process development and mechanism revealed by TEM heating experiments.

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.

Effects of biomechanical and biochemical stimuli on angio- and vasculogenesis in a complex microvasculature-on-chip.

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.

Room Temperature Viscous Flow of Amorphous Silica Induced by Electron Beam Irradiation.

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 T . Those treatments, however, are global and affect the whole component.

Machine Learning-Based Characterization of the Nanostructure in a Combinatorial Co-Cr-Fe-Ni Compositionally Complex Alloy Film.

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.

Microscale 3D Printing and Tuning of Cellulose Nanocrystals Reinforced Polymer Nanocomposites.

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.

Thermally Stable Nanotwins: New Heights for Cu Mechanics.

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.

Combinatorial Study of Phase Composition, Microstructure and Mechanical Behavior of Co-Cr-Fe-Ni Nanocrystalline Film Processed by Multiple-Beam-Sputtering Physical Vapor Deposition.

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.

Mechanisms of Fluorine-Induced Separation of Mass Interference during TOF-SIMS Analysis.

Time-of-flight secondary ion mass spectrometry (TOF-SIMS) is one of very few analytical techniques allowing sample chemical structure to be characterized in three-dimensional (3D) with nanometer resolution. Due to the excellent sensitivity in the order of ppm-ppb and capability of detecting all ionized elements and molecules, TOF-SIMS finds many applications for analyzing nanoparticle-containing systems and thin films used in microdevices for new energy applications, microelectronics, and biomedicine. However, one of the main drawbacks of this technique is potential mass interference between ions having the same or similar masses, which can lead to data misinterpretation.

Microstructure, Hardness, and Elastic Modulus of a Multibeam-Sputtered Nanocrystalline Co-Cr-Fe-Ni Compositional Complex Alloy Film.

A nanocrystalline Co-Cr-Ni-Fe compositional complex alloy (CCA) film with a thickness of about 1 micron was produced by a multiple-beam-sputtering physical vapor deposition (PVD) technique. The main advantage of this novel method is that it does not require alloy targets, but rather uses commercially pure metal sources. Another benefit of the application of this technique is that it produces compositional gradient samples on a disk surface with a wide range of elemental concentrations, enabling combinatorial analysis of CCA films.

High Sensitivity of Fluorine Gas-Assisted FIB-TOF-SIMS for Chemical Characterization of Buried Sublayers in Thin Films.

In this work, we present the potential of high vacuum-compatible time-of-flight secondary ion mass spectrometry (TOF-SIMS) detectors, which can be integrated within focused ion beam (FIB) instruments for precise and fast chemical characterization of thin films buried deep under the sample surface. This is demonstrated on complex multilayer systems composed of alternating ceramic and metallic layers with thicknesses varying from several nanometers to hundreds of nanometers. The typical problems of the TOF-SIMS technique, that is, low secondary ion signals and mass interference between ions having similar masses, were solved using a novel approach of co-injecting fluorine gas during the sample surface sputtering.

Elemental Characterization of Al Nanoparticles Buried under a Cu Thin Film: TOF-SIMS vs STEM/EDX.

In this work, we present a comprehensive comparison of time-of-flight secondary ion mass spectrometry (TOF-SIMS) and scanning transmission electron microscopy combined with energy-dispersive X-ray spectroscopy (STEM/EDX), which are currently the most powerful elemental characterization techniques in the nano- and microscale. The potential and limitations of these methods are verified using a novel dedicated model sample consisting of Al nanoparticles buried under a 50 nm thick Cu thin film. The sample design based on the low concentration of nanoparticles allowed us to demonstrate the capability of TOF-SIMS to spatially resolve individual tens of nanometer large nanoparticles under ultrahigh vacuum (UHV) as well as high vacuum (HV) conditions.

A set of empirical equations describing the observed colours of metal-anodic aluminium oxide-Al nanostructures.

Structural colours have received a lot of attention regarding the reproduction of the vivid colours found in nature. In this study, metal-anodic aluminium oxide (AAO)-Al nanostructures were deposited using a two-step anodization and sputtering process to produce self-ordered anodic aluminium oxide films and a metal layer (8 nm Cr and 25, 17.5 and 10 nm of Au), respectively.

Achieving micron-scale plasticity and theoretical strength in Silicon.

As the backbone material of the information age, silicon is extensively used as a functional semiconductor and structural material in microelectronics and microsystems. At ambient temperature, the brittleness of Si limits its mechanical application in devices. Here, we demonstrate that Si processed by modern lithography procedures exhibits an ultrahigh elastic strain limit, near ideal strength (shear strength ~4 GPa) and plastic deformation at the micron-scale, one order of magnitude larger than samples made using focused ion beams, due to superior surface quality.

Fluorine Gas Coinjection as a Solution for Enhancing Spatial Resolution of Time-of-Flight Secondary Ion Mass Spectrometry and Separating Mass Interference.

Time-of-flight secondary ion mass spectrometry (TOF-SIMS) detectors have been intensively developed in recent decades due to their unprecedented capability of representing a sample elemental composition in a three-dimensional space from nano- to submilliscale with high spatial resolution and mass resolution. A compact high-vacuum-compatible version of these detectors can be integrated into a focused ion beam (FIB) system which, assembled with scanning electron microscopy (SEM), is the most popular tool used in nanotechnology and material science. This gives a new opportunity for combining TOF-SIMS analysis with other instruments within the same analytical chamber.

Application of a Gas-Injection System during the FIB-TOF-SIMS Analysis-Influence of Water Vapor and Fluorine Gas on Secondary Ion Signals and Sputtering Rates.

Combining a Gas-Injection System (GIS) with the Focused Ion Beam (FIB) has a broad scope of applications in sample preparation such as protective layer deposition, increasing material sputtering rates, and reducing FIB-related artifacts. On the other hand, injecting certain specific gases during a Time-of-Flight Secondary Ion Mass Spectrometry (TOF-SIMS) analysis can significantly increase element ionization probability and, therefore, improve the quality of 3D representation of a sample elemental structure. In this work, for the first time, the potential of GIS for enhancing secondary ion signals acquired using a TOF detector incorporated into a commercial Ga FIB-SEM (Focused Ion Beam combined with Scanning Electron Microscope) instrument is presented.

3D Imaging of Nanoparticles in an Inorganic Matrix Using TOF-SIMS Validated with STEM and EDX.

Imaging nano-objects in complex systems such as nanocomposites using time-of-flight secondary ion mass spectrometry (TOF-SIMS) is a challenging task. Due to a very small amount of the material and a matrix effect, the number of generated secondary ions can be insufficient to represent a 3D elemental distribution despite being detected in a mass spectrum. Therefore, a model sample consisting of a ZrCuAg matrix with embedded Al nanoparticles is designed.

Dynamic Plasticity and Failure of Microscale Glass: Rate-Dependent Ductile-Brittle-Ductile Transition.

Glass has been recently envisioned as a stronger and more robust alternative to silicon in microelectromechanical system applications, including high-frequency resonators and switches. Identifying the dynamic mechanical properties of microscale glass is thus vital for understanding their ability to withstand shocks and vibrations in such demanding applications. However, despite nearly half a century of research, the micromechanical properties of glass and amorphous materials in general are primarily limited to quasi-static strain rates below ∼0.