Nano-porous palladium (Pd) thin films could potentially be applied to hydrogen gas sensing materials with high sensitivity and selectivity. In our previous study, a nano-porous Pd film was fabricated with a three-dimensional network structure from an AlPd mother alloy film by a dealloying method using the chelating ability of an organic acid. This process was simple and environmentally friendly because it only required organic acid in a ppm concentration, and did not exhaust a strong acid waste solution, including heavy metal ions. This method was modified to improve the Pd purity of the dealloyed specimen, reaction rate, and morphology control. In this study, the existence of a composition undulation pattern was shown in the AlPd mother alloy film, and its effects on the morphology of the dealloyed specimen were evaluated. Furthermore, this pattern could be controlled by N2 gas addition to the Ar sputtering gas during the preparation of the AlPd mother alloy film.

Data-centric approaches have become increasingly popular in materials science, also known as informational materials science. Nanostructures often play essential roles in materials properties. Nanoinformatics is an important subset of informational materials science and a powerful tool for characterization and design of nanostructures. It allows discovery of meaningful and useful information and patterns from experimental and theoretical data and databases. This article reviews progress in nanoinformatics and informational materials science. Data-centric approaches for materials property description, construction of interatomic potentials, discovery of new inorganic compounds, efficient characterization of ionic transport and interfacial structures, hyperspectral image data analysis, and design of catalytic nanoparticles are outlined.

A complex mechanism of interfacial oxygen scavenging is revealed by electron energy-loss spectroscopy (EELS) for a resistive switching oxide of SrTiO3 with a scavenging layer of Ta. When Ta thin layer is inserted at one of the interfaces of Pt/SrTiO3/Pt structure, a large reduction of electrical resistance is induced for the structure, and oxygen defects are introduced at the interfacial part of SrTiO3. In the resistance decrease by voltage applications, simultaneous occurrence of oxidation and reduction of Ta scavenging layer is shown by EELS analyses from the low-loss spectra. The EELS and scanning transmission electron microscopy observations demonstrate that oxygen scavenging by Ta layer is an interfacial phenomenon where the redox reactions occur at the whole part of the interface. In addition, Pt electrode of the structure, which is chemically inert for oxidation, is revealed to have significant effects in the scavenging processes.

A bilayer film deposition process for synthesizing ultrathin amorphous carbon (a-C) films with structure and properties dominated by those of the sp3-rich bulk layer was developed in this study. This was accomplished by incorporating in conventional filtered cathodic vacuum arc (FCVA) deposition a low-ion-energy pre-deposition step (no substrate biasing) leading to the formation of an ultrathin (<1 nm) carbon layer and a post-deposition step of high-energy Ar+ ion sputtering resulting in film thinning. The thickness and cross-sectional structure of hydrogen-free a-C ultrathin films synthesized by this multistep FCVA process under optimum substrate bias conditions (−100 V pulsed bias voltage) were examined by high-resolution transmission electron microscopy and electron energy loss spectroscopy. The bilayer a-C films synthesized under these conditions exhibit slightly higher sp3 fractions and interface and bulk layers significantly thinner and thicker, respectively, compared with single-layer a-C films of similar thickness deposited under the same FCVA conditions.

A scale formed by heat treatment of Ti in a nitrogen atmosphere containing oxygen at an extremely low partial pressure exhibited an exceptional degree of hydroxyapatite (HAp) formation in a simulated body fluid. Scanning transmission electron microscopy and electron energy loss spectroscopy indicated that the subsurface of this scale was composed of nitrogen doped rutile-type TiO2. The N-K edge energy-loss near edge structure spectrum of this layer in conjunction with the theoretical spectra of possible compounds obtained using the augmented plane wave plus local orbital band method suggested that oxygen sites were replaced by two nitrogens, resulting in an effective charge of +2. The enhanced HAp forming ability of this scale is likely related to the positively charged surface induced by the presence of N. Conversely, the subsurface scale formed by heat treatment in air, in which N is not found, leads to much slower HAp coverage, believed to be related to the lack of surface charge.

Phase separation of InxGa1-xN alloys into Ga-rich and In-rich regions was observed by a number of research groups for samples grown with high indium content, x. Due to the radiation sensitivity of InGaN to beam damage by fast electrons, high-resolution imaging in transmission electron microscopy (TEM) or core-loss electron energy-loss spectroscopy (EELS) may lead to erroneous results. Low-loss EELS can yield spectra of the plasmon loss regions at much lower electron fluxes. Unfortunately, due to their delayed edge onset, the low energetic core losses of Ga and In partially overlap with the plasmon peaks, all of which shift with indium content.

Here we demonstrate a method to quantify phase separation in InGaN thin films from the low-loss region in EELS by simultaneously fitting both plasmon and core losses over the energy range of 13-30eV. Phase separation is shown to lead to a broadening of the plasmon peak and the overlapping core losses, resulting in an unreliable determination of the indium concentration from analyzing the plasmon peak position alone if phase separation is present. For x=0.3 and x=0.59, the relative contributions of the binary compounds are negligibly small and indicate random alloys. For xnom.=0.62 we observed strong broadening, indicating phase separation.

A nanoporous carbon (C) material, functionalized with Cobalt-Oxide/Cobalt (CoO/Co) core-shell nanoparticles (NPs), was structurally and chemically characterized with transmission electron microcopy (TEM) while its electrochemical response for Lithium ion battery (LIB) applications was evaluated as well. The results herein show that the nanoporous C material was uniformly functionalized with the CoO/Co core-shell NPs. Further the NPs were crystalline with fcc-type lattice on the Co2+ oxide shell and hcp-type core of metallic Co0. The electrochemical study was carried out by using galvanostatic charge/discharge cycling at a current density of 1000 mA g−1. The potential of this hybrid material for LIB applications was confirmed and it is attributed to the successful dispersion of the Co2+/ Co0 NPs in the C support.

A systematic x-ray diffraction (XRD) study was performed on room-temperature Xe-irradiated and postirradiation annealed CeO2. Large scale XRD did not show any additional irradiation-induced phases upon irradiation. Depth profiling the CeO2 (111) diffraction peak over the 150 nm deep Xe-irradiated layer (400 keV, 1 × 1020 Xe/m2) by grazing incidence XRD indicated a lattice expansion at the irradiated layer. Postirradiation annealing (1 h at 1000 °C) in an oxygen-containing environment removed the observed XRD features. Electron energy loss spectroscopy (EELS) was performed for cross-sectional samples before and after postirradiation annealing. EELS showed that the Ce charge state changed from +4 to +3 at the CeO2 surface indicating the presence of O vacancies in both as-irradiated and annealed samples. EELS also indicated that the amount of O vacancies was reduced at the irradiated region by annealing. The experimental results are discussed based on electronic properties of CeO2, annihilation of oxygen vacancies, and evolution of irradiation damage.

The emission of crystalline silicon nanoparticles as well as nanowires can be tuned by varying their diameters. The diameter selection is achieved via a difficult chemical procedure that necessitates filtration which cannot be easily scaled up. Herein, we report a novel approach for producing and tuning the emission of freestanding colloidal of amorphous porous silicon nanoparticles (which should not be confused with bulk amorphous silicon nor with porous silicon) via a controlled oxidation without relying on size of nanoparticles. This oxidation increases local strain in the disordered network that causes orbital interactions which modifies the band-gap but a new hybridization.

In his famous 1959 lecture “There’s plenty of room at the bottom,” Richard Feynman put out this challenge: “Is there no way to make the electron microscope more powerful?” He called for “improving the electron microscope by a hundred times,” which, given that the resolution then was about 10 Å, meant he was calling for a resolution in the range of 0.1 Å. Today’s aberration-corrected microscopes have come a long way, achieving a resolution of around 0.5 Å. This has enormously improved our ability to see atomic arrangements in crystals, measure ferroelectric displacements, and even determine valence and spin states with electron energy-loss spectroscopy. However, there remain many structures crucial to materials properties that we cannot yet see. Continuing the road toward Feynman’s goal would bring these structures to light, with yet more dramatic impacts on the entire field of materials science.

BaTiO3–SnO solid solutions have been investigated from the viewpoints of synthesis and Sn ion valence. First-principles calculations show that the solution energy of Sn2+ into the Ba sites in BaTiO3 is less than that into the Ti sites under high pressure. The BaTiO3–SnO solid solutions have been synthesized under high pressure (∼20 GPa) and temperatures using a laser-heated diamond anvil cell. The synthesized materials have been characterized using x-ray diffractometry, scanning transmission electron microscopy, and energy-dispersive x-ray spectroscopy. It is found from these various methods that we have successfully synthesized uniform solid solutions of BaTiO3–SnO. Furthermore, it is also clarified by the Sn L3-edge electron energy loss spectra measurements that the valences of the Sn ions in the BaTiO3–SnO solid solution are 2+. These results indicate that the Sn2+ ions are substituted into the Ba sites, according to the ion size. Consequently, the Sn ions can be substituted into the Ba sites of the shrinking BaTiO3 lattice under high pressure, which is similar to the Ca and Sn co-substitution into Ba sites under ambient pressure as reported previously.

Atomic-resolution structural and spectroscopic characterization techniques (scanning transmission electron microscopy and electron energy loss spectroscopy) are combined with nanoscale electrical measurements (conductive atomic force microscopy) to study at the atomic scale the properties of graphene grown epitaxially through the controlled graphitisation of Si-face and C-face hexagonal SiC(0001) substrates by high temperature annealing. A scanning transmission electron microscopy analysis, carried out at 60KeV of beam energy, below the knock-on threshold for carbon to ensure no damage is imparted to the film by the electron beam, demonstrates that the buffer layer present on the planar SiC(0001) Si-face delaminates from it on the (11-2n) facets of SiC surface steps, In addition, electron energy loss spectroscopy reveals that the delaminated layer has a similar electronic configuration to purely sp2-hybridized graphene. A thin amorphous film is found on the C-face, instead, which strongly suppresses epitaxy with the SiC substrate. Structurally, the amorphous area is inhomgeneous, as its Si-concentration gradually decreases while approaching the first graphene layer, which is purely sp2-hybridized. Based on these features, we discuss differences and similarities between the C-only buffer layer that forms on the Si-face of SiC with respect to the thicker C/Si amorphous film of the C-face.

The preparation of site-specific atom-probe tomography (APT) samples containing localized features has become possible with the use of focused ion beams (FIBs). This technique was used to achieve the analysis of surface oxides and oxidized grain boundaries in this paper. Transmission electron microscopy (TEM), providing microstructural and chemical characterization of the same features, has also been used, revealing crucial additional information.

The study of grain boundary oxidation in stainless steels and nickel-based alloys is required in order to understand the mechanisms controlling stress corrosion cracking in nuclear reactors. Samples oxidized under simulated pressurized water reactor primary water conditions were used, and FIB lift-out TEM and APT specimens containing the same oxidized grain boundary were prepared and fully characterized. The results from both techniques were found fully consistent and complementary.

Chromium-rich spinel oxides grew at the surface and into the bulk material, along grain boundaries. Nickel was rejected from the oxides and accumulated ahead of the oxidation front. Lithium, which was present in small quantities in the aqueous environment during oxidation, was incorporated in the oxide. All phases were accurately quantified and the effect of different experimental parameters were analysed.

This article shows how the scanning transmission electron microscope provides a Z-contrast image (where Z is atomic number) that is often directly interpretable and can show higher resolution than a phase-contrast image. It represents an incoherent mode of imaging, similar to that described by Lord Rayleigh for the optical microscope over a century ago. Today, resolution has reached a half Ångstrom, and spectroscopic analysis of individual atomic columns, even of individual atoms in two-dimensional materials, has become possible.

This paper reports on the defect structures formed upon strain relaxation in pulsed laser-deposited complex oxide superlattices consisting of the ferromagnetic metal, La0.67Sr0.33MnO3, and the antiferromagnetic insulator, La0.67Sr0.33FeO3. Atomic resolution scanning transmission electron microscopy and electron energy loss spectroscopy were used to characterize the structure and chemistry of the defects. For thinner superlattices, strain relaxation occurs through the formation of 2-D stacking faults, whereas for thicker superlattices, the prolonged thermal exposure during film growth leads to the formation of nanoflowers and cracks/pinholes to reduce the overall strain energy.

The possibility has recently been reported of using spatially resolved electron energy loss spectroscopy and cathodoluminescence in scanning (transmission) electron microscopes to probe optical excitations—plasmons, photons, excitons—at a scale that could not have been considered only a few years ago. This allows these excitations to be studied at the relevant scale for the characterization of novel materials with potential applications in nanophotonics and nanoplasmonics. This review aims at describing the state-of-the art experimental and theoretical techniques of this emerging field and its major uses and applications.

The high sensitivity of electron energy-loss spectroscopy (EELS) for detecting light elements at the nanoscale makes it a valuable technique for application to biological systems. In particular, EELS provides quantitative information about elemental distributions within subcellular compartments, specific atoms bound to individual macromolecular assemblies, and the composition of bionanoparticles. EELS data can be acquired either in the fixed beam energy-filtered transmission electron microscope (EFTEM) or in the scanning transmission electron microscope, and recent progress in the development of both approaches has greatly expanded the range of applications for EELS analysis. Near single atom sensitivity is now achievable for certain elements bound to isolated macromolecules, and it becomes possible to obtain three-dimensional compositional distributions from sectioned cells through EFTEM tomography.

We fabricated Fe3O4 thin films on TiN buffered Si by CO/CO2 oxidation at 160 °C. The easy saturation of the magnetization at high magnetic field and high resolution scanning transmission electron microscopy (HRSTEM) images show low defect density, smooth Fe3O4 thin films. Oxidation at 400 °C resulted in an undesirable second phase in between the TiN and the un-oxidized Fe, but changes in total gas pressure did not lead to a second phase. The crystal structure of this second phase is similar to Fe2TiO4 (ulvöspinel) from HRSTEM and STEM electron energy loss spectroscopy. Fe3O4 thin films grown at 160 °C follow a power law growth model with an exponent of 0.23±0.03.

Nonresonant inelastic x-ray scattering (NIXS) measurements probing the 5d → 5f electronic transitions at the uranium O4,5 edges in a localized electron system such as UO2 show a good agreement with many-electron atomic spectral calculations. The higher multipole spectra are split into two peaks that can be assigned as the 5d5/2 and 5d3/2 structures, despite the large electrostatic interactions. A new sum rule for the branching ratio of spin-orbit split core levels in electric multipole spectra, which generalizes the sum rule for dipole transitions in x-ray absorption spectroscopy, allows for a systematic analysis of the NIXS spectra. The branching ratio is linearly proportional to the expectation value of the angular part of the spin-orbit interaction in the initial state, where the rank of the multipole determines the coefficient of the linear dependence. This spin-orbit sum rule can be an important diagnostic tool for high-energy spectroscopies.

Energy-filtered transmission electron microscopy (EFTEM) yields new possibilities for the investigation of Bi2Te3 based nanomaterials. Combined low-loss electron energy-loss spectroscopy (EELS) and energy-dispersive x-ray microanalysis (EDS) and energy-filtered TEM were applied on a Zeiss 912Ω TEM to investigate nanowires, thin films, and bulk materials. Multilayered Bi-Sb-Te nanowires with a diameter of 65 nm and a period of 200 nm and stoichiometric Bi2Te3 nanowires were grown by potential-pulsed electrochemical deposition. Tellurium elemental maps of the multilayered nanowires were obtained by two-window edge-jump ratio images (EJI). EDS chemical analysis showed that small Te fluctuations of 3 at.% yielded significant contrast in EJI. Energy-filtered TEM applied on nano-alloyed Bi2Te3 thin films grown by molecular beam epitaxy (MBE) revealed 10-20 nm thick Bi-rich blocking layers at grain boundaries. Plasmon spectroscopy by EELS was applied on Bi2(Te0.91Se0.09)3 bulk and yielded a plasmon energy of 16.9 eV. Finally, plasmon dispersion was measured for Bi2(Te0.91Se0.09)3 bulk by angle-resolved EELS, which yields a fingerprint of the anisotropy and the dimensionality of the electronic structure of the materials.