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At least 37 records · Page 2

Advanced nanoscale characterization of aluminum nanoparticles with modified surface morphology via atmospheric helium and carbon monoxide plasmas

Aluminum nanoparticles (nAl) have the potential as energetic additives in explosive/propellant formulations. Scalable methodologies must be pursued to mitigate the inactive amorphous alumina shell surrounding the active aluminum (Al) core with modified surface morphology and chemistry for increased combustion effects. This work explores the feasibility of making reactive core/shell nAl with thinned oxide shells and modified surface coatings via a two-step atmospheric plasma surface treatment process in a custom dielectric barrier discharge plasma reactor. The commercial nAl of nominal average size similar to 40-60nm was first treated with helium (He) followed by He/carbon monoxide (CO) plasmas for different durations. The resultant samples were characterized via high-resolution transmission electron microscopy (HRTEM) and Fourier transform IR (FTIR) spectra. HRTEM images revealed sporadic patchy gamma -alumina deposits on particle surfaces and in gaps among particles for all samples, suggesting the non-uniform plasma effects of the He/CO glow. Nanoscale chemical analyses via scanning transmission electron microscopy elemental mapping and x-ray energy dispersive spectroscopy were further performed. Although no carbon-associated structure appeared in electron energy loss spectroscopy (EELS) spectra, the presence of carbonaceous materials was confirmed as a thin dispersive layer evenly distributed on the nAl surface suggesting either its amorphous nature or is present at a level insufficient to generate satisfactory EELS spectra. The trend of intensity profiles for key elements acquired by drawing lines across a single particle on the elemental maps confirmed that carbonaceous materials only existed on the surface and they were most likely carboxylates that increased with increased He/CO treatment duration, as evident by FTIR results. Finally, this work demonstrated the success of atmospheric plasma-treated reactive nAl with comprehensively characterized surface features via advanced microscopy and spectroscopy.

36 MATERIALS SCIENCE↗

Surface morphology of erbium silicide

The surface of rare-earth silicides (Er, Tb, etc.), formed by the reaction of thin-film metal layers with a silicon substrate, is typically dominated by deep penetrating, regularly shaped pits. These pits may have a detrimental effect on the electronic performance of low Schottky barrier height diodes utilizing such silicides on n-type Si. This study suggests that contamination at the metal-Si or silicide-Si interface is the primary cause of surface pitting. Surface pits may be reduced in density or eliminated entirely through either the use of Si substrate surfaces prepared under ultrahigh vacuum conditions prior to metal deposition and silicide formation or by means of ion irradiation techniques. Silicide layers formed by these techniques possess an almost planar morphology.

Lau, S. S.↗

Atomic force microscopy and scanning electron microscopy characterization of the controlling of surface morphology of epoxy‐amine‐cured spin‐coated films

Abstract Atomic force microscopy (AFM) was successfully used to study spin‐coated, amine‐cured epoxy film microstructure and morphology. The air‐epoxy and epoxy‐substrate interfaces were examined using tapping‐mode height and phase imaging AFM. The impact of relative humidity on the morphology and microstructure of the surfaces was determined. AFM was able to elucidate the changes on the surface as relative humidity during processing increased. It was observed that large nodular formations formed on the epoxy surface expose to the air but not epoxy surface formed on the substrate in addition to varying regions of more or less compliant structures, which was attributed to carbamate formation caused by the amine curing agent reaction with atmospheric CO 2 . Scanning electron microscopy (SEM) was used to further elucidate interface and interphase morphology of spin‐coated epoxies. Experimentation also demonstrated that post‐curing above the glass transition did not change the morphology structure, suggesting surface structures are “locked‐in.” SEM was used to further elucidate how the interface and interphase change with changing environmental conditions at both the air‐epoxy and epoxy‐substrate interface/interphases, including the impact of atmospheric CO 2 on Marangoni cell formation.

Shenk, Timothy M.↗

Analysis of the Surface Morphology and Chemical Composition of Zr-Nb3Sn Alloys with Zr Different Concentrations

The Zr inclusion in Nb3Sn can improve the high magnetic field performance of Nb3Sn radio frequency cavities. The focus of this project is to characterize the surface properties and chemical composition of Zr-Nb3Sn. Nb3Sn was doped with two different concentrations of Zr. ~0.5%, and ~24% Zr. Various spectroscopy techniques were used to examine how the surface morphology and chemical composition changes with increasing Zr fraction in Nb3Sn.

Sue, Micah↗

Ion beam sputter modification of the surface morphology of biological implants

The surface chemistry and texture of materials used for biological implants may significantly influence their performance and biocompatibility. Recent interest in the microscopic control of implant surface texture has led to the evaluation of ion beam sputtering as a potentially useful surface roughening technique. Ion sources, similar to electron bombardment ion thrusters designed for propulsive applications, are used to roughen the surfaces of various biocompatible alloys or polymer materials. These materials are typically used for dental implants, orthopedic prostheses, vascular prostheses, and artificial heart components. Masking techniques and resulting surface textures are described along with progress concerning evaluation of the biological response to the ion beam sputtered surfaces.

Weigand, A. J.↗

Ion-beam-sputter modification of the surface morphology of biological implants

The surface chemistry and texture of materials used for biological implants may significantly influence their performance and biocompatibility. Recent interest in the microscopic control of implant surface texture has led to the evaluation of ion-beam sputtering as a potentially useful surface roughening technique. Ion sources, similar to electron-bombardment ion thrusters designed for propulsive applications, are used to roughen the surfaces of various biocompatible alloys or polymer materials. These materials are typically used for dental implants, orthopedic prostheses, vascular prostheses, and artificial heart components. Masking techniques and resulting surface textures are described along with progress concerning evaluation of the biological response to the ion-beam-sputtered surfaces.

Weigand, A. J.↗

Surface Morphology of Undoped and Doped ZnSe Films

Rare-earth doped ions in polar II-VI semiconductors have recently played an important role in the optical properties of materials and devices. In this study, undoped ZnSe and erbium doped ZnSe films were grown by radio frequency (RF) magnetron sputtering method. Atomic Force Microscopy (AFM) was used together with optical microscopy and UV-Vis spectroscopy to characterize the films. Doped samples were found to have higher surface roughness and quite different surface morphology compared to that of undoped samples. The grown films generally show a relatively smooth and uniform surface indicating that they are of overall good quality. The impact of plasma etching on ZnSe:Er film examined under AFM is also discussed.

George, T.↗

Analysis of the Surface Morphology and Chemical Composition of Zr-Nb3Sn Alloys with Zr Different Concentrations

The inclusion of zirconium (Zr) in niobium-tin (Nb3Sn) significantly enhances the performance of Nb3Sn radiofrequency cavities in high magnetic fields. This research project is dedicated to characterizing the surface properties and chemical composition of Zr-doped Nb3Sn. Two different concentrations of Zr were used for doping: approximately 0.5% and 24%. Various spectroscopy techniques were employed to analyze how the surface morphology and chemical composition of Nb3Sn change with increasing Zr content. The findings of this study indicate that the grain size decreases as the Zr concentration increases. In samples with 24% Zr, nanometer-sized particles, likely oxides, were observed. X-ray photoelectron spectroscopy (XPS) data revealed that the thickness of niobium oxides (NbOx) decreases with increasing Zr, while the thickness of tin oxides (SnOx) increases. Additionally, grain size distribution analysis showed that the average grain size is around 5300 nm , with a grain area density of about 165 grains/μm .

Sue, Micah↗

The Seismic Effect of Impacts on Asteroid Surface Morphology: Early Modeling Results

In recent years, spacecraft observations of asteroids 951 Gaspra, 243 Ida, 253 Mathilde, and 433 Eros have shown the overriding dominance of impact processes with regard to the structure and appearance of these small, irregular bodies. One currently unanswered question is: to what degree does seismic shaking from impacts affect the surface morphology of these bodies? Through detailed modeling, we begin to address this question.

Richardson, J. E.↗

Sputter-Deposited Mo Thin Films: Multimodal Characterization of Structure, Surface Morphology, Density, Residual Stress, Electrical Resistivity, and Mechanical Response

Multimodal datasets of materials are rich sources of information which can be leveraged for expedited discovery of process–structure–property relationships and for designing materials with targeted structures and/or properties. For this data descriptor article, we provide a multimodal dataset of magnetron sputter-deposited molybdenum (Mo) thin films, which are used in a variety of industries including high temperature coatings, photovoltaics, and microelectronics. In this dataset we explored a process space consisting of 27 unique combinations of sputter power and Ar deposition pressure. Here, the phase, structure, surface morphology, and composition of the Mo thin films were characterized by x-ray diffraction, scanning electron microscopy, atomic force microscopy, and Rutherford backscattering spectrometry. Physical properties—namely, thickness, film stress and sheet resistance—were also measured to provide additional film characteristics and behaviors. Additionally, nanoindentation was utilized to obtain mechanical load-displacement data. The entire dataset consists of 2072 measurements including scalar values (e.g., film stress values), 2D linescans (e.g., x-ray diffractograms), and 3D imagery (e.g., atomic force microscopy images). An additional 1889 quantities, including film hardness, modulus, electrical resistivity, density, and surface roughness, were derived from the experimental datasets using traditional methods. Minimal analysis and discussion of the results are provided in this data descriptor article to limit the authors’ preconceived interpretations of the data. Overall, the data modalities are consistent with previous reports of refractory metal thin films, ensuring that a high-quality dataset was generated. The entirety of this data is committed to a public repository in the Materials Data Facility.

36 MATERIALS SCIENCE↗

Ice Surface Morphology and Flow on Malaspina Glacier, Alaska: Implications for Regional Tectonics in the Saint Elias Orogen

The Saint Elias Mountains in southern Alaska are located at a structural syntaxis where the coastal thrust and fold belt of the Fairweather plate boundary intersects thrust faults and folds generated by collision of the Yakutat Terrane. The axial trace of this syntaxis extends southeastward out of the Saint Elias Mountains and beneath Malaspina Glacier where it is hidden from view and cannot be mapped using conventional methods. Here we examine the surface morphology and flow patterns of Malaspina Glacier to infer characteristics of the bedrock topography and organization of the syntaxis. Faults and folds beneath the eastern part of the glacier trend northwest and reflect dextral transpression near the terminus of the Fairweather fault system. Those beneath the western part of the glacier trend northeast and accommodate folding and thrust faulting during collision and accretion of the Yakutat Terrane. Mapping the location and geometry of the structural syntaxis provides important constraints on spatial variations in seismicity, fault kinematics, and crustal shortening beneath Malaspina Glacier, as well as the position of the collisional deformation front within the Yakutat Terrane. We also speculate that the geometrical complexity of intersecting faults within the syntaxis formed a barrier to rupture propagation during two regional Mw 8.1earthquakes in September 1899.

ice velocities↗

Analysis of the Surface Morphology and Chemical Composition of Zr-Nb3Sn Alloys with Different Zr Concentrations

In the field of superconducting science, Nb has been the material of choice for Radio Frequency (RF) Cavities for years. However, in recent years Nb3Sn has shown to be a promising alternative to Nb. Its combination of a significantly high superconducting transition temperature and a much higher value of upper critical magnetic field (Hc2), has been the reason the alloy has been so widely studied. This project aims to develop materials to further improve the high magnetic field performance of Nb3Sn by improving its upper critical magnetic field and critical current density (Jc). One way to improve the Jc and the Hc2 is to create more grain boundaries in the Nb3Sn alloy allowing them to trap more magnetic flux lines in the materials. To do this the grains must be made smaller which will naturally cause the formation of more grain boundaries. A common way to create smaller grains is by doping an impurity in the alloy. In this study, Nb3Sn was doped with Zr to form Zr-Nb3Sn alloys. This project investigates the surface properties and chemical composition of Zr-Nb3Sn alloys with varying zirconium concentrations (~0.5% and ~24% Zr). Using Scanning Electron Microscopy (SEM), Energy Dispersive Spectroscopy (EDS), and X-ray Photoemission Spectroscopy (XPS), allowed for the characterization of the differences in surface morphology and elemental composition between samples. SEM images were quantified using ImageJ giving insight into grain distribution. The results indicate that increased Zr concentration creates smaller grains in the Zr-Nb3Sn alloy. Furthermore, the ~ 24% Zr grew nanoscale particles on the surface that are possible oxides. XPS data revealed that as Zr concentration increased, the total Nb oxides (NbOx) thickness decreased. Conversely, as Zr concentration increased, the surface Sn oxides (SnOx) also increased slightly. Quantification via ImageJ of SEM data showed that the ~ 0.5% Zr sample had a grain size of ~ 5300 nm2. These results show that Zr inclusion leads to smaller grain formations, which is promising in the world of superconducting RF cavities for high magnetic field applications.

Sue, Micah↗

Impact of Controlled Storage Conditions on the Hydrolysis and Surface Morphology of Amorphous-UO 3

The hydration and morphological effects of amorphous (A)-UO 3 following storage under varying temperature and relative humidity have been investigated. This study provides valuable insight into U-oxide speciation following aging, the U-oxide quantitative morphological data set, and, overall, the characterization of nuclear material provenance. A-UO 3 was synthesized via the washed uranyl peroxide synthetic route and aged based on a 3-factor circumscribed central composite design of experiment. Target aging times include 2.57, 7.00, 14.0, 21.0, and 25.4 days, temperatures of 5.51, 15.0, 30.0, 45.0, and 54.5 °C, and relative humidities of 14.2, 30.0, 55.0, 80.0, and 95.8% were examined. Following aging, crystallographic changes were quantified via powder X-ray diffraction and an internal standard Rietveld refinement method was used to confirm the hydration of A-UO 3 to crystalline schoepite phases. The particle morphology from scanning electron microscopy images was quantified using both the Morphological Analysis of MAterials software and machine learning. Results from the machine learning were processed via agglomerative hierarchical clustering analysis to distinguish trends in morphological attributes from the aging study. Significantly hydrated samples were found to have a much larger, plate-like morphology in comparison to the unaged controls. Predictive modeling via a response surface methodology determined that while aging time, temperature, and relative humidity all have a quantifiable effect on A-UO 3 crystallographic and morphological changes, relative humidity has the most significant impact.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Surface morphology and chemistry of rusty particle 60002,108

Scanning electron microscope, energy dispersive X-ray, and microprobe analyses of the surface of rusty colored particle 60002,108 from deep core 60002 reveal the particle to be basically metallic Ni-Fe that probably grew in contact with silicate minerals, principally plagioclase and pyroxene, and was later partially oxidized and hydrated. A yellowish wrinkled and 'shatter cone' like granular material that is either iron oxide or oxyhydrate may have formed while the particle was in the lunar environment. Ruby-red mounds of lawrencite formed, and the reaction of lawrencite, metallic Ni-Fe, and water vapor resulted in aprons of iron oxyhydrate that surrounds these mounds and flows out over the preexisting yellowish granular substrate. The observations do not allow one to distinguish unequivocally between the initiation of hydration of the ruby-red lawrencite mounds in the lunar environment followed by reaction in the terrestrial and/or spacecraft environment or only reaction in the terrestrial and/or spacecraft environment. The relationship of the lawrencite-rich mounds to the yellowish granular substrate favors the first possibility.

Carter, J. L.↗

Effect of Diel Cycling Temperature, Relative Humidity, and Synthetic Route on the Surface Morphology and Hydrolysis of α -U 3 O 8

The speciation and morphological changes of α-U 3 O 8 following aging under diel cycling temperature and relative humidity (RH) have been examined. This work advances the knowledge of U-oxide hydration as a result of synthetic route and environmental conditions, ultimately giving novel insight into nuclear material provenance. α-U 3 O 8 was synthesized via the washed uranyl peroxide (UO 4 ) and ammonium uranyl carbonate (AUC) synthetic routes to produce unaged starting materials with different morphologies. α-U 3 O 8 from UO 4 is comprised of subrounded particles, while α-U 3 O 8 from AUC contains blocky, porous particles approximately an order of magnitude larger than particles from UO 4 . For aging, a humidity chamber was programmed for continuous daily cycles of 12 “high” hours of 45 °C and 90% RH, and 12 “low” hours of 25 °C and 20% RH. Samples were analyzed at varying intervals of 14, 24, 36, 43, and 54 days. At each aging interval, crystallographic changes were measured via powder X-ray diffraction coupled with whole pattern fitting for quantitative analysis. Morphologic effects were studied via scanning electron microscopy and 12-way classification via machine learning. While all samples were found to have distinguishing morphologic characteristics (93.2% classification accuracy), α-U 3 O 8 from UO 4 had more apparent change with increasing aging time. Nonetheless, α-U 3 O 8 from AUC was found to hydrate more quickly than α-U 3 O 8 from UO 4 , which can likely be attributed to its larger surface area and porous starting material morphology.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Effect of Gold Catalyst Surface Morphology on Wetting Behavior and Electrochemical CO 2 Reduction Performance in a Large-Area Zero-Gap Gas Diffusion Electrolyzer

We report catalyst surface area and wetting behavior are key factors in determining the performance of gas diffusion electrode (GDE) electrolyzers for electrochemical CO 2 reduction. In this work, we report the integration of sub-1 μm thick nanoporous gold (npAu) catalyst coatings into a large-area (25 cm 2 ) zero-gap electrolyzer. The npAu coatings were prepared by magnetron sputtering (MS) of thin AgAu alloy films on the microporous carbon layer of a gas diffusion layer (GDL) followed by Ag leaching. Compared to MS Au films of the same thickness, npAu catalyst coatings enable higher Faradaic efficiencies and improved catalyst stability for CO 2 -to-CO reduction with Faradaic efficiencies of up to 88% at 100 mA/cm 2 . For a 800 nm npAu coating, the device level energy efficiency for CO 2 to CO conversion reaches 45% (52% for CO + H 2 ) at 100 mA/cm 2 with a single pass CO 2 conversion efficiency of ~12%. Contact angle measurements reveal that npAu coatings provide a more hydrophobic electrode interface compared to MS Au coatings, suggesting that the more hydrophobic interfacial environment of npAu coatings helps mitigating electrode flooding which is associated with performance deterioration over time.

30 DIRECT ENERGY CONVERSION↗