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At least 1,603 records · Page 89

Influence of Protection Layers on Thermal Stability of Nitride Thin Films

Nitrides are commonly studied for their properties relevant to numerous coating applications, and have been recently used to synthesize newly predicted materials in thin film form. However, thermodynamic stability of such nitride materials is difficult to experimentally evaluate, due to limited thermal budget of thin films. Here we show that thermal stability of nitride films can be extended using protection layers. Specifically, we find that zirconium nitride (ZrN) thin films are stable up to at least 1200°C annealing temperature in N2 atmosphere, if aluminum nitride (AlN) diffusion barriers and capping layers are used. X-ray diffraction (XRD) measurements show the expected thermodynamically stable rocksalt structure of ZrN, and scanning electron microscopy (SEM) confirms compact microstructure of these ZrN films. Without such protection layers, transient bixbyite Zr2ON2 phase and high-temperature ZrSi2 phase are observed after annealing by XRD, SEM, and auger electron spectroscopy (AES), due to side reaction with native surface oxide (ZrOx) and substrate (Si) respectively. These results demonstrate that protection layers are beneficial to increase the thermal budget of nitride thin films, for evaluating thermodynamic stability of new nitride materials, for capturing transient metastable phases during crystallization, and for using functional nitride coatings in extreme environments.

36 MATERIALS SCIENCE↗

FIU Project1: Chemical Process Alternatives for Radioactive Waste [Slides]

"The U.S. DOE Hanford Site has the largest number of high-level waste (HLW) storage tanks and the largest volume of HLW in the United States. The safe storage, retrieval, treatment, and disposal of approximately 53 million gallons of highly toxic, high-level radioactive waste stored in Hanford’s 177 underground tanks are a national priority. Retrieval and treatment of waste from these tanks pose a considerable challenge. Florida International University has been conducting research on several promising alternative processes and technologies that can be applied to address several technology gaps in the current waste retrieval and conditioning plans. Specifically, FIU has been involved in: the evaluation of non-metallic materials in the waste transfer system, evaluation of alternative HLW instrumentation for in-tank applications and the development of technologies to assist in the inspection of tank bottoms at Hanford."

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Development of advanced material composites for use as internal insulation for LH2 tanks (gas layer concept)

A program is described that was conducted to develop an internal insulation system for potential application to the liquid hydrogen tanks of a reusable booster, where the tanks would be subjected to repeated high temperatures. The design of the internal insulation is based on a unique gas layer concept, in which capillary or surface tension effects are used to maintain a stable gas layer, within a cellular core structure, between the tank wall and the contained liquid hydrogen. Specific objectives were to select materials for insulation systems that would be compatible with wall temperatures of 350 F and 650 F during reentry into the earth's atmosphere, and to fabricate and test insulation systems under conditions simulating the operating environment. A materials test program was conducted to evaluate the properties of candidate materials at elevated temperatures and at the temperature of liquid hydrogen, and to determine the compatibility of the materials with a hydrogen atmosphere at the appropriate elevated temperature. The materials that were finally selected included Kapton polyimide films, silicone adhesives, fiber glass batting, and in the case of the 350 F system, Teflon film.

Gille, J. P.↗

Investigation into Spectroscopic Techniques for Thermal Barrier Coating Spall Detection

Spectroscopic methods are proposed for detection of thermal barrier coating (TBC) spallation from engine hot zone components. These methods include absorption and emission of airborne marker species originally embedded in the TBC bond coat. In this study, candidate marker materials for this application were evaluated. Thermochemical analysis of candidate marker materials combined with additional constraints such as toxicity and uniqueness to engine environment, provided a short list of four potential species: platinum, copper oxide, zinc oxide. and indium. The melting point of indium was considered to be too low for serious consideration. The other three candidate marker materials, platinum, copper oxide, and zinc oxide were placed in a high temperature furnace and emission and absorption properties were measured over a temperature range from 800-1400 C and a spectral range from 250 to 18000 nm. Platinum did not provide the desired response, likely due to the low vapor Pressure of the metallic species and the low absorption of the oxide species. It was also found, however. that platinum caused a broadening of the carbon dioxide absorption at 4300 nm. The nature of this effect is not known. Absorption and emission caused by sodium and potassium impurities in the platinum were found in the platinum tests. Zinc oxide did not provide the desired response, again, most likely due to the low vapor pressure of the metallic species and the low absorption of the oxide species. Copper oxide generated two strongly temperature dependent absorption peaks at 324.8 and 327.4 nm. The melting point of copper oxide was determined to be too low for serious consideration as marker material.

deGroot, Wim↗

Guide for Oxygen Compatibility Assessments on Oxygen Components and Systems

A viewgraph presentation evaluating the compatibility of oxygen components and systems is shown. The topics include: 1) Application; 2) Gaining Wide Subscription; 3) Approach; 4) Establish Worst-Case Operating Conditions; 5) Assess Materials Flammability; 6) Evaluate Ignition Mechanisms; 7) Evaluate Kindling Chain; 8) Determine Reaction Affect; 9) Document Results; 10) Example of Documentation; and 11) Oxygen Compatibility Assessment Team.

Rosales, Keisa R.↗

On The Development of Additive Construction Technologies for Application to Development of Lunar/Martian Surface Structures Using In-Situ Materials

For long-duration missions on other planetary bodies, the use of in-situ materials will become increasingly critical. As man's presence on these bodies expands, so must the breadth of the structures required to accommodate them including habitats, laboratories, berms, radiation shielding for natural radiation and surface reactors, garages, solar storm shelters, greenhouses, etc. Planetary surface structure manufacturing and assembly technologies that incorporate in-situ resources provide options for autonomous, affordable, pre-positioned environments with radiation shielding features and protection from micrometeorites, exhaust plume debris, and other hazards. This is important because gamma and particle radiation constitute a serious but reducible threat to long-term survival of human beings, electronics, and other materials in space environments. Also, it is anticipated that surface structures will constitute the primary mass element of lunar or Martian launch requirements. The ability to use in-situ materials to construct these structures will provide a benefit in the reduction of up-mass that would otherwise make long-term Moon or Mars structures cost prohibitive. The ability to fabricate structures in situ brings with it the ability to repair these structures, which allows for self-sufficiency necessary for long-duration habitation. Previously, under the auspices of the MSFC In Situ Fabrication and Repair (ISFR) project and more recently, under the joint MSFC/KSC Additive Construction with Mobile Emplacement (ACME) project, the MSFC Surface Structures Group has been developing materials and construction technologies to support future planetary habitats with in situ resources. One such technology, known as Contour Crafting (additive construction), is shown in Figure 1, along with a typical structure fabricated using this technology. This paper will present the results to date of these efforts, including development of novel nozzle concepts for advanced layer deposition using the Contour Crafting process. This process, conceived initially for rapid development of cementitious structures on Earth, also lends itself exceptionally well to the automated fabrication of planetary surface structures using minimally processed regolith as aggregate, and imported binder material or binders developed from in situ materials. This process has been used successfully in the fabrication of construction elements using lunar regolith simulant and Mars regolith simulant, both with various binder materials. These binder materials have resulted from extensive evaluation and include both "imported" binder materials that might be launched from Earth as well as some binder materials that can theoretically also be derived from existing regolith materials. They were chosen to 1) reduce penetrating radiation as much as possible, primarily with hydrogen-bearing polymers, 2) attempt to provide an air-tight structure, 3) sufficiently mix and adsorb to regolith grains for strength, 4) maximize tolerance to day-night thermal cycling, 5) possibly increase electrical conductivity to dissipate any accumulated static charge, and 6) ease their application on planetary surfaces (specifically, the accommodation of reduced atmosphere and lack of heat sinks). Some of these materials have been tested with respect to radiation mitigation, micrometeorite resistance, and resistance to larger, slower-traveling pieces of regolith impinging on the surface, simulating nearby launch and landing activities. Conceptual designs for a Continuous Feedstock Delivery/Mixing System (CFDMS) will also be presented and future planned activities will be discussed as well.

Werkheiser, Niki↗

MMIC-I: A Robotic Platform for Assembly Integration and Internal Locomotion through Mechanical Meta-Material Structures

In-space assembly is crucial to creating large-scale space structures and enabling long term space missions. Natural limitations in the size of transportation vehicles and ISRU production facilities necessitate an additive strategy with the size of the typical structural unit being essentially fixed and inversely proportional to the final assembly size. In prior robotic and space assembly examples, reversible mechanical integration of structural modules is typically achieved with actuated alignment and fastening mechanisms onboard every structural module. Additive assembly or manufacturing planning approaches often feature a “build front” that receives new materials or parts and progresses gradually across the target geometry. The system we describe here places much of the alignment and fastener actuation systems onboard a mobile robot that can operate at a build front while companion robots (Scaling Omni-directional Lattice Locomoting Explorer, SOLLE) provide part or material transportation. The design and evaluation of this Mobile Meta-Material Interior Co-Integrator (MMIC-I), an inchworm-style locomoting robotic assembler, is described here with an emphasis on ease of assembly and a low number of unique parts for a simple design. It is designed to assist in alignment of cuboctahedron structural unit cells with captive fasteners, defining the build front in operation. Adjacent structural unit cells are locked together with specified axial and rotational actuation of the fasteners. Hardware prototypes show that the robot is able to successfully locomote to any indexed location within a lattice structure and bolt together each set of fasteners on any interface.

Robotics↗

Sustainability pathways for perovskite photovoltaics

Solar energy is the fastest-growing source of electricity generation globally. As deployment increases, photovoltaic (PV) panels need to be produced sustainably. Therefore, the resource utilization rate and the rate at which those resources become available in the environment must be in equilibrium while maintaining the well-being of people and nature. Metal halide perovskite (MHP) semiconductors could revolutionize PV technology due to high efficiency, readily available/accessible materials and low-cost production. Here we outline how MHP-PV panels could scale a sustainable supply chain while appreciably contributing to a global renewable energy transition. Further, we evaluate the critical material concerns, embodied energy, carbon impacts and circular supply chain processes of MHP-PVs. The research community is in an influential position to prioritize research efforts in reliability, recycling and remanufacturing to make MHP-PVs one of the most sustainable energy sources on the market.

14 SOLAR ENERGY↗

Concealed Cathode Degradation in Lithium-Ion Cells with a Ni-Rich Oxide

Difficulties with sourcing cobalt and the interest in increasing cell energy have motivated the development of Ni-rich oxide materials for lithium-ion battery cathodes. Despite the intense research on the topic, there is limited information available on the long-term performance of novel cathode formulations. Here, we evaluate the stability of LiNi 0.9 Mn 0.05 Co 0.05 O 2 in full-cells tested for over five months, assessing how cycling, voltage and electrolyte additives impact cathode aging. We use differential voltage analysis to extract insights about the cathode from the full-cell data and identify the isolation of cathode particles in the delithiated (charged) state as a relevant mode of aging. Importantly, this particular mechanism of cathode aging does not cause immediate cell capacity fade, causing the simple analysis of cell capacity retention to overestimate the cathode stability under the investigated conditions. So, our observations serve as cautionary tale indicating that careful analysis of data from extended testing may be required for assessing the performance of Ni-rich cathodes and for evaluating how these materials are affected by electrolyte additives.

25 ENERGY STORAGE↗

A study for development of aerothermodynamic test model materials and fabrication technique

A literature survey, materials reformulation and tailoring, fabrication problems, and materials selection and evaluation for fabricating models to be used with the phase-change technique for obtaining quantitative aerodynamic heat transfer data are presented. The study resulted in the selection of two best materials, stycast 2762 FT, and an alumina ceramic. Characteristics of these materials and detailed fabrication methods are presented.

Dean, W. G.↗

Evaluation of Aluminum-Boron Carbide Neutron Absorbing Materials for Interim Storage of Used Nuclear Fuel

The objective of this work was to understand the corrosion behavior of Boral® and Bortec® neutron absorbers over long-term deployment in a used nuclear fuel dry cask storage environment. Corrosion effects were accelerated by flowing humidified argon through an autoclave at temperatures up to 570°C. Test results show little corrosion of the aluminum matrix but that boron is leaching out of the samples. Initial tests performed at 400 and 570°C were hampered by reduced flow caused by the rapid build-up of solid deposits in the outlet lines. Analysis of the deposits by XRD shows that the deposits are comprised of boron trioxide and sassolite (H 3 BO 3 ). The collection of boron- containing compounds in the outlet lines indicated that boron was being released from the samples. Observation of the exposed samples using SEM and optical microscopy show the growth of new phases in the samples. These phases were most prominent in Bortec® samples exposed at 570°C. Samples of Boral® exposed at 570°C showed minimal new phase formation but showed nearly the complete loss of boron carbide particles. Boron carbide loss was also significant in Boral samples at 400°C. However, at 400°C phases similar to those found in Bortec® were observed. The rapid loss of the boron carbide particles in the Boral® is suspected to inhibit the formation of the new secondary phases. However, Material samples in an actual dry cask environment would be exposed to temperatures closer to 300°C and less water than the lowest test. The results from this study conclude that at the temperature and humidity levels present in a dry cask environment, corrosion and boron leaching will have no effect on the performance of Boral® and Bortec® to maintain criticality control.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Evaluation of a metering, mixing, and dispensing system for mixing polysulfide adhesive

Tests were performed to evaluate whether a metered mixing system can mix PR-1221 polysulfide adhesive as well as or better than batch-mixed adhesive; also, to evaluate the quality of meter-mixed PR-1860 and PS-875 polysulfide adhesives. These adhesives are candidate replacements for PR-1221 which will not be manufactured in the future. The following material properties were evaluated: peel strength, specific gravity and adhesive components of mixed adhesives, Shore A hardness, tensile adhesion strength, and flow rate. Finally, a visual test called the butterfly test was performed to observe for bubbles and unmixed adhesive. The results of these tests are reported and discussed.

Evans, Kurt B.↗

Consumables and wastes estimations for the First Lunar Outpost

The First Lunar Outpost mission is a design reference mission for the first human return to the moon. This paper describes a set of consumables and waste material estimations made on the basis of the First Lunar Outpost mission scenario developed by the NASA Exploration Programs Office. The study includes the definition of a functional interface framework and a top-level set of consumables and waste materials to be evaluated, the compilation of mass flow information from mission developers supplemented with information from the literature, and the analysis of the resulting mass flow information to gain insight about the possibility of material flow integration between the moon outpost elements. The results of the study of the details of the piloted mission and the habitat are used to identify areas where integration of consumables and wastes across different mission elements could provide possible launch mass savings.

Theis, Ronald L. A.↗

Lightweight Materials for Automotive Application: An Assessment of Material Production Data for Magnesium and Carbon Fiber

The use of lightweight materials in vehicle components, also known as “lightweighting,” can result in automobile weight reduction, which improves vehicle fuel economy and generally its environmental footprint. Materials often used for vehicle lightweighting include aluminum, magnesium, and polymers reinforced with either glass or carbon fiber. However, because alternative materials typically used for vehicle lightweighting require more energy to make on a per part basis than the material being replaced (often steel or iron), the fuel efficiency improvement induced by a weight reduction is partially offset by an increased energy for the vehicle material production. To adequately quantify this tradeoff, reliable and current values for life-cycle production energy are needed for both conventional and alternative materials. Our focus here is on the production of two such alternative materials: magnesium and carbon fibers. Both these materials are low density solids with good structural properties. These properties have enabled their use in applications where weight is an issue, not only for automobiles but also for aerospace applications. This report addresses the predominant production methods for these materials and includes a tabulation of available material and energy input data necessary to make them. The life cycle inventory (LCI) information presented herein represents a process chain analysis (PCA) approach to life cycle assessment (LCA) and is intended for evaluation as updated materials production data for magnesium and carbon fiber for inclusion into the Greenhouse gases, Regulated Emissions, and Energy use in Transportation model (GREET2_2012). The summary life-cycle metrics used to characterize the cradle-to-gate environmental performance of these materials are the cumulative energy demand (CED) and greenhouse gas emissions (GHG) per kilogram of material.

32 ENERGY CONSERVATION, CONSUMPTION, AND UTILIZATI↗

Materials and Methods for Streamlined Laboratory Analysis of Environmental Samples, FY 2016 Report

The International Atomic Energy Agency (IAEA) relies upon laboratory analysis of environmental samples (typically referred to as “swipes”) collected during on-site inspections of safeguarded facilities to support the detection and deterrence of undeclared activities. Unfortunately, chemical processing and assay of the samples is slow and expensive. A rapid, effective, and simple extraction process and analysis method is needed to provide certified results with improved timeliness at reduced costs (principally in the form of reduced labor), while maintaining or improving sensitivity and efficacy. To address these safeguard needs the Pacific Northwest National Laboratory (PNNL) explored and demonstrated improved methods for environmental sample (ES) analysis. Improvements for both bulk and particle analysis were explored. To facilitate continuity and adoption, the new sampling materials and processing methods will be compatible with existing IAEA protocols for ES analysis. PNNL collaborated with Oak Ridge National Laboratory (ORNL), which performed independent validation of the new bulk analysis methods and compared performance to traditional IAEA’s Network of Analytical Laboratories (NWAL) protocol. ORNL efforts are reported separately. This report describes PNNL’s FY 2016 progress, which was focused on analytical application supporting environmental monitoring of uranium enrichment plants and nuclear fuel processing. In the future the technology could be applied to other safeguard applications and analytes related to fuel manufacturing, reprocessing, etc. PNNL’s FY 2016 efforts were broken into two tasks and a summary of progress, accomplishments and highlights are provided below. Principal progress and accomplishments on Task 1, Optimize Materials and Methods for ICP-MS Environmental Sample Analysis, are listed below. • Completed initial procedure for rapid uranium extraction from ES swipes based upon carbonate-peroxide chemistry (delivered to ORNL for evaluation). • Explored improvements to carbonate-peroxide rapid uranium extraction chemistry. • Evaluated new sampling materials and methods (in collaboration with ORNL). • Demonstrated successful ES extractions from standard and novel swipes for a wide range uranium compounds of interest including UO 2 F 2 and UO 2 (NO 3 ) 2 , U 3 O 8 and uranium ore concentrate. • Completed initial discussions with commercial suppliers of PTFE swipe materials. • Submitted one manuscript for publication. Two additional drafts are being prepared. Principal progress and accomplishments on Task 2, Optimize Materials and Methods for Direct SIMS Environmental Sample Analysis, are listed below. • Designed a SIMS swipe sample holder that retrofits into existing equipment and provides simple, effective, and rapid mounting of ES samples for direct assay while enabling automation and laboratory integration. • Identified preferred conductive sampling materials with better performance characteristics. • Ran samples on the new PNNL NWAL equivalent Cameca 1280 SIMS system. • Obtained excellent agreement between isotopic ratios for certified materials and direct SIMS assay of very low levels of LEU and HEU UO 2 F 2 particles on carbon fiber sampling material. Sample activities range from 1 to 500 CPM (uranium mass on sample is dependent upon specific isotope ratio but is frequently in the subnanogram range). • Found that the presence of the UF molecular ions, as measured by SIMS, provides chemical information about the particle that is separate from the uranium isotopics and strongly suggests that those particles originated from an UF6 enrichment activity. • Submitted one manuscript for publication. Another manuscript is in preparation.

98 NUCLEAR DISARMAMENT, SAFEGUARDS, AND PHYSICAL P↗

An efficient computational approach to model statistical correlations in photon counting x-ray detectors

Purpose: To introduce and evaluate an increment matrix approach (IMA) describing the signal statistics of energy-selective photon counting detectors including spatial–spectral correlations between energy bins of neighboring detector pixels. The importance of the occurring correlations for image-based material decomposition is studied. Methods: An IMA describing the counter increase patterns in a photon counting detector is proposed. This IMA has the potential to decrease the number of required random numbers compared to Monte Carlo simulations by pursuing an approach based on convolutions. To validate and demonstrate the IMA, an approximate semirealistic detector model is provided, simulating a photon counting detector in a simplified manner, e.g., by neglecting count rate-dependent effects. In this way, the spatial–spectral correlations on the detector level are obtained and fed into the IMA. The importance of these correlations in reconstructed energy bin images and the corresponding detector performance in image-based material decomposition is evaluated using a statistically optimal decomposition algorithm. Results: The results of IMA together with the semirealistic detector model were compared to other models and measurements using the spectral response and the energy bin sensitivity, finding a good agreement. Correlations between the different reconstructed energy bin images could be observed, and turned out to be of weak nature. These correlations were found to be not relevant in image-based material decomposition. An even simpler simulation procedure based on the energy bin sensitivity was tested instead and yielded similar results for the image-based material decomposition task, as long as the fact that one incident photon can increase multiple counters across neighboring detector pixels is taken into account. Conclusions: The IMA is computationally efficient as it required about 10{sup 2} random numbers per ray incident on a detector pixel instead of an estimated 10{sup 8} random numbers per ray as Monte Carlo approaches would need. The spatial–spectral correlations as described by IMA are not important for the studied image-based material decomposition task. Respecting the absolute photon counts and thus the multiple counter increases by a single x-ray photon, the same material decomposition performance could be obtained with a simpler detector description using the energy bin sensitivity.

60 APPLIED LIFE SCIENCES↗

Microgravity materials processing for commercial applications

An evaluation is made of the development status of materials processing techniques in microgravity environments; the classes of materials treated to date encompass glasses, ceramics, crystals, semiconductors, metals and their alloys, polymers, composites, and such biological substances as pharmaceuticals. Attention is given to the commercial development of composite and mixed-phase materials with substantially improved properties as a result of microgravity processing, as well as to current research into catalysts and Type II-VI semiconductor crystals such as CdTe.

Kohli, R.↗

IRMA

IRMA (In)elastic Representation of Materials As S(α,β) evaluations IRMA turns one phonon model into three outputs that usually require three separate tool chains: an evaluated nuclear-data file, predicted neutron-scattering spectra, and scattering kernels for Monte Carlo transport. The three outputs draw on a single, consistent description of the material, so the evaluation, the spectroscopy that can validate it, and the transport that uses it always agree about the physics. Nuclear data. IRMA writes ENDF-6 File 7 thermal scattering evaluations on automatically constructed (α, β) grids. This part reimplements and generalizes NJOY's LEAPR: the classic kernels reproduce freshly generated NJOY2016 tapes digit for digit and published reference tapes to about 1e-4, and the generalized paths add the exact coherent one-phonon term, anisotropic Debye-Waller tensors, coherent elastic for arbitrary crystals, and a per-species partition for polyatomic materials. The tapes feed NJOY, AMPX, FUDGE, and every transport code downstream of them. Neutron spectroscopy. The irma.spectra forward model projects the same physics onto an instrument's kinematics and resolution: INS spectra for VISION and generic indirect geometries, and 2-D S(Q,E) powder maps for direct-geometry spectrometers, from a phonopy model or straight from a phonon DOS. It can be used to predict a proposed measurement before beam time; in analysis, it supplies the calculated single-scattering counterpart of a measured spectrum, from the same material description the evaluation was built from. Monte Carlo transport. The irma.ncrystal exporter writes per-temperature scattering kernels for the companion NCrystal plugin, so McStas, OpenMC, and other NCrystal-aware codes sample the same physics. The exported kernels carry the per-site anisotropic Debye-Waller tensors, keeping directional coherent-elastic physics that NCrystal's standard scalar treatment does not represent. With the same physics inside a transport code, an entire beamline becomes a virtual experiment: IRMA's end-to-end validation ran a custom McStas implementation of the ARCS spectrometer, assembled from the existing McVine and McStas models, against measured data. From a bare crystal structure. The irma mlip front end builds the phonon model itself: a structure file and a choice of potential are enough. Nine pretrained machine-learned interatomic potentials are supported, on a laptop CPU, with no first-principles calculation; an approximate phonon model for a new material costs minutes, not a DFT campaign, and the build emits prefilled inputs for all three outputs. The result is a good starting point rather than a finished evaluation: survey-quality physics with every parameter exposed for review. A converged atomistic calculation enters the same way, as a phonopy model, when higher fidelity is needed.

Ramic, Kemal [Oak Ridge National Laboratory (ORNL)↗