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At least 577 records · Page 32

Dry etching of epitaxial InGaAs/InAlAs/InAlGaAs structures for fabrication of photonic integrated circuits

A dry etching process to transfer the pattern of a photonic integrated circuit design for high-speed laser communications is described. The laser stack under consideration is a 3.2-µm-thick InGaAs/InAlAs/InAlGaAs epitaxial structure grown by molecular beam epitaxy. The etching was performed using Cl2-based inductively-coupled-plasma and reactive-ion-etching (ICP-RIE) reactors. Four different recipes are presented in two similar ICP-RIE reactors, with special attention paid to the etched features formed with various hard mask compositions, in-situ passivations, and process temperatures. The results indicate that it is possible to produce high-aspect-ratio features with sub-micron separation on this multilayer structure. Additionally, the results of the etching highlight the tradeoffs involved with the corresponding recipes.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Surface conversion techniques for low energy neutral atom imagers

This investigation has focused on development of key technology elements for low energy neutral atom imaging. More specifically, we have investigated the conversion of low energy neutral atoms to negatively charged ions upon reflection from specially prepared surfaces. This 'surface conversion' technique appears to offer a unique capability of detecting, and thus imaging, neutral atoms at energies of 0.01 - 1 keV with high enough efficiencies to make practical its application to low energy neutral atom imaging in space. Such imaging offers the opportunity to obtain the first instantaneous global maps of macroscopic plasma features and their temporal variation. Through previous in situ plasma measurements, we have a statistical picture of large scale morphology and local measurements of dynamic processes. However, with in situ techniques it is impossible to characterize or understand many of the global plasma transport and energization processes. A series of global plasma images would greatly advance our understanding of these processes and would provide the context for interpreting previous and future in situ measurements. Fast neutral atoms, created from ions that are neutralized in collisions with exospheric neutrals, offer the means for remotely imaging plasma populations. Energy and mass analysis of these neutrals provides critical information about the source plasma distribution. The flux of neutral atoms available for imaging depends upon a convolution of the ambient plasma distribution with the charge exchange cross section for the background neutral population. Some of the highest signals are at relatively low energies (well below 1 keV). This energy range also includes some of the most important plasma populations to be imaged, for example the base of the cleft ion fountain.

Quinn, J. M.↗

In-Situ Alloying of GRCop-42 via Additive Manufacturing: Precipitate Analysis

GRCop-42, a Cu-4at% Cr-2at% Nb alloy, was designed as a high temperature, high strength, high heat flux material for rocket engine combustion chamber liners by NASA Glenn Research Center. In situ alloying of GRCop-42 (ISGRCop-42) using powder bed fusion (PBF) additive manufacturing (AM) takes elemental powders of Cu, Cr, and Nb to be introduced into the PBF environment and develop the GRCop alloy while simultaneously building an AM component. Elemental powders were milled together prior to printing in an effort to facilitate the alloying process. Success of the in situ alloying process may provide lower cost, faster lead times, alloying optimization, and more design freedom in the development of regeneratively-cooled rocket propulsion systems. Evaluation of the ISGRCop-42 was conducted using a phase extraction procedure to isolate the Cr2Nb precipitates from the pure Cu matrix. The isolated precipitates were then examined using x-ray powder diffraction (XRD), scanning electron microscopy (SEM), and energy dispersion spectroscopy (EDS). It was found that ISGRCop-42 successfully and repeatedly formed Cr2Nb at a yield as high as 89% of potential Cr2Nb. Further, it was identified that the preparation of the powder was the most influential factor in alloying success, and the second most influential factor was the laser power.

In Situ alloying↗

Planning for the semiconductor manufacturer of the future

Texas Instruments (TI) is currently contracted by the Air Force Wright Laboratory and the Defense Advanced Research Projects Agency (DARPA) to develop the next generation flexible semiconductor wafer fabrication system called Microelectronics Manufacturing Science & Technology (MMST). Several revolutionary concepts are being pioneered on MMST, including the following: new single-wafer rapid thermal processes, in-situ sensors, cluster equipment, and advanced Computer Integrated Manufacturing (CIM) software. The objective of the project is to develop a manufacturing system capable of achieving an order of magnitude improvement in almost all aspects of wafer fabrication. TI was awarded the contract in Oct., 1988, and will complete development with a fabrication facility demonstration in April, 1993. An important part of MMST is development of the CIM environment responsible for coordinating all parts of the system. The CIM architecture being developed is based on a distributed object oriented framework made of several cooperating subsystems. The software subsystems include the following: process control for dynamic control of factory processes; modular processing system for controlling the processing equipment; generic equipment model which provides an interface between processing equipment and the rest of the factory; specification system which maintains factory documents and product specifications; simulator for modelling the factory for analysis purposes; scheduler for scheduling work on the factory floor; and the planner for planning and monitoring of orders within the factory. This paper first outlines the division of responsibility between the planner, scheduler, and simulator subsystems. It then describes the approach to incremental planning and the way in which uncertainty is modelled within the plan representation. Finally, current status and initial results are described.

Fargher, Hugh E.↗

Development and Processing of Nickel Aluminide-Carbide Alloys

With the upper temperature limit of the Ni-based superalloys attained, a new class of materials is required. Intermetallics appear as likely candidates because of their attractive physical properties. With a relatively low density, high thermal conductivity, excellent oxidation resistance, high melting point, and simple crystal structure, nickel aluminide (NiAl) appears to be a potential candidate. However, NiAl is limited in structural applications due to its low room temperature fracture toughness and poor elevated temperature strength. One approach to improving these properties has been through the application of eutectic composites. Researchers have shown that containerless directional solidification of NiAl-based eutectic alloys can provide improvement in both the creep strength and fracture toughness. Although these systems have shown improvements in the mechanical properties, the presence of refractory metals increases the density significantly in some alloys. Lower density systems, such as the carbides, nitrides, and borides, may provide NiAl-based eutectic structure. With little or no information available on these systems, experimental investigation is required. The objective of this research was to locate and develop NiAl-carbide eutectic alloys. Exploratory arc-melts were performed in NiAl-refractory metal-C systems. Refractory metal systems investigated included Co, Cr, Fe, Hf, Mo, Nb, Ta, Ti, W, and Zr. Systems containing carbides with excellent stability (i.e.,HfC, NbC, TaC, TiC, and ZrC) produced large blocky cubic carbides in an NiAl matrix. The carbides appeared to have formed in the liquid state and were randomly distributed throughout the polycrystalline NiAl. The Co, Cr, Fe, Mo, and W systems contained NiAl dendrites with a two-phase interdendritic microconstituent present. Of these systems, the NiAl-Mo-C system had the most promising microstructure for in-situ composites. Three processing techniques were used to evaluate the NiAl-Mo-C system: arc-melting, slow cooling, and containerless directional solidification. Arc-melting provided a wide range of compositions in an economical and simple fashion. The slow cooled ingots provided larger ingots and slower cooling rates than arc-melting. Directional solidification was used to produce in-situ composites consisting of NiAl reinforced with molybdenum carbides.

Newport, Timothy Scott↗

Infrared thermography NDT for in-situ defect detection in sandwich composite panel manufacturing

Composite manufacturing presents numerous challenges, as defects can arise from various sources throughout the process. In sandwich composite structures, the integration of a foam core introduces additional complexity and increases the likelihood of defect formation like delamination. To mitigate these issues and reduce the risk of future structural failures, in-situ monitoring during manufacturing is essential. This study investigates infrared (IR) thermography as a non-destructive technique for detecting manufacturing defects in foam-core sandwich composite panels under thermally excited conditions representative of in-situ processing. A stationary FLIR A8590 IR camera (640 × 512 pixels, 30Hz, 17mm lens, 9 ft stand-off distance) was used to monitor prefabricated panels subjected to controlled external heating simulating compression molding and resin cure exotherm. Interlaminar delamination defects with characteristic sizes ranging from 0.25 × 0.25in² to 5 × 5in² produced measurable surface temperature depressions of approximately 4–10°C during transient cooling, exceeding the effective noise floor of the camera by more than two standard deviations. Thicker laminates exhibited prolonged defect detectability windows due to increased thermal diffusion time. In contrast, embedded Teflon inclusions generated weak thermal contrasts of ≤ 3°C, approaching the measurement noise floor, due to limited thermal property contrast with the surrounding glass fiber composite. These results establish quantitative detectability limits for stationary thermographic inspection of sandwich composite panels under manufacturing-representative thermal cycles.

Barakat, Abdallah [ORNL] (ORCID:0000000296141398)↗

Reactive extrusion of frontally polymerizing continuous carbon fiber reinforced polymer composites

The manufacturing of carbon fiber-reinforced polymer (CFRP) composites demands rapid and energy-efficient strategies. Frontal polymerization (FP) enables the manufacturing of CFRP using dicyclopentadiene (DCPD) thermoset polymer which meets these requirements. In this work, we introduce reactive extrusion of CFRP (RE-CFRP), where two rollers provide localized heat and pressure to sustain the curing reaction and the consolidation of a continuous carbon fiber tow pre-impregnated with DCPD. We study the effect of the extrusion speed, temperature, and compaction force on the properties of the produced CFRP. Mechanical testing confirms that the resulting fiber volume fraction and the elastic modulus are similar to bulk cured tows. A homogenized thermo-chemical model is developed to study the effect of the process parameters on the polymerization reaction. The process produces hollow woven composite tubes directly via extrusion and in situ curing. Overall, this process offers advantages in curing, tooling, speed, and energy.

36 MATERIALS SCIENCE↗

Real-time laser ultrasonic monitoring of laser-induced thermal processes

Abstract Intra- and inter-layer integrity of components fabricated with advanced manufacturing techniques, such as laser powder bed fusion, is dependent upon rapid heating, melting, and solidification processes. There is a need for new techniques to provide in situ feedback of these processes. Here a laser-based ultrasonic technique to probe thermal effects induced by a high-power continuous wave laser in titanium samples is described. Numerical simulations were performed to show that, for a spatially uniform heating beam, laser-induced surface acoustic waves are strongly influenced by surface heating conditions, are dispersive in the case of rapid heating, and that an abrupt velocity reduction happens upon the onset of surface melting. Furthermore, laser-based ultrasound experimental results which monitor the transient change of surface wave travel time associated with high power laser surface heating are provided. A pulsed laser is used to generate high frequency surface acoustic waves that propagate through the laser-heated region and are detected using a photorefractive crystal-based interferometer. Qualitative agreement is observed between theory and experiment with both showing a rapid reduction in the surface wave velocity at the onset of illumination and further decrease in surface wave velocity associated with melting. It is demonstrated that changes in the surface wave velocity can be used to track local heating and detect the onset of surface melting in real time.

36 MATERIALS SCIENCE↗

KSC Intern Narrative Report

There are limited resources on extraterrestrial bodies and current launch vehicles can only send finite resources on deep space missions. Transporting resources needed for deep space missions is extremely expensive; at tens of thousands of dollars per pound launched. In order to sustain life and establish outposts on other celestial bodies, it is necessary to find a way to utilize the resources that are readily available in these environments. This process is called In Situ Resource Utilization (ISRU), which is comprised of searching for, collecting, processing, and storing materials found on other celestial bodies and using them for construction, science applications, propulsion, and other life sustaining purposes. The processing and use of regolith, which is a loose rocky material found on the surface of bodies like the Moon or Mars, is the main focus of ISRU work done in Swamp Works in the Engineering Development Lab at Kennedy Space Center (KSC). The research Swamp Works has done in regolith applications ranges from construction and infrastructure to propellant production to storage of oxygen and water.

George, Amber↗

Conceptual process design and techno-economic assessment of ex situ catalytic fast pyrolysis of biomass: A fixed bed reactor implementation scenario for future feasibility

Ex situ catalytic fast pyrolysis of biomass is a promising route for the production of fungible liquid biofuels. There is significant ongoing research on the design and development of catalysts for this process. However, there are a limited number of studies investigating process configurations and their effects on biorefinery economics. Herein we present a conceptual process design with techno-economic assessment; it includes the production of upgraded bio-oil via fixed bed ex situ catalytic fast pyrolysis followed by final hydroprocessing to hydrocarbon fuel blendstocks. This study builds upon previous work using fluidized bed systems, as detailed in a recent design report led by the National Renewable Energy Laboratory (NREL/TP-5100-62455); overall yields are assumed to be similar, and are based on enabling future feasibility. Assuming similar yields provides a basis for easy comparison and for studying the impacts of areas of focus in this study, namely, fixed bed reactor configurations and their catalyst development requirements, and the impacts of an inline hot gas filter. A comparison with the fluidized bed system shows that there is potential for higher capital costs and lower catalyst costs in the fixed bed system, leading to comparable overall costs. The key catalyst requirement is to enable the effective transformation of highly oxygenated biomass into hydrocarbons products with properties suitable for blending into current fuels. Potential catalyst materials are discussed, along with their suitability for deoxygenation, hydrogenation and C–C coupling chemistry. This chemistry is necessary during pyrolysis vapor upgrading for improved bio-oil quality, which enables efficient downstream hydroprocessing; C–C coupling helps increase the proportion of diesel/jet fuel range product. One potential benefit of fixed bed upgrading over fluidized bed upgrading is catalyst flexibility, providing greater control over chemistry and product composition. Since this study is based on future projections, the impacts of uncertainties in the underlying assumptions are quantified via sensitivity analysis. As a result, this analysis indicates that catalyst researchers should prioritize by: carbon efficiency > catalyst cost > catalyst lifetime, after initially testing for basic operational feasibility.

09 BIOMASS FUELS↗

What Can Plastic Flow Fields Tell Us About Heat Sources in Deformation Processing?

We characterize primary (shape-change) and secondary (friction) deformation, and associated temperature fields, in metal cutting and forming processes, using in situ imaging and simulation. The experimental configurations enable access to the deformation zones and die contact-interfaces, for measuring deformation, temperature, and frictional drag. Infra-red thermography reveals that the plastic strain-rate field is an excellent proxy for the deformation-induced heat sources. Both spatially confined and diffuse strain-rate fields occur, depending on the initial workpiece deformation state. When the strain rate is confined, as in pre-hardened material, the temperature modeling is much simplified, as the heat source is also now localized. However complex, microstructure-driven deformation modes, like sinuous flow in annealed metals, result in spatially diffuse strain-rate and body heat sources, more challenging to analyze. Furthermore, our unified measurements should be of value for accurately estimating the fraction of plastic dissipation that is converted into heat in large-strain deformation processes.

36 MATERIALS SCIENCE↗

Direct Visualization of Laser-Induced Coalescence and Alloying of Au into Ag Nanowires

Noble metal nanocomposites with controlled morphology and composition have been largely useful in a wide variety of applications like catalysis, plasmonics, and biological applications. Herein, we show pulsed-laser-assisted fabrication of beaded Au-Ag nanowires with a variety of morphologies and compositions via coalescence and alloying of Au nanoparticles (NP) into a Ag nanowire (NW). Direct visualization of the evolution process with in situ laser heating transmission electron microscopy (ILH-TEM) leads to unambiguous insights into the mechanism of formation for the first time. Ag, being a soft material, melts at the surface to bridge the gap between the NP-NW, forming a cup-like morphology underneath the Au NP via capillary action. Progressive laser irradiation leads to wetting of the Au NP with Ag, forming an envelope around the NP. This is associated with the formation of a valley in Ag NW around the NP, which flattens gradually by partial embedding of the NP. Interdiffusion of Au into Ag and vice versa sets in at this stage, leading to the depletion of Au from the Au-rich NP region. Prolonged irradiation leads to gradual intermixing of Au-Ag forming beaded Au-doped Ag nanowires with homogeneous composition. Such a step-by-step understanding of the coalescence and alloying process has implications in nanowelding, which holds the future in designing efficient transparent conductors and printed electronics.

Isik, Tugba↗

A Standardized Analysis Process Using Digital Image Correlation to Calculate In Situ Cladding Strain from Modified Burst Tests for Fuel Performance Code Validation

Historical data collection on nuclear fuel cladding materials has focused on generating a statistically significant amount of data to assess the material and its failure behavior. Furthermore, data generated to support material model and failure criteria development were previously posttest evaluations, so a large number of tests was required to gain new understanding. A way to expedite this process is to develop techniques capable of generating large, high-fidelity data sets from a single test with lower uncertainty or quantified uncertainty. One such example of this approach is Oak Ridge National Laboratory’s use of modified burst tests (MBTs) to analyze the mechanical behavior and failure conditions of cladding during a simulated reactivity-initiated accident (RIA). Each test incorporates digital image correlation (DIC) analysis techniques that are used to assess the accumulated strain in situ, as well as eventual cladding failure. This work has been fruitful in defining strain-to-failure conditions for materials like silicon carbide (SiC) fiber–reinforced/SiC matrix composite tubes (SiC/SiC), iron-chromium-aluminum (FeCrAl) alloy tubes, and chromium-coated Zircaloy-4 tubes. However, there are numerous DIC software available, including open-source and proprietary software. The different DIC software use various algorithms to process images and calculate displacement values. Using these different software and algorithms can lead to varying results, and perhaps larger-than-expected uncertainties. In the present study, previously published MBT data encompassing a variety of test conditions were reanalyzed with two different DIC software to assess the variance in the calculated strain results. The data consisted of SiC/SiC, FeCrAl, and chromium-coated Zircaloy-4 tubes. Plots of the calculated strains during the transient revealed good agreement between the two DIC software. The average root-mean-square errors between the two software was 0.20% strain, which is slightly larger than a previously reported error value for these tests. In conclusion, this variance in results is low enough that this analysis method can be used for code validation.

Reactivity-initiated accident↗

In Situ Liquid Secondary Ion Mass Spectrometry: A Surprisingly Soft Ionization Process for Investigation of Halide Ion Hydration

The understanding of ion solvation phenomenon is of significance due to their influences on many important chemical, biological and environmental processes. Mass spectrometry (MS) based methods have been used to investigate this topic with molecular insights. As ion-solvent interactions are weak, ionization processes should be as soft as possible in order to retain solvation structures. An in situ liquid secondary ion MS (SIMS) approach developed in our group has been recently utilized in investigations of Li ion solvation in non-aqueous solution and detected a series of solvated Li ions. As traditionally SIMS has long been recognized as a hard ionization process with strong damage occurring at the sputtering interface, it is very interesting to study further how soft in situ liquid SIMS can be. In this work, we used halide ion hydration as an example to compare the ionization performance of in situ liquid SIMS approach with regular electrospray ionization MS (ESI-MS). Results show that although ESI has been recognized as a soft ionization method, nearly no solvated halide ions were detected by ESI-MS analysis, which acquired only strong signals of salt ion clusters. In contrast, in liquid SIMS spectra, a series of obvious hydrated halide ion compositions could be observed. We further evaluated the hydration numbers of halide ions and revealed the effects of the ion size, charge density and polarizability on the hydration phenomenon. Our findings demonstrated that the in situ liquid SIMS approach is surprisingly soft, and expected to have very broad applications on investigation of various ion-solvent interactions and many other interesting chemical processes (e.g., the initial nucleation of nanoparticle formation) in liquid environment.

Zhang, Yanyan↗

Superconducting Nd 1- x Eu x NiO 2 thin films using in situ synthesis

We report on superconductivity in Nd 1-x Eu x NiO 2 using Eu as a 4f dopant of the parent NdNiO 2 infinite-layer compound. We use an all–in situ molecular beam epitaxy reduction process to achieve the superconducting phase, providing an alternate method to the ex situ CaH 2 reduction process to induce superconductivity in the infinite-layer nickelates. The Nd 1-x Eu x NiO 2 samples exhibit a step-terrace structure on their surfaces, have a T c onset of 21 K at x = 0.25, and have a large upper critical field that may be related to Eu 4f doping.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Enhancement of transport critical current density of SmFeAsO{sub 1−x}F{sub x} tapes fabricated by an ex-situ powder-in-tube method with a Sn-presintering process

SmFeAsO{sub 1−x}F{sub x} (Sm1111) tapes were prepared by an ex-situ powder-in-tube method with a Sn-presintering process. Scanning electron microscopy revealed apparent difference in microstructure between Sn-presintered tapes and the previously reported polycrystalline Sm1111 bulk, since Sn has reduced FeAs wetting phase and filled the voids between Sm1111 grains. The Sn-presintered tapes showed significant enhanced field dependences of transport J{sub c} compared with Sn-added tapes. A highest transport critical current density (J{sub c}) of 3.45 × 10{sup 4} A cm{sup −2} at 4.2 K and self-field is achieved. Magneto-optical imaging further confirmed large and well-distributed global and intergranular J{sub c} in Sn-presintered Sm1111 tapes.

36 MATERIALS SCIENCE↗

NASICON Na 3 V 2 (PO 4 ) 3 Enables Quasi-Two-Stage Na + and Zn 2+ Intercalation for Multivalent Zinc Batteries

Identifying positive electrode materials capable of reversible multivalent electrochemistry in electrolytes containing divalent ions such as Mg 2+ , Ca 2+ , and Zn 2+ at high operating potentials remains an ongoing challenge in “beyond lithium-ion” research. In this paper, we explore the Zn 2+ charge-storage mechanism of a vanadium-based Na + superionic conductor (NASICON), Na 3 V 2 (PO 4 ) 3 . By using X-ray synchrotron techniques to unravel potential-dependent structure–property relationships, we ascribe the reversible electrochemical behavior of Na 3 V 2 (PO 4 ) 3 to a quasi-two-stage intercalation process that involves both Na+ and Zn 2+ . Initial charging of Na 3 V 2 (PO 4 ) 3 leads to a Na + -extracted phase corresponding to Na 3 V 2 (PO 4 ) 3 , whereas subsequent discharge results predominantly in Na + intercalation followed by Zn 2+ intercalation. Operando X-ray diffraction of Na 3 V 2 (PO 4 ) 3 was used to study the phase changes associated with the first charge/discharge process, and ex situ measurements were used to precisely link the changes in the crystal structure to a quasi-two-stage intercalation of Na + and Zn 2+ . The corresponding changes in the V-oxidation state, V-O coordination, and the presence of Zn 2+ were confirmed by X-ray absorption spectroscopy. The results of this work present a comprehensive understanding of the charge-storage properties for a well-established NASICON structure that confers both the high capacity (~100 mA h g -1 ) and high potential (1.35 and 1.1 V vs Zn/Zn 2+ ).

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Delivery of Vegetable Oil Suspensions in a Shear Thinning Fluid for Enhanced Bioremediation

In situ anaerobic biological processes are widely applied for dechlorination of chlorinated solvents in groundwater. A wide range of organic substrates have been tested and applied to support the dechlorination processes. Vegetable oils are a promising substrate and have been shown to induce effective dechlorination, have limited geochemical impacts, and good longevity. Distribution of vegetable oil in the subsurface, because it is a non-aqueous phase material, has typically been addressed by creating emulsified oil solutions. In this study, inexpensive waste vegetable oils were suspended in a xanthan gum solution, a shear-thinning fluid, as an alternative oil delivery mechanism. The stability, oil droplet size and distribution, and rheological behavior of the oil suspensions that are created in the xanthan solutions were studied in batch experiments. The injectability of the suspensions and oil distribution in porous medium were evaluated in column tests. Numerical modeling of the oil droplet transport and distribution in porous media was conducted to help interpret the column-test data. Batch studies showed that simple mixing of vegetable oil and xanthan solution produced stable suspensions of the oil as micron-size droplets. The mixture rheology retains shear-thinning properties that facilitate improved uniformity of substrate distribution in heterogeneous aquifers. Column tests demonstrated successful injection of the vegetable oil suspension into porous medium. This study provided evidence that vegetable oil suspensions in xanthan are a potential substrate to support in situ anaerobic bioremediation with favorable injection properties.

Zhong, Lirong↗