Is the Ne operation of the helium ion microscope suitable for electron backscatter diffraction sample preparation?

Electron backscatter diffraction (EBSD) is a powerful characterization technique which allows the study of microstructure, grain size, and orientation as well as strain of a crystallographic sample. In addition, the technique can be used for phase analysis. A mirror-flat sample surface is required for this analysis technique and different polishing approaches have been used over the years. A commonly used approach is the focused ion beam (FIB) polishing. Unfortunately, artefacts that can be easily induced by Ga FIB polishing approaches are seldom published. This work aims to provide a better understanding of the underlying causes for artefact formation and to assess if the helium ion microscope is better suited to achieve the required mirror-flat sample surface when operating the ion source with Ne instead of He. Copper was chosen as a test material and polished using Ga and Ne ions with different ion energies as well as incident angles. The results show that crystal structure alterations and, in some instances, phase transformation of Cu to Cu3Ga occurred when polishing with Ga ions. Polishing with high-energy Ne ions at a glancing angle maintains the crystal structure and significantly improves indexing in EBSD measurements. By milling down to a depth equaling the depth of the interaction volume, a steady-state condition of ion impurity concentration and number of induced defects is reached. The EBSD measurements and Monte Carlo simulations indicate that when this steady-state condition is reached more quickly, which can be achieved using high-energy Ne ions at a glancing incidence, then the overall damage to the specimen is reduced.

Scanning transmission helium ion microscopy on carbon nanomembranes.

A dark-field scanning transmission ion microscopy detector was designed for the helium ion microscope. The detection principle is based on a secondary electron conversion holder with an exchangeable aperture strip allowing its acceptance angle to be tuned from 3 to 98 mrad. The contrast mechanism and performance were investigated using freestanding nanometer-thin carbon membranes. The results demonstrate that the detector can be optimized either for most efficient signal collection or for maximum image contrast. The designed setup allows for the imaging of thin low-density materials that otherwise provide little signal or contrast and for a clear end-point detection in the fabrication of nanopores. In addition, the detector is able to determine the thickness of membranes with sub-nanometer precision by quantitatively evaluating the image signal and comparing the results with Monte Carlo simulations. The thickness determined by the dark-field transmission detector is compared to X-ray photoelectron spectroscopy and energy-filtered transmission electron microscopy measurements.

Biowaste-Derived, Self-Organized Arrays of High-Performance 2D Carbon Emitters for Organic Light-Emitting Diodes.

Low-cost flexible organic light-emitting diodes (OLEDs) with nanoemitter material from waste open up new opportunities for sustainable technology. The common emitter materials generated from waste are carbon dots (CDs). However, these have poor luminescent properties. Further solid-state emission quenching makes application in display devices challenging. Here, flexible and rigid OLED devices are demonstrated using self-assembled 2D arrays of CDs derived from waste material, viz., human hair. High-performance CDs with a quantum yield (QY) of 87%, self-assembled into 2D arrays, are achieved by improving the crystallinity and decreasing the CDs' size distribution. The CD island array exhibits ultrahigh hole mobility (≈10-1 cm2 V-1 s-1 ) and significant reduction in solid-state emission quenching compared to pristine CDs; hence, it is used here as an emitting layer in both indium tin oxide (ITO)-coated glass and ITO-coated flexible poly(ethylene terephthalate) (PET) substrate OLED devices, without any hole-injection layer. The flexible OLED device exhibits a stable, voltage-independent blue/cyan emission with a record maximum luminescence of 350 cd m-2 , whereas the OLED device based on the rigid glass substrate shows a maximum luminescence of 700 cd m-2 . This work sets up a platform to develop next-generation OLED displays using CD emitters derived from the biowaste material.

Aberrant activation of Wnt signaling pathway altered osteocyte mineralization.

Mineralization of bone is a dynamic process, involving a complex interplay between cells, secreted macromolecules, signaling pathways, and enzymatic reactions; the dysregulation of bone mineralization may lead to serious skeletal disorders, including hypophosphatemic rickets, osteoporosis, and rheumatoid arthritis. Very few studies have reported the role of osteocytes - the most abundant bone cells in the skeletal system and the major orchestrators of bone remodeling in bone mineralization, which is owed to their nature of being deeply embedded in the mineralized bone matrix. The Wnt/ß-catenin signaling pathway is actively involved in various life processes including osteogenesis; however, the role of Wnt/ß-catenin signaling in the terminal mineralization of bone, especially in the regulation of osteocytes, is largely unknown. This research demonstrates that during the terminal mineralization process, the Wnt/ß-catenin pathway is downregulated, and when Wnt/ß-catenin signaling is activated in osteocytes, dendrite development is suppressed and the expression of dentin matrix protein 1 (DMP1) is inhibited. Aberrant activation of Wnt/ß-catenin signaling in osteocytes leads to the spontaneous deposition of extra-large mineralized nodules on the surface of collagen fibrils. The altered mineral crystal structure and decreased bonding force between minerals and the organic matrix indicate the inferior integration of minerals and collagen. In conclusion, Wnt/ß-catenin signaling plays a critical role in the terminal differentiation of osteocytes and as such, targeting Wnt/ß-catenin signaling in osteocytes may serve as a potential therapeutic approach for the management of bone-related diseases.

Superplastic nanoscale pore shaping by ion irradiation.

Exposed to ionizing radiation, nanomaterials often undergo unusual transformations compared to their bulk form. However, atomic-level mechanisms of such transformations are largely unknown. This work visualizes and quantifies nanopore shrinkage in nanoporous alumina subjected to low-energy ion beams in a helium ion microscope. Mass transport in porous alumina is thus simultaneously induced and imaged with nanoscale precision, thereby relating nanoscale interactions to mesoscopic deformations. The interplay between chemical bonds, disorders, and ionization-induced transformations is analyzed. It is found that irradiation-induced diffusion is responsible for mass transport and that the ionization affects mobility of diffusive entities. The extraordinary room temperature superplasticity of the normally brittle alumina is discovered. These findings enable the effective manipulation of chemical bonds and structural order by nanoscale ion-matter interactions to produce mesoscopic structures with nanometer precision, such as ultra-high density arrays of sub-10-nm pores with or without the accompanying controlled plastic deformations.

Bactericidal Effects of Natural Nanotopography of Dragonfly Wing on Escherichia coli.

Nanotextured surfaces (NTSs) are critical to organisms as self-adaptation and survival tools. These NTSs have been actively mimicked in the process of developing bactericidal surfaces for diverse biomedical and hygiene applications. To design and fabricate bactericidal topographies effectively for various applications, understanding the bactericidal mechanism of NTS in nature is essential. The current mechanistic explanations on natural bactericidal activity of nanopillars have not utilized recent advances in microscopy to study the natural interaction. This research reveals the natural bactericidal interaction between E. coli and a dragonfly wing's (Orthetrum villosovittatum) NTS using advanced microscopy techniques and proposes a model. Contrary to the existing mechanistic models, this experimental approach demonstrated that the NTS of Orthetrum villosovittatum dragonfly wings has two prominent nanopillar populations and the resolved interface shows membrane damage occurred without direct contact of the bacterial cell membrane with the nanopillars. We propose that the bacterial membrane damage is initiated by a combination of strong adhesion between nanopillars and bacterium EPS layer as well as shear force when immobilized bacterium attempts to move on the NTS. These findings could help guide the design of novel biomimetic nanomaterials by maximizing the synergies between biochemical and mechanical bactericidal effects.

Interaction of adult human neural crest-derived stem cells with a nanoporous titanium surface is sufficient to induce their osteogenic differentiation.

Osteogenic differentiation of various adult stem cell populations such as neural crest-derived stem cells is of great interest in the context of bone regeneration. Ideally, exogenous differentiation should mimic an endogenous differentiation process, which is partly mediated by topological cues. To elucidate the osteoinductive potential of porous substrates with different pore diameters (30 nm, 100 nm), human neural crest-derived stem cells isolated from the inferior nasal turbinate were cultivated on the surface of nanoporous titanium covered membranes without additional chemical or biological osteoinductive cues. As controls, flat titanium without any topological features and osteogenic medium was used. Cultivation of human neural crest-derived stem cells on 30 nm pores resulted in osteogenic differentiation as demonstrated by alkaline phosphatase activity after seven days as well as by calcium deposition after 3 weeks of cultivation. In contrast, cultivation on flat titanium and on membranes equipped with 100 nm pores was not sufficient to induce osteogenic differentiation. Moreover, we demonstrate an increase of osteogenic transcripts including Osterix, Osteocalcin and up-regulation of Integrin ß1 and α2 in the 30 nm pore approach only. Thus, transplantation of stem cells pre-cultivated on nanostructured implants might improve the clinical outcome by support of the graft adherence and acceleration of the regeneration process.

Oriented attachment explains cobalt ferrite nanoparticle growth in bioinspired syntheses.

Oriented attachment has created a great debate about the description of crystal growth throughout the last decade. This aggregation-based model has successfully described biomineralization processes as well as forms of inorganic crystal growth, which could not be explained by classical crystal growth theory. Understanding the nanoparticle growth is essential since physical properties, such as the magnetic behavior, are highly dependent on the microstructure, morphology and composition of the inorganic crystals. In this work, the underlying nanoparticle growth of cobalt ferrite nanoparticles in a bioinspired synthesis was studied. Bioinspired syntheses have sparked great interest in recent years due to their ability to influence and alter inorganic crystal growth and therefore tailor properties of nanoparticles. In this synthesis, a short synthetic version of the protein MMS6, involved in nanoparticle formation within magnetotactic bacteria, was used to alter the growth of cobalt ferrite. We demonstrate that the bioinspired nanoparticle growth can be described by the oriented attachment model. The intermediate stages proposed in the theoretical model, including primary-building-block-like substructures as well as mesocrystal-like structures, were observed in HRTEM measurements. These structures display regions of substantial orientation and possess the same shape and size as the resulting discs. An increase in orientation with time was observed in electron diffraction measurements. The change of particle diameter with time agrees with the recently proposed kinetic model for oriented attachment.

Review and outlook: from single nanoparticles to self-assembled monolayers and granular GMR sensors.

This paper highlights recent advances in synthesis, self-assembly and sensing applications of monodisperse magnetic Co and Co-alloyed nanoparticles. A brief introduction to solution phase synthesis techniques as well as the magnetic properties and aspects of the self-assembly process of nanoparticles will be given with the emphasis placed on selected applications, before recent developments of particles in sensor devices are outlined. Here, the paper focuses on the fabrication of granular magnetoresistive sensors by the employment of particles themselves as sensing layers. The role of interparticle interactions is discussed.