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At least 829 records · Page 46

InP substrate evaluation by MOVPE growth of lattice matched epitaxial layers.

InP substrates form the starting point for a wide variety of semiconductor devices. The surface morphology produced during epitaxy depends critically on the starting substrate. We evaluated (1 0 0)-oriented InP wafers from three different vendors by growing thick (5 mu m) lattice-matched epilayers of InP, Gain As, and AlInAs. We assessed the surfaces with differential interference contrast microscopy and atomic force microscopy. Wafers with near singular (1 0 0) orientations produced inferior surfaces in general. Vicinal substrates with small misorientations improved the epitaxial surface for InP dramatically, reducing the density of macroscopic defects while maintaining a low RMS roughness. GaInAs and AlInAs epitaxy step-bunched forming undulations along the miscut direction. Sulfur-doped wafers were considered for singular (1 0 0) and for 0.2 degrees misorientation toward (1 1 0). We found that mound defects observed for InP and GaInAs layers on iron-doped singular wafers were absent for singular sulfur-doped wafers. These observations support the conclusion that dislocation termination at the surface and expansion of the step spiral lead to the macroscopic defects observed.

36 MATERIALS SCIENCE↗

Numerical Analysis of Molten Pool Behavior and Spatter Formation with Evaporation During Selective Laser Melting of 316L Stainless Steel

During the selective laser-melting process, material evaporation and resultant spatter are common phenomena that bring about many defects. However, the underlying physical phenomena such as molten pool behavior and spatter formation, as evaporation occurred, are sparsely understood and difficult to observe during the process. Thus, a three–dimensional powder-scale model was established to investigate the thermal and flow behavior of the molten pool, the morphology evolution of the molten pool and keyhole, and the spatter formation with evaporation in the selective laser-melting processing of 316L stainless steel. Phase transitions and variations in interfacial force were taken into account in this model. The modified phase-field method was applied to trace the melt–gas interface. The results showed that keyhole formed in molten pool under recoil pressure, and that there were some differences in the temperature distribution and flow behavior inside and outside the keyhole. In addition, the dimension and surface morphology of the molten pool and keyhole depth altered and gradually stabilized during the process. Moreover, droplet spatter formation at rear of molten pool proceeded roughly as follows: the backward ejection of melt vapor would induce a depression in molten pool and a bump on the molten pool surface, the bump moved backward and subsequently a liquid column formed, then the liquid column formed a neck and gradually pinched off, resulting in the droplet spatter. Furthermore, the characteristic morphology of the scan track and dimension of the molten pool were obtained through experiments, which showed good agreement with the simulation results.

36 MATERIALS SCIENCE↗

Characterization of diamond thin films deposited by a CO{sub 2} laser-assisted combustion-flame method

Diamond thin films were deposited by a CO{sub 2} laser-assisted O{sub 2}/C{sub 2}H{sub 2}/C{sub 2}H{sub 4} combustion-flame process. The effect of the deposition parameters, in particular the laser wavelength and power, on the film surface morphology, microstructure and phases present was the primary focus of the work. The laser power was set at 100, 400 and 800 W while the wavelength was varied and set at 10.591 {mu}m in the untuned condition and set at 10.532 {mu}m to resonantly match the CH{sub 2}-wagging vibrational mode of the C{sub 2}H{sub 4} molecule when in the tuned condition. When the laser was coupled to the combustion flame during deposition the diamond film growth was enhanced as the lateral grain size increased from 1 {mu}m to greater than 5 {mu}m. The greatest increase in grain size occurred when the wavelength was in the tuned condition. Scanning transmission electron microscopy images from focused-ion beam cross-sectioned samples revealed a sub-layer of smaller grains less than 1 {mu}m in size near the substrate surface at the lower laser powers and untuned wavelength. X-ray diffraction results showed a more intense Diamond (111) peak as the laser power increased from 100 to 800 W for the films deposited with the tuned laser wavelength. Micro-Raman spectra showed a diamond peak nearly twice as intense from the films with the tuned laser wavelength.

36 MATERIALS SCIENCE↗

Regeneration of Active Surface Alloys during Cyclic Oxidation and Reduction: Oxidation of H 2 on Pd/Ag(111)

The surface morphology and composition of a catalyst during excursions between oxidizing and reducing conditions can change substantially, especially in bimetallic alloys. Both thermodynamic and kinetic factors play a role in determining the properties of alloy surfaces where the active phase may be a metastable state. Previously, Ag oxide reduction was shown to be dramatically enhanced when Pd is on the surface; however, Pd is more stable when dissolved in Ag, raising the question as to whether a highly active Pd surface state will persist over multiple reaction cycles—a requirement for catalytic function. Experiments herein demonstrate that the enhanced chemical functionality due to the presence of Pd on the surface is retained, based on the enhanced rate of silver oxide reduction over multiple oxidation/reduction cycles for a Pd/Ag(111) model. Repeated oxidation and reduction promote PdAg alloying and reversible structural and compositional changes are detected using X-ray photoelectron spectroscopy. Furthermore, this study establishes that metastable phases can persist in reactive processes on surfaces, indicating their potential in heterogeneous catalysis.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Properties of nano structured Ag-TiO{sub 2} composite coating on stainless steel using RF sputtering method

RF Sputtering system is one of the Physical Vapour Deposition (PVD) methods that have been widely used to produce hard coating. This technique is used to deposit thin layers of metallic substrates such as stainless steel (SS). From this process, a good adhesiveness and wear resistance coating can be produced for biomedical applications. In this study, RF sputtering method was used to deposit TiO{sub 2}-Ag composite coatings via various deposition parameters. The parameters are RF power of 350W, gas composition (Ar: O{sub 2}) 50:5 and deposition time at 1, 2, 4 and 6 hours. Scanning Electron Microscopy (SEM), X-Ray Diffraction (XRD) and Raman spectroscopy were used to characterize surface area of coated samples. The formation of nanocrystalline thin film and the surface morphology were examined using SEM. The crystallite size of TiO{sub 2}-Ag composite coatings were estimated between 20-60 nm based on XRD analysis using Scherer equation and SEM evaluation. The Raman and XRD results suggested that the structure of the TiO{sub 2}-Ag consist of anatase and rutile phases. It also showed that the intensity of anatase peaks increased after samples undergone annealing process at 500 Degree-Sign C.

36 MATERIALS SCIENCE↗

Wet chemical synthesis and characterization of AgGaSe{sub 2} nanoparticles

AgGaSe{sub 2} compound semiconductor nanoparticles were synthesized by wet chemical method using mercaptoacetic acid as a capping agent at room temperature. The synthesized powders belong to chalcopyrite structure confirmed by powder XRD. The surface morphology and crystalline size were observed by high resolution scanning electron microscope (HR-SEM). The stoichiometric composition of AgGaSe{sub 2} nanoparticles was confirmed by Energy dispersive X-ray (EDX) analysis. Different functional group vibrations of mercaptoacetic acid capped nanoparticles were studied using FT-IR spectrum. The absorbance and optical bandgap of the nanoparticles were determined using diffuse reflectance spectroscopy (DRS).

36 MATERIALS SCIENCE↗

Rectifying behaviour of spin coated pn hetero-junction

Rectifying pn hetero- junction is fabricated with an acceptor p-type organic semiconductor namely tetra- chloro dihydroxy tetra-iodo fluorescein (Rose Bengal (RB)) followed by an inorganic n-type ZnO semiconductor on indium tin oxide (ITO) substrate. The n-type ZnO films are formed by unintentional doping and doping with aluminium (Al) and yttrium (Y) donors. The surface morphology and the distribution of grains are observed from scanning electron microscopy (SEM) and atomic force microscopy (AFM). The current-voltage (I-V) characteristic of the rectifying diode is measured to characterize the junction properties. The I-V plots obtained from the hetero- junction with electric contact shows a diode characteristic different from that of an ideal behavior. The overall efficiency of the diode exhibits a greater dependency on the film crystallinity, carrier concentration, and reverse saturation current.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

On shock driven jetting of liquid from non-sinusoidal surfaces into a vacuum

Other work employed Richtmyer-Meshkov theory to describe the development of spikes and bubblesfrom shocked sinusoidal surfaces. Here, we discuss the effects of machining different two-dimensional shaped grooves in copper and examine the resulting flow of the material after being shocked into liquid on release. For these simulations, a high performance molecular dynamics code, SPaSM, was used with machined grooves of kh 0 = 1 and kh 0 = 1/8, where 2h 0 is the peak-to-valley height of the perturbation with wavelength λ, and k = 2π/λ. The surface morphologies studied include a Chevron, a Fly-Cut, a Square-Wave, and a Gaussian. Furthermore, we describe extensions to an existing ejecta source model that better captures the mass ejected from these surfaces. We also investigate the same profiles at length scales of order 1 cm for an idealized fluid equation of state using the FLASH continuum hydrodynamics code. Our findings indicate that the resulting mass can be scaled by the missing area of a sinusoidal curve with an effective wavelength, λeff , that has the same missing area. Finally, our extended ejecta mass formula works well for all the shapes considered and captures the corresponding time evolution and total mass.

36 MATERIALS SCIENCE↗

Evaluation of Thermal Control Coatings for Flexible Ceramic Thermal Protection Systems

This report summarizes the evaluation and testing of high emissivity protective coatings applied to flexible insulations for the Reusable Launch Vehicle technology program. Ceramic coatings were evaluated for their thermal properties, durability, and potential for reuse. One of the major goals was to determine the mechanism by which these coated blanket surfaces become brittle and try to modify the coatings to reduce or eliminate embrittlement. Coatings were prepared from colloidal silica with a small percentage of either SiC or SiB6 as the emissivity agent. These coatings are referred to as gray C-9 and protective ceramic coating (PCC), respectively. The colloidal solutions were either brushed or sprayed onto advanced flexible reusable surface insulation blankets. The blankets were instrumented with thermocouples and exposed to reentry heating conditions in the Ames Aeroheating Arc Jet Facility. Post-test samples were then characterized through impact testing, emissivity measurements, chemical analysis, and observation of changes in surface morphology. The results show that both coatings performed well in arc jet tests with backface temperatures slightly lower for the PCC coating than with gray C-9. Impact testing showed that the least extensive surface destruction was experienced on blankets with lower areal density coatings.

Kourtides, Demetrius↗

Microstructural investigations of light-emitting porous Si layers

The structural and morphological characteristics of visible-light-emitting porous Si layers produced by anodic and stain etching of single-crystal Si substrates are compared using transmission electron microscopy and atomic force microscopy (AFM). AFM of conventionally anodized, laterally anodized and stain-etched Si layers show that the layers have a fractal-type surface morphology. The anodized layers are rougher than the stain-etched films. At higher magnification 10 nm sized hillocks are visible on the surface. Transmission electron diffraction patterns indicate an amorphous structure with no evidence for the presence of crystalline Si in the near-surface regions of the porous Si layers.

George, T.↗

Structural and optical properties of ZnO thin films grown by rapid atmospheric mist chemical vapor technique

In this work, the effect of deposition time on the structural and optical properties of ZnO films deposited by Ultrasonic Spray Mist-CVD was studied aiming the application in perovskite solar cells, as holes blocking layer. Crystallinity, surface morphology and optical properties of the ZnO films were investigated by X-ray Diffraction (XRD), Scanning Electron Microscopy (SEM), Atomic Force Microscopy (AFM), conventional and Photoluminescence (PL) spectroscopies, respectively. The XRD measurement proves the existence of the hexagonal wurtzite phase and a high degree of crystallinity with [001] preferential orientation. The SEM study shows that the films possess a compact structure. Smooth and homogenous surface was confirmed also by AFM. The obtained results indicate that ZnO films deposited by a simple, safe and cost-effective method present a great potential for application in perovskite solar cells.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Sol–gel method as a way of carbonyl iron powder surface modification for interaction improvement

This article presents a method for modification of carbonyl iron particles’ surface (CIP), (d{sub 50}=4–9 µm) by silica coatings obtained using the sol–gel method. Reaction parameters were determined to obtain dry magnetic powder with homogeneous silica coatings without further processing and without any by-product in the solid or liquid phase. This approach is new among the commonly used methods of silica coating of iron particles. No attempt has been made to cover a carbonyl iron surface by silica in a waste-free method, up to date. In the current work two different silica core/shell structures were made by the sol–gel process, based on different silica precursors: tetraethoxy-silane (TEOS) and tetramethoxy-silane (TMOS). The dependence between the synthesis procedure and thickness of silica shell covering carbonyl iron particles has been described. Surface morphology of the modified magnetic particles and the coating thickness were characterized with the use of scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Determination of the physicochemical structure of the obtained materials was performed by the energy-dispersive X-ray spectroscope (EDS), and the infrared technique (IR). The surface composition was analyzed using X-ray photoelectron spectroscopy (XPS). Additionally, distribution of particle size was measured using light microscopy. The new, efficient process of covering micro-size CIP with a nanometric silica layer was shown. Results of a performed analysis confirm the effectiveness of the presented method. - Highlights: • Proper covering CIP by sol–gel silica layer avoids agglomeration. • A new solid waste-free method of CIP coating is proposed. • Examination of the properties of modified CIP in depends on washing process. • Coatings on CIP particles doesn’t change the magnetic properties of particles.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Observing Chemical and Morphological Changes in a Cu@TiO x Core@Shell Catalyst: Impact of Reversible Metal-Oxide Interactions on CO 2 Activation and Hydrogenation

A combination of several in-situ techniques (XRD, XAS, AP-XPS, E-TEM) was used to explore links between the structural and chemical properties of a Cu@TiO x catalyst under CO 2 hydrogenation conditions. The active phase of the catalyst involved an inverse oxide/metal configuration, but the initial core@shell motif was disrupted during the pre-treatment in H 2 . As a consequence of strong metal-support interactions, the titania shell cracked and Cu particles migrated from the core to on top of the oxide with the simultaneous formation of a Cu-Ti-O x phase. The generated Cu particles had a diameter of 20-40 nm and were decorated by small clusters of TiO x (< 5 nm in size). Results of in-situ XAS and XRD and images of E-TEM showed a very dynamic system, where the inverse oxide/metal configuration promoted the reactivity of the system towards CO 2 and H 2 . At room temperature, CO 2 oxidized the Cu nanoparticles (CO 2,gas → CO gas + O oxide ) inducing a redistribution of the TiO x clusters and big modifications in catalyst surface morphology. The generated oxide overlayer disappeared at elevated temperatures (> 180 °C) upon exposure to H 2 , producing a transient surface that was very active for the reverse water-gas shift reaction (CO 2 + H 2 → CO + H 2 O) but was not stable at 250 °C. When oxidation and reduction occurred at the same time, under a mixture of CO 2 and H 2 , the surface structure evolved toward a dynamic equilibrium that strongly depended on the temperature. Neither CO 2 nor H 2 can be considered as passive reactants. In the Cu@TiO x system, morphological changes were linked to variations in the composition of metal-oxide interfaces which were reversible with temperature or chemical environment and affected the catalytic activity of the system. Finally, the present study illustrates the dynamic nature of phenomena associated with the trapping and conversion of CO 2 .

36 MATERIALS SCIENCE↗

Enhanced field emission properties of tilted graphene nanoribbons on aggregated TiO{sub 2} nanotube arrays

Highlights: • Graphene nanoribbons (GNBs) slanted on aggregate TiO{sub 2} nanotube (A-TNTs) as field-emitters. • Turn-on electric field and field enhancement factor β are dependent on the substrate morphology. • Various quantities of GNRs are deposited on top of A-TNTs (GNRs/A-TNTs) with different morphologies. • With an increase of GNBs compositions, the specimens' turn-on electric field is reduced to 2.8 V/μm. • The field enhancement factor increased rapidly to about 1964 with the addition of GNRs. - Abstract: Graphene nanoribbons (GNRs) slanted on aggregate TiO{sub 2} nanotube arrays (A-TNTs) with various compositions as field-emitters are reported. The morphology, crystalline structure, and composition of the as-obtained specimens were characterized by field-emission scanning electron microscopy (FE-SEM), X-ray diffraction (XRD) and Raman spectrometry. The dependence of the turn-on electric field and the field enhancement factor β on substrate morphology was studied. An increase of GNRs reduces the specimens’ turn-on electric field to 2.8 V/μm and the field enhancement factor increased rapidly to about 1964 with the addition of GNRs. Results show a strong dependence of the field emission on GNR composition aligned with the gradient on the top of the A-TNT substrate. Enhanced FE properties of the modified TNTs can be mainly attributed to their improved electrical properties and rougher surface morphology.

36 MATERIALS SCIENCE↗

Microstructural and Superconducting Radiofrequency Properties of Multilayer Sequentially Sputtered Nb 3 Sn films

Nb 3 Sn is considered as a potential candidate for superconducting radiofrequency cavities for particle acceleration due to its higher transition temperature of 18.3 K and higher superheating field of 400 mT. Nb 3 Sn films can be grown inside the surface of a Nb cavity by sequentially sputtering multiple layers of Nb and Sn thin films followed by annealing at 950 °C for 3 h. We report on the properties of Nb 3 Sn films grown on Nb substrates by magnetron sputtering. The films’ crystal structure, surface morphology, and composition were characterized by X-ray diffraction, scanning electron microscopy, and energy-dispersive X-ray spectroscopy. The films had a polycrystalline Nb 3 Sn structure with a fine-grain surface and an atomic Sn composition of ~23%. The RF surface resistance of the films was measured for different temperatures at 7.4 GHz to understand the feasibility of this method for the SRF application. The RF surface resistance of the films was 5 mΩ at 12 K, which is about 2 orders of magnitude higher than 60 μΩ previously measured in Nb 3 Sn films grown by Sn vapor diffusion. Finally, the sputtered film had a superconducting transition at 17.2 K, which is also lower than 17.9 K observed in Nb 3 Sn film prepared by vapor diffusion.

43 PARTICLE ACCELERATORS↗

Microtopographic evolution of lava flows at Cima volcanic field, Mojave Desert, California

Microtopographic profiles were measured and power spectra calculated for dated lava flow surfaces at Cima volcanic field in the eastern Mojave Desert of California in order to quantify changes in centimeter- to meter-scale roughness as a function of age. For lava flows younger than about 0.8 m.y., roughness over all spatial scales decreases with age, with meter-scale roughness decreasing slightly more than centimeter scales. Flows older than about 0.8 m.y. show a reversal of this trend, becoming as rough as young flows at these scales. Modeling indicates that eolian deposition can explain most of the change observed in the offset, or roughness amplitude, of power spectra of flow surface profiles up to 0.8 m.y. Other processes, such as rubbing and stone pavement development, appear to have a minor effect in this age range. Changes in power spectra of surfaces older than about 0.8 m.y. are consistent with roughening due to fluvial dissection. These results agree qualitatively with a process-response model that attributes systematic changes in flow surface morphology to cyclic changes in the rates of eolian, soil formation, and fluvial processes. Identification of active surficial processes and estimation of the extent of their effects, or stage of surficial evolution, through measurement of surface roughness will help put the correlation of surficial units on a quantitative basis. This may form the basis for the use of radar remote sensing data to help in regional correlations of surficial units.

Farr, Tom G.↗

Probing the Influence of Thermally Induced Structural Changes on the Microstructural Evolution in Shale using Multiscale X-ray Scattering Measurements

Various pathways to accelerate the recovery of hydrocarbons from unconventional subsurface environments have been proposed, including the use of high-temperature fluids. However, the influence of temperature on the structural and microstructural changes in complex subsurface materials characterized by compositional and morphological heterogeneity are not very well understood. In this study, in operando ultrasmall angle, small angle, and wide-angle X-ray scattering (USAXS/ SAXS/WAXS) measurements were performed to link the structural and morphological changes in shale when heated from 30 to 1150 °C. The structural changes observed from the wide-angle X-ray scattering measurements were complemented by the changes in the porosity, particle size, and surface morphology. Overall, we report the combined USAXS/SAXS measurements showed enhanced smoothness in the pore–solid interface on heating. The dehydroxylation of illite and calcination of calcium carbonate were noted prior to the formation of denser and sintered silicate and alumino-silicate phases such as Mg 2 SiO 4 (forsterite), Fe 0.3 Mg 0.7 (SiO 3 ) (enstatite), and Al 2.35 Si 0.64 O 4.82 (mullite).

54 ENVIRONMENTAL SCIENCES↗

Laser-metal interaction dynamics during additive manufacturing resolved by detection of thermally-induced electron emission

In situ monitoring is required to improve the understanding and increase the reliability of additive manufacturing methods such as laser powder bed fusion (LPBF). Current diagnostic methods for LPBF capture optical images, X-ray radiographs, or measure the emission of thermal or acoustic signals from the component. Herein, a methodology based on the thermal emission of electrons - thermionic emission - from the metal surface during LPBF is proposed which can resolve laser-material interaction dynamics. The high sensitivity of thermionic emission to surface temperature and surface morphology is revealed to enable precise determination of the transition between conduction and keyhole mode melting regimes. Increases in thermionic emission are correlated to laser scanning conditions that give rise to pore formation and regions where surface defects are pronounced. The information presented here is a critical step in furthering our understanding and validation of laser-based metal additive manufacturing.

36 MATERIALS SCIENCE↗