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At least 883 records · Page 49

Highly ordered self-assembled nanoscale periodic faceting in GaAs(631) homoepitaxial growth

We report on the self-assembly of large-order-correlated nanoscale faceting on GaAs(631)A substrates grown by molecular beam epitaxy. The surface morphology of the grown samples as a function of the growth temperature and the As-beam equivalent pressure was studied using atomic force microscopy. A two-dimensional autocorrelation function analysis was performed in order to quantitatively determine the uniformity of the surface corrugation. By optimizing the growth conditions, correlated faceted areas as large as 1.7 Multiplication-Sign 1.7 {mu}m{sup 2} are obtained. The highly ordered surface corrugation discussed here provides useful insights to prepare highly ordered facet planes for the self organized growth of quantum wires.

36 MATERIALS SCIENCE↗

Surface plasmon resonance in nanostructured Ag incorporated ZnS films

Silver incorporated zinc sulfide thin films are prepared by RF magnetron sputtering technique and the influence of silver incorporation on the structural, optical and luminescence properties is analyzed using techniques like grazing incidence X-Ray diffraction (GIXRD), atomic force microscopy (AFM), field emission scanning electron microscopy (FESEM), energy dispersive X-ray spectroscopy (EDS), micro-Raman spectroscopy, UV-Vis spectroscopy and laser photoluminescence spectroscopy. XRD analysis presents hexagonal wurtzite structure for the films. A reduction of crystallinity of the films is observed due to Ag incorporation. The Raman spectral analysis confirms the reduction of crystallinity and increase of strain due to the Ag incorporation. AFM analysis reveals a rough surface morphology for the undoped film and Ag incorporation makes the films uniform, dense and smooth. A blue shift of band gap energy with increase in Ag incorporation is observed due to quantum confinement effect. An absorption band (450-650 nm region) due to surface plasmon resonance of the Ag clusters present in the ZnS matrix is observed for the samples with higher Ag incorporation. The complex dielectric constant, loss factor and distribution of volume and surface energy loss of the ZnS thin films are calculated. Laser photoluminescence measurements gives an intense bluish green emission from the ZnS films and a quenching of the PL emission is observed which can be due to the metal plasmonic absorption and non-radiative energy transfer due to Ag incorporation.

36 MATERIALS SCIENCE↗

Correlation of shape changes of grain surfaces and reversible stress evolution during interruptions of polycrystalline film growth

Short interruptions of the growth of polycrystalline films often lead to stress evolution that is reversed when growth is resumed. Correlated in situ stress measurements and ex situ transmission electron microscopy and atomic force microscopy characterizations of grain boundary surface grooves as a function of the interruption time are reported for films deposited at different temperatures and held for different times before quenching to room temperature. These studies suggest that during film deposition surface grooves at grain boundaries are kinetically constrained to be shallow, while during a growth interruption surface diffusion allows grain boundary grooves to deepen and approach their equilibrium depth. The latter relieves a component of the compressive stress associated with trapped atoms in the grain boundaries. When growth is resumed, the non-equilibrium surface morphology is reestablished and the compressive stress increases to its pre-interruption value.

36 MATERIALS SCIENCE↗

Aqueous phase deposition of dense tin oxide films with nano-structured surfaces

Dense tin oxide films were successfully fabricated in an aqueous solution. The pH of the solutions was controlled to pH 1.3 by addition of HCl. Precise control of solution condition and crystal growth allowed us to obtain dense tin oxide films. Concave–convex surface of fluorine-doped tin oxide (FTO) substrates was entirely-covered with the continuous films. The films were about 65 nm in thickness and had nano-structured surfaces. Morphology of the films was strikingly different from our previous reported nano-sheet assembled structures. The films were not removed from the substrates by strong water flow or air blow to show strong adhesion strength. The aqueous solution process can be applied to surface coating of various materials such as nano/micro-structured surfaces, particles, fibers, polymers, metals or biomaterials. - Graphical abstract: Dense tin oxide films of 65 nm were successfully fabricated in an aqueous solution. They had nano-structured surfaces. Concave-convex substrates were entirely-covered with the continuous films. - Highlights: • Dense tin oxide films of 65 nm were successfully fabricated in an aqueous solution. • They had nano-structured surfaces. • Concave–convex substrates were entirely-covered with the continuous films.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Influence of period and amplitude of microwaviness on KH{sub 2}PO{sub 4} crystal's laser damage threshold

The laser induced damage threshold (LIDT) has become a technical bottleneck which restricts the application and development of the inertial confinement fusion. Using single point diamond turning method to process KH{sub 2}PO{sub 4} (KDP) crystals, the periodic microwaviness will be left on the machined surface which has a significant impact on the LIDT. In this paper, after acquiring the frequency information of machined surface of KDP crystals with the power spectral density method, we analyze quantitatively the influence of microwaviness on the LIDT of KDP crystal with the Fourier modal theory. Research results indicate that: the surface morphology of KDP crystal is consisted of the subwaviness with different characteristic spatial frequencies; and the reduced amount of the LIDT of KDP crystal leaded by such subwaviness is different; the experimental results of the LIDT are consistent with the theoretical calculations basically; for the machine tool and the processing technology we used, the leading frequency of microwaviness which caused the LIDT decreasing is between (350 {mu}m){sup -1} and (30 {mu}m){sup -1}, especially between (90 {mu}m){sup -1} and (180 {mu}m){sup -1}.

36 MATERIALS SCIENCE↗

Evaluation of the effect of organic pro-degradant concentration in polypropylene exposed to the natural ageing

The production and consumption of plastics in the last decade has recorded a remarkable increase in the scientific and industrial interest in environmentally degradable polymer (EDPs). Polymers wastes are deposited improperly, such as dumps, landfills, rivers and seas, causing a serious problem by the accumulation in the environment. The abiotic processes, like the photodegradation, are the most efficient occurring in the open environmental, where the polymers undergo degradation from the action of sunlight that result from direct exposure to solar radiation, however depend of the type of chemical ageing, which is the principal component of climatic ageing. The subject of this work is to study the influence of concentration of organic pro-degradant (1, 2 and 3 % w/w) in the polypropylene (PP) exposed in natural ageing. PP samples with and without the additive were processed in plates square form, obtained by thermal compression molding (TCM) using a press at 200°C under 2 tons for 5 min, and then were exposed at natural ageing during 120 days. The presence of organic additive influenced on PP degradability, this fact was assessed by changes in the thermal and morphology properties of the samples after 120 days of natural ageing. Scanning Electronic Microscopy (SEM) results of the morphological surface of the modified PP samples showed greater degradation photochemical oxidative when compared to neat PP, due to increase of rugosity and formation of microvoids. PP samples with different pro-degradant concentration under natural ageing presented a degree of crystallinity, obtained by Differential Scanning Calorimeter (DSC) increases in comparing the neat PP.

36 MATERIALS SCIENCE↗

Sodium Dodecyl Sulfate–Mediated Graphene Sensor for Electrochemical Detection of the Antibiotic Drug: Ciprofloxacin

The present study involves detecting and determining CIP by a new electrochemical sensor based on graphene (Gr) in the presence of sodium dodecyl sulfate (SDS) employing voltammetric techniques. Surface morphology studies of the sensing material were analyzed using a scanning electron microscope (SEM) and atomic force microscope (AFM). In the electroanalysis of CIP at the developed electrode, an enhanced anodic peak response was recorded, suggesting the electro-oxidation of CIP at the electrode surface. Furthermore, we evaluated the impact of the electrolytic solution, scan rate, accumulation time, and concentration variation on the electrochemical behavior of CIP. The possible electrode mechanism was proposed based on the acquired experimental information. A concentration variation study was performed using differential pulse voltammetry (DPV) in the lower concentration range, and the fabricated electrode achieved a detection limit of 2.9 × 10 -8 M. The proposed sensor detected CIP in pharmaceutical and biological samples. The findings displayed good recovery, with 93.8% for tablet analysis and 93.3% to 98.7% for urine analysis. The stability of a developed electrode was tested by inter- and intraday analysis.

36 MATERIALS SCIENCE↗

Isolated nano-tendril bundles on tungsten surfaces exposed to radiofrequency helium plasma

The DIONISOS experiment is used to study the impact of RF helium (He) plasma on the surface morphology of tungsten (W). Modulation of incident He ion energy with a span on the order of 50 eV and below the sputtering threshold at a frequency of 13.56 MHz results in nano-tendril bundles (NTBs) and free-standing W whiskers on the surface at 1020 K. The NTBs are distributed intra-granularly with coverage of less than 10% while reaching up to 30 microns normal to the surface for He ion fluence of 5.8 x 10^25 m^-2 and a flux density of 1.0 x 10^22 m^-2 s^-1. Analysis of the NTB interior and sub-surface structure is provided through focused ion beam cross section.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Surface-Height Determination of Crevassed Glaciers-Mathematical Principles of an Autoadaptive Density-Dimension Algorithm and Validation Using ICESat-2 Simulator (SIMPL) Data

Glacial acceleration is a main source of uncertainty in sea-level-change assessment. Measurement of ice-surface heights with a spatial and temporal resolution that not only allows elevation-change calculation, but also captures ice-surface morphology and its changes is required to aid in investigations of the geophysical processes associated with glacial acceleration.The Advanced Topographic Laser Altimeter System aboard NASAs future ICESat-2 Mission (launch 2017) will implement multibeam micropulse photon-counting lidar altimetry aimed at measuring ice-surface heights at 0.7-m along-track spacing. The instrument is designed to resolve spatial and temporal variability of rapidly changing glaciers and ice sheets and the Arctic sea ice. The new technology requires the development of a new mathematical algorithm for the retrieval of height information.We introduce the density-dimension algorithm (DDA) that utilizes the radial basis function to calculate a weighted density as a form of data aggregation in the photon cloud and considers density an additional dimension as an aid in auto-adaptive threshold determination. The auto-adaptive capability of the algorithm is necessary to separate returns from noise and signal photons under changing environmental conditions. The algorithm is evaluated using data collected with an ICESat-2 simulator instrument, the Slope Imaging Multi-polarization Photon-counting Lidar, over the heavily crevassed Giesecke Braer in Northwestern Greenland in summer 2015. Results demonstrate that ICESat-2 may be expected to provide ice-surface height measurements over crevassed glaciers and other complex ice surfaces. The DDA is generally applicable for the analysis of airborne and spaceborne micropulse photon-counting lidar data over complex and simple surfaces.

Herzfeld, Ute C.↗

Scanning Transmission X-ray Microscopy: Applications in Atmospheric Aerosol Research

Scanning transmission x-ray microscopy (STXM) combines x-ray microscopy and near edge x-ray absorption fine structure spectroscopy (NEXAFS). This combination provides spatially resolved bonding and oxidation state information. While there are reviews relevant to STXM/NEXAFS applications in other environmental fields (and magnetic materials) this chapter focuses on atmospheric aerosols. It provides an introduction to this technique in a manner approachable to non-experts. It begins with relevant background information on synchrotron radiation sources and a description of NEXAFS spectroscopy. The bulk of the chapter provides a survey of STXM/NEXAFS aerosol studies and is organized according to the type of aerosol investigated. The purpose is to illustrate the current range and recent growth of scientific investigations employing STXM-NEXAFS to probe atmospheric aerosol morphology, surface coatings, mixing states, and atmospheric processing.

47 OTHER INSTRUMENTATION↗

Growth of encapsulating carbon on supported Pt nanoparticles studied by in situ TEM

Carbon deposition on MgO-supported Pt nanoparticles from ethylene decomposition was explored by in situ transmission electron microscopy (TEM) at the atomic level. An imaging strategy was established for controlling beam-gas-sample interactions that minimizes beam-induced changes of the reaction. Using this strategy, it was possible to observe how carbon encapsulation occurs on Pt nanoparticles and the role of the Pt surface morphology. The evidence indicates that multiple partial layers grew simultaneously prior to full encapsulation of the nanoparticle. The growth of carbon on Pt nanoparticles was discovered to induce significant changes in the nanoparticle shape, resulting in particles becoming rounder as coking progressed. Closer examination of the surface structure revealed that in some cases carbon growth induced step formation.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Influence of the pH value of a colloidal gold solution on the absorption spectra of an LSPR-assisted sensor

The localized surface plasmon resonances (LSPRs) of gold particles assembled on a crystal plate are a powerful tool for biological sensors. Here, we prepare gold colloids in different pH solutions. We monitor the effects of the particle radius and particle coverage on the absorption spectra of AT-cut (r-face dihedral angle of about 3°) crystal plates supporting gold nanoparticles. The surface morphologies were monitored on silicon dioxide substrates using ultraviolet and visible (UV-vis) spectroscopy, and atomic force microscopy (AFM). The results showed that the gold particle coverage decreases with increasing pH value of the gold colloid solution. This phenomenon demonstrates that self-assembled gold surfaces were formed via the electrostatic adsorption of gold particles on the positively charged, ionized amino groups on the crystal plates in the acidic solution. The spectrum of gold nanoparticles with different coverage degree on the crystal plates showed that the LSPR properties are highly dependent on pH.

36 MATERIALS SCIENCE↗

Hydroxyapatite coating on biodegradable AZ31 and Mg-Ca alloys prepared by RF-magnetron sputtering

A thin film of hydroxyapatite (HA) was deposited on AZ31 and Mg-Ca alloys by using radio frequency (RF) magnetron sputtering. The thickness of the HA coating was determined to be 750 nm. The phase composition, microstructure, and surface morphology of the HA coatings were investigated using X-ray diffraction and scanning electron microscopy. In vitro degradation behaviour of the HA coated alloys was evaluated in simulated body fluid (SBF) and 3.5wt.% NaCl solution using electrochemical method. The coatings homogeneously covered the entire surface of the substrates. The coating structure corresponded to a nanostructured HA. The ultrathin coating significantly improved the degradation resistance of the alloy. Nanocrystalline HA coating significantly improved the corrosion resistance of the Mg-Ca and AZ31 magnesium alloys. The polarization resistance (Rp) of the coated Mg-Ca alloy was more than two-order of magnitude higher and the corrosion current density I{sub corr} reduced by ∼ 98% as compared to the base alloy.

36 MATERIALS SCIENCE↗

Microstructure of In-Core Molten Salt Corrosion Hastelloy N{sup R} and 316 Stainless Steel

Since 2011, many materials have been discussed for potential application in Fluoride salt-cooled High-temperature nuclear Reactors (FHRs), which are emerging as leading reactor concept for the next generation of nuclear reactors thanks to the benefits of a high degree of passive safety, high thermal efficiency, and low spent fuel volume. Among these discussed materials, Hastelloy N{sup R} and 316L stainless steel have been selected as the most likely candidate alloys for FHRs. To provide direct experience in integrating a real system using molten FLiBe salt for reactor operation, these two candidate alloys were experimentally tested in Li-7 enriched Li{sub 2}BeF{sub 4} (FLiBe) molten salt in the core of MIT Research Reactor (MITR) at 700 deg. C for 1000 hours. After in-core corrosion testing, some basic post-irradiation examinations (PIE) including weight change per unit area and surface profile as well as surface morphology were conducted in the MIT Nuclear Reactor Laboratory (NRL) and compared with out-of-reactor corrosion samples. The deep understanding of these alloys in high-temperature molten salt with strong neutron irradiation requires further microstructural analysis such as electron microscopy and energy dispersive spectroscopy on the surface and cross-section of the in-core corrosion tested samples. The challenge in the microstructural analysis is due to the high radioactivity from the gamma emitting isotopes formed in alloys during neutron irradiation. Additionally, the facilities that are authorized for radioactive materials are very limited on campus. In this study, the microstructure of the in-core corrosion tested Hastelloy N{sup R} and 316L stainless steel specimen was analyzed by using the facilities at the Center for Advanced Energy Studies (CAES) at Idaho National Laboratory (INL) through the Nuclear Science User Facilities (NSUF) Rapid Turnaround Experiment (RTE) program.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Optical, morphological and durability studies of quaternary chalcogenide Ge-Sb(As)-(S,Te) films

Highlights: • Films of two glassy chalcogenide systems of Ge{sub x}-Sb/As{sub 40-x}-S{sub 50}-Te{sub 10} were studied. • Optical constants as function of films composition are obtained in 0.25–30 μm range. • The transparent zone of the films is in the (0.6–2.5) μm spectral range. • The vibrational modes were determined from IR-SE, FTIR and Raman. • The stability of the films after QT was proved by AFM, SEM and SE analyses. - Abstract: Thin films from two glassy systems of Ge{sub x}Sb{sub 40-x}S{sub 50}Te{sub 10} and Ge{sub x}As{sub 40-x}S{sub 50}Te{sub 10}, with compositions x = 10, 20 and 27 at. %, were deposited on optical glass substrates by vacuum thermal evaporation of powdered parent chalcogenide glasses. The complex refractive index and dielectric constants of the films are determined by ellipsometry in a wide spectral range of 0.25–30 μm. In the transparent spectral region of 0.6–2.5 μm the refractive index values are within 2.9–2.3 and 3.3–2.4 for the As-contained and Sb-contained films, respectively. From the IR and Raman data analysis the basic chemical and oxygen-related impurity bonds are identified. The films durability properties were established by applying the US Military Standard quality tests. The quality-test-induced-changes in surface morphology were evaluated. The films are relatively stable after quality test treatments, which cause a small degree of densification and surface roughening for Sb-containing films and surface flattening for As-containing ones.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Surface defects on the Gd{sub 2}Zr{sub 2}O{sub 7} oxide films grown on textured NiW technical substrates by chemical solution method

Epitaxial growth of oxide thin films has attracted much interest because of their broad applications in various fields. In this study, we investigated the microstructure of textured Gd{sub 2}Zr{sub 2}O{sub 7} films grown on (001)〈100〉 orientated NiW alloy substrates by a chemical solution deposition (CSD) method. The aging effect of precursor solution on defect formation was thoroughly investigated. A slight difference was observed between the as-obtained and aged precursor solutions with respect to the phase purity and global texture of films prepared using these solutions. However, the surface morphologies are different, i.e., some regular-shaped regions (mainly hexagonal or dodecagonal) were observed on the film prepared using the as-obtained precursor, whereas the film prepared using the aged precursor exhibits a homogeneous structure. Electron backscatter diffraction and scanning electron microscopy analyses showed that the Gd{sub 2}Zr{sub 2}O{sub 7} grains present within the regular-shaped regions are polycrystalline, whereas those present in the surrounding are epitaxial. Some polycrystalline regions ranging from several micrometers to several tens of micrometers grew across the NiW grain boundaries underneath. To understand this phenomenon, the properties of the precursors and corresponding xerogel were studied by Fourier transform infrared spectroscopy and coupled thermogravimetry/differential thermal analysis. The results showed that both the solutions mainly contain small Gd−Zr−O clusters obtained by the reaction of zirconium acetylacetonate with propionic acid during the precursor synthesis. The regular-shaped regions were probably formed by large Gd−Zr−O frameworks with a metastable structure in the solution with limited aging time. This study demonstrates the importance of the precise control of chemical reaction path to enhance the stability and homogeneity of the precursors of the CSD route. - Highlights: •We investigate microstructure of Gd{sub 2}Zr{sub 2}O{sub 7} films grown by a chemical solution route. •The aging effect of precursor solution on formation of surface defect was thoroughly studied. •Gd−Zr−O clusters are present in the precursor solutions.

36 MATERIALS SCIENCE↗

Enhanced Catalytic Properties of Molybdenum Promoted Mesoporous Cobalt Oxide: Structure-Surface-Dependent Activity for Selective Synthesis of 2-Substituted Benzimidazoles

High-valent molybdenum ions were substituted into the cobalt oxide lattice through a one step, sol-gel method and investigated for selective synthesis of 2-substituted benzimidazoles. Catalyst synthesis involves surfactant assisted soft templating inverse micelle method, which forms mesopores by interconnected intraparticle voids. Substitutional doping of Mo 6+ resulted in materials with modified structural, morphological, surface, and redox properties. The catalytic activity increased with Mo concentration until an optimum amount (3 % Mo incorporation). Modified material shows lattice expansion, increased surface oxygen vacancies, and high surface area, which are responsible for the higher catalytic activity in selective benzimidazole synthesis reaction. A strong correlation between surface properties of the catalyst and the product selectivity was observed and plausible mechanistic and kinetic data are proposed and collected, respectively.

2-substituted benzimidazoles↗

Analysis of neptunium oxides produced through modified direct denitration

Production of neptunium-237 ( 237 Np) target materials for plutonium-238 ( 238 Pu) radioisotope thermoelectric generators (RTGs) for deep space exploration requires advanced chemistry and engineering development. Currently, the domestic Pu-238 Supply Program at Oak Ridge National Laboratory produces neptunium dioxide (NpO 2 ) for target material using a modified direct denitration (MDD) flowsheet. Although the chemistry, reaction mechanisms, and product characteristics of MDD are well understood for uranium, corresponding studies of the neptunium system are still needed to continue optimization of target material properties, production equipment design, and production flowsheets. Here, the objective of this work is to characterize crystalline phases, morphology, surface texture, and particle size of NpO 2 produced via MDD reactions. Solid-phase characterization techniques, including powder X-ray diffraction (pXRD) and scanning electron microscopy with energy-dispersive spectroscopy (SEM-EDS), were employed to achieve this objective. Subsequent data processing using the Morphological Analysis for Material Attribution (MAMA) software was performed to analyze particle morphology and size. Broadly, the powders were found to contain a mixture of NpO 2 and Np 2 O 5 after denitration with a variety of morphologies. After high-firing, the product was found to be NpO 2 with a typical polycrystalline oxide morphology and a grain size ranging from 0.72 to 0.94 µm. These analyses provide knowledge on the reaction pathway for a non-traditional NpO 2 synthesis method and offer additional unique insight into production-scale environments for transuranic materials.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗