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At least 523 records · Page 29

Wetting and Brazing of Chromium Film-Deposited Alumina Using AgCu Filler Metal

Wetting behavior of AgCu filler on chromium film-deposited Al{sub 2}O{sub 3} ceramics was studied by sessile drop method under vacuum, and brazing of chromium-deposited alumina using AgCu was carried out. Cr film can improve the wettability of AgCu filler on alumina ceramics, and the contact angle decreased dramatically. However, with further increase in temperature and extension of wetting time, Cr atom might diffuse excessively to molten alloy or substrate leading to thinned or disappeared Cr film on alumina; thus, the contact angle of AgCu on alumina increased. The reliable alumina joint was obtained via chromium deposition using AgCu filler brazed at 900 °C for 10 min, and no hard or brittle intermetallic compounds formed in the brazed joint. The maximum shear strength of 16.8 MPa was achieved when the thickness of deposited chromium film was 2 μm.

36 MATERIALS SCIENCE↗

Machine-to-machine variability of roughness and corrosion in additively manufactured 316L stainless steel

Numerous studies on the corrosion response of metal AM have been conducted. Nonetheless, the specimens being tested are commonly ground or polished to remove the outer as-built surface. If metal AM is truly going to be employed as a transformative technology that can produce complex shapes that do not require traditional machining, then the material needs to be evaluated in the as-built state. The reality is that AM alloys have shown significant inconsistencies regarding as-built surface texture, topology, and residual stress. One metric that has shown significant unpredictability in the literature is the susceptibility to localized corrosion of typically passive alloys, such as stainless steel (SS). There are a large number of studies that have attempted to understand the corrosion response of metal AM materials, but these studies are typically performed on materials that have been printed on a single machine and often mechanically polished to a smooth finish. This study compares the corrosion response of as-built AM, laser-beam powder bed fusion (LB-PBF), 316L SS parts that have been fabricated on five different machines. The majority of this work focused on understanding the susceptibility to localized corrosion of AM metals with respect to machine-dependent variables, namely surface roughness, and build angle. Surface roughness data was collected using scanning white light triangulation, laser scanning confocal microscopy, and coherence scanning interferometry. The results show that there is significant variability (p two-tail < 0.05) in the susceptibility to local corrosion initiation of LB-PBF 316L SS samples built on different machines. Surface oxides were probed with electron dispersive spectroscopy and revealed that variations in local corrosion susceptibility likely arise from differences in the stability of the passive film caused by chemical segregation, unique microstructure, and tortuous roughness features at the as-built surfaces. The variability of roughness and corrosion properties from test samples printed on different machines was corroborated by property measurements performed at five different testing sites, proving reproducibility of the data. Most importantly, this study shows that if the as-built surface layer is removed through grinding or electropolishing the machine-to-machine variation observed in the corrosion susceptibility is reduced.

36 MATERIALS SCIENCE↗

A single-composition CaSi{sub 2}O{sub 2}N{sub 2}:RE (RE=Ce{sup 3+}/Tb{sup 3+}, Eu{sup 2+}, Mn{sup 2+}) phosphor nanofiber mat: Energy transfer, luminescence and tunable color properties

CaSi{sub 2}O{sub 2}N{sub 2}:RE (RE = Ce{sup 3+}/Tb{sup 3+}, Eu{sup 2+}, Mn{sup 2+}) phosphor nanofiber mat has been prepared via the electrospinning process and further annealing treatment. The diameter of nanofiber precursors are generally in a range of 400–600 nm, which exhibits smooth and uniform surface morphology. After removing the polymer template by high temperature treatment, the fabricated mats have been transformed into a phosphor film and maintain uniform nanofiber network microstructures. Photoluminescence (PL) properties of CaSi{sub 2}O{sub 2}N{sub 2} phosphor nanofiber mat have been activated by Ce{sup 3+}/Tb{sup 3+}, Eu{sup 2+} and Mn{sup 2+}. The emission color of CaSi{sub 2}O{sub 2}N{sub 2}:Ce{sup 3+}/Tb{sup 3+}, Eu{sup 2+}, Mn{sup 2+} phosphor mats can be adjusted by modifying the concentration of doped Tb{sup 3+}/Mn{sup 2+}/Eu{sup 2+} and the resultant energy transfer process. Owing to the energy transfer of Ce{sup 3+}-Tb{sup 3+}, the emitting color of the phosphor mat can be changed from blue to green. Meanwhile, we still found that the switching of emitting colors from blue to red and blue to yellow can be achieved via the energy transfer of Ce{sup 3+}-Mn{sup 2+} and Ce{sup 3+}-Eu{sup 2+}, respectively. We demonstrated a white light emission phosphor nanofiber mat by using CaSi{sub 2}O{sub 2}N{sub 2} system, which exhibited promising applications for near-UV WLEDs. - Graphical abstract: CIE chromaticity coordinates of CaSi{sub 2}O{sub 2}N{sub 2}:Ce{sup 3+}/Tb{sup 3+}, Eu{sup 2+}, Mn{sup 2+} samples. The lighting optical images with a drive current of 100 mA: three LEDs with nanofiber mats of CaSi{sub 2}O{sub 2}N{sub 2}: 0.02Ce{sup 3+}, 0.03Tb{sup 3+}(b), CaSi{sub 2}O{sub 2}N{sub 2}: 0.02Ce{sup 3+}, 0.01Eu{sup 2+}(c) and CaSi{sub 2}O{sub 2}N{sub 2}: 0.02Ce{sup 3+}, 0.12Mn{sup 2+}(d). Display Omitted.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Sequential Doping of Ladder-Type Conjugated Polymers for Thermally Stable n-Type Organic Conductors

Doping of organic semiconductors is a powerful tool to optimize the performance of various organic (opto)electronic and bioelectronic devices. Despite recent advances, the low thermal stability of the electronic properties of doped polymers still represents a significant obstacle to implementing these materials into practical applications. Hence, the development of conducting doped polymers with excellent long-term stability at elevated temperatures is highly desirable. Here, we report on the sequential doping of the ladder-type polymer poly(benzimidazobenzophenanthroline) (BBL) with a benzimidazole-based dopant (i.e., N-DMBI). By combining electrical, UV–vis/infrared, X-ray diffraction, and electron paramagnetic resonance measurements, we quantitatively characterized the conductivity, Seebeck coefficient, spin density, and microstructure of the sequentially doped polymer films as a function of the thermal annealing temperature. Importantly, we observed that the electrical conductivity of N-DMBI-doped BBL remains unchanged even after 20 h of heating at 190 °C. This finding is remarkable and of particular interest for organic thermoelectrics.

36 MATERIALS SCIENCE↗

Near band edge emission characteristics of sputtered nano-crystalline ZnO films

Sputtered zinc oxide (ZnO) thin films deposited on unheated glass substrate under different sputtering gas mixtures (Ar+O{sub 2}) have been investigated using X-ray diffraction and photo luminescence spectroscopy. Earlier reported studies on ZnO films prepared by different techniques exhibit either a sharp/broad near band edge (NBE) emission peak depending on the crystalline quality of the film. In the present study zinc oxide films, grown on unheated substrates, are seen to possess a preferred (002) orientation with a microstructure consisting of clustered nano-sized crystallites. The splitting in the near band edge emission (NBE) into three characteristic peaks is attributed to quantum confinement effect, and is observed specifically under an excitation of 270 nm. Deep level emission (DLE) in the range 400 to 700 nm is not observed indicating absence of deep level radiative defects.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Spatially correlated incommensurate lattice modulations in an atomically thin high-temperature Bi 2.1 Sr 1.9 CaCu 2.0 O 8+y superconductor

Strong variations in superconducting critical temperatures in different families of the cuprate perovskites, even with similar hole doping in their copper-oxygen planes, suggest the importance of lattice modulation effects. The one-dimensional incommensurate lattice modulation (ILM) of Bi 2 Sr 2 CaCu 2 O 8+y , with the average atomic positions perturbed beyond the unit cell6, offer s an ideal test ground for studying the interplay between superconductivity and the long-range incommensurate lattice fluctuations. Here we report Scanning nano X-ray Diffraction (SnXRD) imaging of incommensurate lattice modulations in Bi 2 Sr 2 CaCu 2 O 8+y Van der Waals heterostructures of thicknesses down to two-unit cells. Using SnXRD, we probe that the long-range and short-range incommensurate lattice modulations in bulk sample surface with spatial resolution below 100 nm. We find that puddle-like domains of ILM of size uniformly evolving with dimensionality. In the 2-unit cell thin sample, it is observed that the wavevectors of the long- and short-range orders become anticorrelated with emerging spatial patterns having a directional gradient. The emerging patterns, originated by tiny tuning of lattice strain, induce static mesoscopic charge density waves. Finally, our findings thus demonstrate that the strain can be used to tune and control the electromagnetic properties of two-dimensional high-temperature superconductors.

36 MATERIALS SCIENCE↗

Evaluation of sucrose crystallization kinetics using confocal microscopy: Determining differences in sucrose crystallization kinetics between single and polycrystal studies

Sucrose solution crystal growth kinetics are dependent on temperature, concentration, and impurities. A double polarized confocal microscopy system was used to obtain photographs with high contrast between growing crystals and the background for color background removal image processing. Seeded solutions of 72 wt% sucrose at 27, 35, 45, and 55°C were compared for single and polycrystals. Polycrystal analysis was determined to offer more rapid image processing and to be more applicable to systems in real operating conditions, while single-crystal analysis was determined to give more comprehensive descriptions of individual crystal behavior at the cost of slower processing.

36 MATERIALS SCIENCE↗

Deep Etching Process Developed for the Fabrication of Silicon Carbide Microsystems

Silicon carbide (SiC), because of its superior electrical and mechanical properties at elevated temperatures, is a nearly ideal material for the microminiature sensors and actuators that are used in harsh environments where temperatures may reach 600 C or greater. Deep etching using plasma methods is one of the key processes used to fabricate silicon microsystems for more benign environments, but SiC has proven to be a more difficult material to etch, and etch depths in SiC have been limited to several micrometers. Recently, the Sensors and Electronics Technology Branch at the NASA Glenn Research Center at Lewis Field developed a plasma etching process that was shown to be capable of etching SiC to a depth of 60 mm. Deep etching of SiC is achieved by inductive coupling of radiofrequency electrical energy to a sulfur hexafluoride (SF6) plasma to direct a high flux of energetic ions and reactive fluorine atoms to the SiC surface. The plasma etch is performed at a low pressure, 5 mtorr, which together with a high gas throughput, provides for rapid removal of the gaseous etch products. The lateral topology of the SiC microstructure is defined by a thin film of etch-resistant material, such as indium-tin-oxide, which is patterned using conventional photolithographic processes. Ions from the plasma bombard the exposed SiC surfaces and supply the energy needed to initiate a reaction between SiC and atomic fluorine. In the absence of ion bombardment, no reaction occurs, so surfaces perpendicular to the wafer surface (the etch sidewalls) are etched slowly, yielding the desired vertical sidewalls.

Beheim, Glenn M.↗

Fuel cell nanocatalyst with voltage reversal tolerance

In some embodiments, the present disclosure provides a fuel cell catalyst having a catalyst surface bearing a non-occluding layer of iridium. In some embodiments, the present disclosure provides a fuel cell catalyst comprising a catalyst surface bearing a sub-monolayer of iridium. In some embodiments, the present disclosure provides a fuel cell catalyst comprising a catalyst surface bearing a layer of iridium having a planar equivalent thickness of between 1 and 100 Angstroms. In some embodiments, the fuel cell catalyst comprises nanostructured elements comprising microstructured support whiskers bearing a thin film of nanoscopic catalyst particles. The layer of iridium typically has a planar equivalent thickness of between 1 and 100 Angstroms and more typically between 5 and 60 Angstroms. The fuel cell catalyst typically comprises no electrically conductive carbon material and typically comprises at least a portion of the iridium in the zero oxidation state.

30 DIRECT ENERGY CONVERSION↗

Mechanisms of Asymmetric Membrane Formation in Nonsolvent-Induced Phase Separation

We report the first simulations of nonsolvent-induced phase separation (NIPS) that predict membrane microstructures with graded asymmetric pore size distribution. In NIPS, a polymer solution film is immersed in a nonsolvent bath, enriching the film in nonsolvent, and leading to phase separation that forms a solid polymer-rich membrane matrix and polymer-poor membrane pores. We demonstrate how mass-transfer-induced spinodal decomposition, thermal fluctuations, and glass-transition dynamics implemented with mobility contrast between the polymer-rich and polymer-poor phases are essential to the formation of asymmetric membrane microstructures. Specifically, we show that the competition between the propagation of the phase-separation and glass-transition fronts determines the degree of pore-size asymmetry. In conclusion, we also explore the sensitivity of these microstructures to the initial film composition, and compare their formation in 2D and 3D.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Spherulite-enhanced macroscopic polarization in molecular ferroelectric films from vacuum deposition

Proton-transfer type molecular ferroelectrics hold significant promise for practical application due to their large spontaneous polarizations, high Curie temperatures, and small switching fields. However, it remains puzzling that preparation of quasi-2D films exhibiting macroscopic ferroelectric behaviors has been reported in only few molecular ferroelectrics. To address this puzzle, we studied the impact of microstructures on the macroscopic ferroelectric properties of 5,6-dichloro-2-methylbenzimidazole (DC-MBI) films grown using the low-temperature deposition followed by the restrained crystallization (LDRC) method. Our findings revealed a competition between dense spherulites and porous microstructures containing randomly oriented nanograins in the as-grown films. Post-growth annealing at moderate temperature promotes the formation of spherulites, leading to macroscopic ferroelectric polarization switching. These results underscore the critical role of microstructure density in determining macroscopic ferroelectric properties, potentially resolving the puzzle for the absence of such behavior in many molecular ferroelectric films. Here, we anticipate that the approach proposed in this study to enhance microstructure density will significantly advance the fabrication of quasi-2D molecular ferroelectric films and unlock their potential in device applications.

36 MATERIALS SCIENCE↗

Sample Preparation and Experimental Design for In Situ Multi-Beam Transmission Electron Microscopy Irradiation Experiments

We discuss the need to understand materials exposed to overlapping extreme environments such as high temperature, radiation, or mechanical stress. When these stressors are combined there may be synergistic effects that enable unique microstructural evolution mechanisms to activate. Understanding of these mechanisms is necessary for the input and refinement of predictive models and critical for engineering of next generation materials. The basic physics and underlying mechanisms require advanced tools to be investigated. The in situ ion irradiation transmission electron microscope (I 3 TEM) is designed to explore these principles. To quantitatively probe the complex dynamic interactions in materials, careful preparation of samples and consideration of experimental design is required. Particular handling or preparation of samples can easily introduce damage or features that obfuscate the measurements. There is no one correct way to prepare a sample; however, many mistakes can be made. The most common errors and things to consider are highlighted within. The I 3 TEM has many adjustable variables and a large potential experimental space, therefore it is best to design experiments with a specific scientific question or questions in mind. Experiments have been performed on large number of sample geometries, material classes, and with many irradiation conditions. The following are a subset of examples that demonstrate unique in situ capabilities utilizing the I 3 TEM. Au nanoparticles prepared by drop casting have been used to investigate the effects of single ion strikes. Au thin films have been used in studies on the effects of multibeam irradiation on microstructure evolution. Zr films have been exposed to irradiation and mechanical tension to examine creep. Ag nanopillars were subjected to simultaneous high temperature, mechanical compression, and ion irradiation to study irradiation induced creep as well. These results impact fields including: structural materials, nuclear energy, energy storage, catalysis, and microelectronics in space environments.

47 OTHER INSTRUMENTATION↗

Refractive Imaging of Air Shock Above Microscale Defects in Pentaerythritol Tetranitrate (PETN) Films

Physical vapor deposition (PVD) of high explosives can produce energetic samples with unique microstructure and morphology compared to traditional powder processing techniques, but challenges may exist in fabricating explosive films without defects. Deposition conditions and substrate material may promote microcracking and other defects in the explosive films. Here, we investigate effects of engineered microscale defects (gaps) on detonation propagation and failure for pentaerythritol tetranitrate (PETN) films using ultra-high-speed refractive imaging and hydrocode modelling. Observations of the air shock above the gap reveal significant instabilities during gap crossing and re-ignition.

36 MATERIALS SCIENCE↗

Anomalous Hall Effect in Epitaxial Ni–Mn–Ga Thin Films Grown on MgO(001) Substrate during the Martensitic Transformation

Epitaxial Ni–Mn–Ga thin films had been grown on MgO (001) by DC magnetron sputtering. And the anomalous Hall effect (AHE), microstructures, magnetism, and magnetoresistance (MR) were investigated. The AHE was measured in the film of Ni{sub 47.8}Mn{sub 30.8}Ga{sub 21.4} during the martensitic transformation. Meanwhile, the mechanism of the AHE was explained which indicates that the hall resistivity measured in our sample is primarily determined by AHE. The microstructures of the austenite phase and 7M martensite plates at room temperature had been observed on the film of Ni{sub 46.7}Mn{sub 31.7}Ga{sub 21.6} and Ni{sub 47.8}Mn{sub 30.8}Ga{sub 21.4}, respectively. Magnetic measurements reveal that all films possessed the martensitic transformation during the heating and cooling processes. In addition, the MR showed a negative value during the martensitic transformation which is mainly due to the reduction of spin-dependent scattering.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗