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At least 307 records · Page 17

Adaptation of an In Situ Ground-Based Tropospheric OH/HO2 Instrument for Aircraft Use

In-situ HO(x) (OH and HO2) measurements are an essential part of understanding the photochemistry of aircraft exhaust in the atmosphere. HO(x) affects the partitioning of nitrogen species in the NO(y) family. Its reactions are important sources and sinks for tropospheric ozone, thus providing a link between the NO(x) in aircraft exhaust and tropospheric ozone. OH mixing ratios are enhanced in aircraft wakes due to the photolysis of the HONO that is made close to the engine. Measurements of HO(x) in aircraft wakes, along with NO(x) measurements, thus provides a constraint on chemical models of the engine combustion and exhaust. The development of the Airborne Tropospheric Hydrogen Oxides Sensor (ATHOS) is reported. We designed, developed, and successfully flew this instrument. It was part of the instrument complement on board the NASA DC-8 during SUCCESS, which took place in Kansas in April and May, 1996. ATHOS has a limit-of-detection for OH (S/N = 2) of 10(exp 5) OH molecules cm(exp -3) in less than 150 seconds. While this sensitivity is about 2-3 times less than the initial projections in the proposal, it is more than adequate for good measurements of OH and HO2 from the planetary boundary layer to the stratosphere. Our participation in SUCCESS was to be engineering test flights for ATHOS; however, the high-quality measurements we obtained are being used to study HO(x) photochemistry in contrails, clouds, and the clear air.

Brune, William H.↗

Joining of Silicon Carbide-Based Ceramics by Reaction Forming Method

Recently, there has been a surge of interest in the development and testing of silicon-based ceramics and composite components for a number of aerospace and ground based systems. The designs often require fabrication of complex shaped parts which can be quite expensive. One attractive way of achieving this goal is to build up complex shapes by joining together geometrically simple shapes. However, the joints should have good mechanical strength and environmental stability comparable to the bulk materials. These joints should also be able to maintain their structural integrity at high temperatures. In addition, the joining technique should be practical, reliable, and affordable. Thus, joining has been recognized as one of the enabling technologies for the successful utilization of silicon carbide based ceramic components in high temperature applications. Overviews of various joining techniques, i.e., mechanical fastening, adhesive bonding, welding, brazing, and soldering have been provided in recent publications. The majority of the techniques used today are based on the joining of monolithic ceramics with metals either by diffusion bonding, metal brazing, brazing with oxides and oxynitrides, or diffusion welding. These techniques need either very high temperatures for processing or hot pressing (high pressures). The joints produced by these techniques have different thermal expansion coefficients than the ceramic materials, which creates a stress concentration in the joint area. The use temperatures for these joints are around 700 C. Ceramic joint interlayers have been developed as a means of obtaining high temperature joints. These joint interlayers have been produced via pre-ceramic polymers, in-situ displacement reactions, and reaction bonding techniques. Joints produced by the pre-ceramic polymer approach exhibit a large amounts of porosity and poor mechanical properties. On the other hand, hot pressing or high pressures are needed for in-situ displacement reactions and reaction bonding techniques. Due to the equipment required, these techniques are impractical for joining large or complex shaped components.

Singh, M.↗

Real time acousto-ultrasonic NDE technique for monitoring damage in ceramic composites under dynamic loads

Research effort was directed towards developing a near real-time, acousto-ultrasonic (AU), nondestructive evaluation (NDE) tool to study the failure mechanisms of ceramic composites. Progression of damage is monitored in real-time by observing the changes in the received AU signal during the actual test. During the real-time AU test, the AU signals are generated and received by the AU transducers attached to the specimen while it is being subjected to increasing quasi-static loads or cyclic loads (10 Hz, R = 1.0). The received AU signals for 64 successive pulses were gated in the time domain (T = 40.96 micro sec) and then averaged every second over ten load cycles and stored in a computer file during fatigue tests. These averaged gated signals are representative of the damage state of the specimen at that point of its fatigue life. This is also the first major attempt in the development and application of real-time AU for continuously monitoring damage accumulation during fatigue without interrupting the test. The present work has verified the capability of the AU technique to assess the damage state in silicon carbide/calcium aluminosilicate (SiC/CAS) and silicon carbide/ magnesium aluminosilicate (SiC/MAS) ceramic composites. Continuous monitoring of damage initiation and progression under quasi-static ramp loading in tension to failure of unidirectional and cross-ply SiC/CAS and quasi-isotropic SiC/MAS ceramic composite specimens at room temperature was accomplished using near real-time AU parameters. The AU technique was shown to be able to detect the stress levels for the onset and saturation of matrix cracks, respectively. The critical cracking stress level is used as a design stress for brittle matrix composites operating at elevated temperatures. The AU technique has found that the critical cracking stress level is 10-15% below the level presently obtained for design purposes from analytical models. An acousto-ultrasonic stress-strain response (AUSSR) model for unidirectional and cross-ply ceramic composites was formulated. The AUSSR model predicts the strain response to increasing stress levels using real-time AU data and classical laminated plate theory. The Weibull parameters of the AUSSR model are used to calculate the design stress for thermo-structural applications. Real-time AU together with the AUSSR model was used to study the failure mechanisms of SiC/CAS ceramic composites under static and fatigue loading. An S-N curve was generated for a cross-ply SiC/CAS ceramic composite material. The AU results are corroborated and complemented by other NDE techniques, namely, in-situ optical microscope video recordings and edge replication.

Tiwari, Anil↗

Free-Flying Magnetometer Data System

The Free-Flying Magnetometer (FFM) is an autonomous "sensorcraft" developed at the Jet Propulsion Laboratory (JPL) for the Enstrophy sounding rocket mission. This mission was a collaborative project between the University of New Hampshire, Cornell University and JPL. The science goal of the mission was the study of current filamentation phenomena in the northern auroral region through multipoint measurements of magnetic field. The technical objective of the mission was the proof of concept of the JPL FFM design and the demonstration of an in-situ multipoint measurement technique employing many free-flying spacecraft. Four FFMs were successfully deployed from a sounding rocket launched from Poker Flats, Alaska on February 11, 1999. These hockey-puck-sized (80 mm diameter, 38 mm. height, 250 gram mass) free flyers each carry a miniature 3-axis flux-gate magnetometer that output +/- 2 V signals corresponding to a +/- 60,000 nT measurement range for each axis. The FFM uses a synchronized four-channel Sigma(Delta) Analog-to-Digital Converter (ADC) having a dynamic range of +/- 2.5V and converting at a rate of 279 samples/second/channel. Three channels are used to digitize the magnetometer signals to 17-bit (1.144 nT/bit) resolution. The fourth ADC channel is multiplexed for system monitoring of four temperature sensors and two battery voltages. The FFM also contains two sun sensors, a laser diode which emits a fan-shaped beam, a miniature S-band transmitter for direct communication to the ground station antennas, an ultra-stable Temperature Compensated Crystal Oscillator (TCXO) clock, an integrated data subsystem implemented in a Field-Programmable Gate Array (FPGA), a 4 Mbit Static Random Access Memory (SRAM) for data storage and Lithium Thionyl Chloride batteries for power. Communicating commands to the FFM prior to deployment is achieved with an infrared (IR) link. The FFM IR receiver responds to 9-bit pulse coded signals that are generated by an IR Light Emitting Diode (LED) in the payload for turning FFM power on or off and placing the FFM in a test mode or flight mode. The IR links are also used to synchronize (zero) the clocks onboard all the FFMs through a reset pulse originating from the payload GPS receiver that is issued when the FFMs are in flight mode. The FPGA based data subsystem manages continuous data collection from the four ADC channels and sun sensors, formatting and storing the data to SRAM, and controlling downlink transmission. The transmitter is powered only after a 2547 frame SRAM buffer has been filled (approx. 5 minutes of data). The data is Viterbi encoded and sent to the S-band transmitter via a First-In-First-Out (FIFO) buffer who's output is clocked at 100 bits/second. After the 26-second transmission, the transmitter is turned off to reduce noise coupling to the sensitive magnetometer. The data subsystem control consists of a master state machine that performs data flow management and is interfaced through a prioritized interrupt scheme to state machines that service the ADC, sun sensors and transmitter FIFO. Continuous data collection prevents the missing of data during transmission and provides implicit time tagging of the data acquired by the ADC because of synchronization with the TCXO clock.

Blaes, B.↗

Precision Agriculture using Networks of Degradable Analytical Sensors (PANDAS) (Final Technical Report)

Precision agriculture, where sensing of soil, environment and crop conditions are used to precisely synchronize inputs (such as water and fertilizer) to crop needs enhances input use efficiency. This can improve yields and farm profitability while mitigating environmental losses, improving soil carbon content and substantially decreasing energy use for food, feed and fuel crops. Unfortunately, farmers are not yet able to harness the full potential of these management technologies as there is a lack of available management information, and there is therefore a need for sensors that are able to economically measure spatio-temporal variability in soil and crop properties of extremely heterogeneous farm fields precisely at high resolution and at low cost. Real-time, in-situ monitoring of agricultural soil conditions is today carried out using devices that limit the total number of nodes that can be used economically to typically one per acre or less. Higher spatio-temporal resolution sensing would enable more precise agricultural input optimization, with significant benefits to the farmer and the environment. In order to address this issue, this project focused on developing additively manufactured, biodegradable, soil sensors with predicted costs of < $\$$1 per unit to monitor crop inputs (such as water and fertilizer) that predictably, harmlessly degrade away into the soil when no longer needed. These sensor nodes should be easy to place, accurately and continuously monitor soil and crop conditions for an entire season, be read remotely using existing farm equipment, require no ongoing maintenance, not impede farm operations and produce no persistent waste. This approach could enable a >100× increase in information density over current solutions for precision farming of row and other crops, and lead to significant reductions in input energy use and provide increased yield for biofuel crops. Over the course of this project the team at the University of Colorado Boulder, University of California Berkeley, and Colorado State University/Kansas State University investigated a wide range of printable biodegradable electronic materials and sensor designs for determining soil moisture and soil nitrate concentration. These efforts expanded the available materials set for printed soil degradable electronic materials, particularly for conductors, enabling high conductivity and stability. Printed soil moisture and nitrate sensors with suitable sensitivity and selectivity were developed and characterized. Low power and passive wireless electronic systems were integrated with the soil sensors, and testing was carried out with completed sensors to understand their functionality under agricultural conditions. Additionally, other sensor types enabled by the biodegradable materials set created during this project, such as soil microbial activity sensors, were also developed and demonstrated. Project outputs include 10 peer reviewed publications, 4 patent applications, 21 technical presentations, 3 PhD thesis, 10 media reports, 8 additional grants worth over $\$$6M, and the formation of 3 start-up companies.

32 ENERGY CONSERVATION, CONSUMPTION, AND UTILIZATI↗

AFM Studies of Lunar Soils and Application to the Mars 2001 Mission

The upcoming Mars 01 mission will carry an Atomic Force Microscope (AFM) as part of the Mars Environmental Compatibility Assessment (MECA) instrument. By operating in a tapping mode, the AFM is capable of sub-nanometer resolution in three dimensions and can distinguish between substances of different compositions by employing phase contrast imaging. To prepare for the Mars 01 mission, we are testing the AFM on a lunar soil to determine its ability to define particle shapes and sizes and grain-surface textures. The test materials are from the Apollo 17 soil 79221, which is a mixture of agglutinates, impact and volcanic beads, and mare and highland rock and mineral fragments. The majority of the lunar soil particles are less than 100 microns in size, comparable to the sizes estimated for martian dust. We have used the AFM to examine several different soil particles at various resolutions. The instrument has demonstrated the ability to identify parallel ridges characteristic of twinning on a 150 micron plagioclase feldspar particle. Extremely small (10-100 nanometer) adhering particles are visible on the surface of the feldspar grain, and they appear elongate with smooth surfaces. Phase contrast imaging of the nanometer particles shows several compositions to be present. When the AFM was applied to a 100 micron glass spherule, it was possible to define an extremely smooth surface; this is in clear contrast to results from a basalt fragment which exhibited a rough surface texture. Also visible on the surface of the glass spherule were chains of 100 nanometer and smaller impact melt droplets. For the '01 Mars mission, the AFM is intended to define the size and shape distributions of soil particles, in combination with the NMCA optical microscope system and images from the Robot Arm Camera (RAC). These three data sets will provide a means of assessing potentially hazardous soil and dust properties. The study that we have conducted on the lunar soils now suggests that the NMCA experiment will be able to define grain transport and weathering processes. For example, it should be possible to determine if Martian grains have been subjected to aeolian or water transport, volcanic activity, impact melting processes, in-situ weathering, and a host of other processes. Additionally, textural maturity could be assessed (via freshness and form of fracture patterns and grain shapes). Thus, the AFM has the potential to shed new light on Martian surface processes by adding the submicroscopic dimension to planetary investigations.

Weitz, C. M.↗

Whole metagenome sequencing and 16S rRNA gene amplicon analyses reveal the complex microbiome responsible for the success of enhanced in-situ reductive dechlorination (ERD) of a tetrachloroethene-contaminated Superfund site

The North Railroad Avenue Plume (NRAP) Superfund site in New Mexico, USA exemplifies successful chlorinated solvent bioremediation. NRAP was the result of leakage from a dry-cleaning that operated for 37 years. The presence of tetrachloroethene biodegradation byproducts, organohalide respiring genera (OHRG), and reductive dehalogenase (rdh) genes detected in groundwater samples indicated that enhanced reductive dechlorination (ERD) was the remedy of choice. This was achieved through biostimulation by mixing emulsified vegetable oil into the contaminated aquifer. This report combines metagenomic techniques with site monitoring metadata to reveal new details of ERD. DNA extracts from groundwater samples collected prior to and at four, 23 and 39 months after remedy implementation were subjected to whole metagenome sequencing (WMS) and 16S rRNA gene amplicon (16S) analyses. The response of the indigenous NRAP microbiome to ERD protocols is consistent with results obtained from microcosms, dechlorinating consortia, and observations at other contaminated sites. WMS detects three times as many phyla and six times as many genera as 16S. Both techniques reveal abundance changes in Dehalococcoides and Dehalobacter that reflect organohalide form and availability. Methane was not detected before biostimulation but appeared afterwards, corresponding to an increase in methanogenic Archaea. Assembly of WMS reads produced scaffolds containing rdh genes from Dehalococcoides, Dehalobacter, Dehalogenimonas, Desulfocarbo, and Desulfobacula. Anaerobic and aerobic cometabolic organohalide degrading microbes that increase in abundance include methanogenic Archaea, methanotrophs, Dechloromonas, and Xanthobacter, some of which contain hydrolytic dehalogenase genes. Aerobic cometabolism may be supported by oxygen gradients existing in aquifer microenvironments or by microbes that produce O 2 via microbial dismutation. The NRAP model for successful ERD is consistent with the established pathway and identifies new taxa and processes that support this syntrophic process. This project explores the potential of metagenomic tools (MGT) as the next advancement in bioremediation.

59 BASIC BIOLOGICAL SCIENCES↗

Transition from Pool to Flow Boiling: The Effect of Reduced Gravity

Applications of boiling heat transfer in space can be found in the areas of thermal management, fluid handling and control, power systems, on-orbit storage and supply systems for cryogenic propellants and life support fluids, and for cooling of electronic packages for power systems associated with various instrumentation and control systems. Recent interest in exploration of Mars and other planets, and the concepts of in-situ resource utiliLation on Mars highlights the need to understand the effect of gravity on boiling heat transfer at gravity levels varying from 1>= g/g(sub e) >=10(exp -6). The objective of the proposed work was to develop a mechanistic understanding of nucleate boiling and critical heat flux under low and micro-gravity conditions when the velocity of the imposed flow is small. For pool boiling, the effect of reduced gravity is to stretch both the length scale as well as the time scale for the boiling process. At high flow velocities, the inertia of the liquid determines the time and the length scales and as such the gravitational acceleration plays little role. However, at low velocities and at low gravity levels both liquid inertia and buoyancy are of equal importance. At present, we have little understanding of the interacting roles of gravity and liquid inertia on the nucleate boiling process. Little data that has been reported in the literature does not have much practical value in that it can not serve as a basis for design of heat exchange components to be used in space. Both experimental and complete numerical simulations of the low velocity, low-gravity nucleate boiling process were carried out. A building block type of approach was used in that first the growth and detachment process of a single bubble and flow and heat transfer associated with the sliding motion of the bubble over the heater surface after detachment was studied. Liquid subcooling and flow velocity were varied parametrically. The experiments were conducted at 1 g(sub e), while varying the orientation of surface with respect to the gravity vector. In the laboratory experiments, holographic interferometry was used to obtain data on velocity and temperature fields associated with a bubble prior to, and after detachment and during sliding motion. A test rig for conducting experiments in the KC-135 was developed, but experiments could not be conducted due to the unavailability of the aircraft prior to completion of the project. Numerical simulations modeling the micro and macro regions of the bubble were carried out in three dimensions. The results of the experiments were used to validate analytical/numerical models.

Dhir, Vijay K.↗

Origin and Reactivity of the Martian Soil: A 2003 Micromission

The role of water in the development of the martian surface remains a fundamental scientific question. Did Mars have one or more "warm and wet" climatic episodes where liquid water was stable at the surface? If so, the mineral phases present in the soils should be consistent with a history of aqueous weathering. More generally, the formation of hydrated mineral phases on Mars is a strong indicator of past habitable surface environments. The primary purpose of this investigation is to help resolve the question of whether such aqueous indicators are present on Mars by probing the upper meter for diagnostic mineral species. According to Burns [1993], the formation of the ferric oxides responsible for the visible color of Mars are the result of dissolution of Fe (+2) phases from basalts followed by aqueous oxidation and precipitation of Fe" mineral assemblages. These precipitates likely included iron oxyhydroxides such as goethite (a-FeOOH) and lepidocrocite (g-FeOOH), but convincing evidence for these phases at the surface is still absent. The stability of these minerals is enhanced beneath the surface, and thus we propose a subsurface search for hydroxylated iron species as a test for a large-scale chemical weathering process based on interactions with liquid water. It is also possible that the ferric minerals on Mars are not aqueous alteration products of the rocks. A chemical study of the Pathfinder landing site concluded that the soils are not directly derived from the surrounding rocks and are enhanced in Mg and Fe. The additional source of these elements might be from other regions of Mars and transported by winds, or alternatively, from exogenic sources. Gibson [1970] proposed that the spectral reflectivity of Mars is consistent with oxidized meteoritic material. Yen and Murray [1998] further extend Gibson's idea and show, in the laboratory, that metallic iron can be readily oxidized to maghemite and hematite under present-day martian surface conditions (in the absence of liquid water). A test for a meteoritic component of the soil can be conducted, as described below, by searching for the presence of Ni at the martian surface. The average abundance of nickel in an Fe-Ni meteorite is about 7% and, if present at measurable levels in the soil, would be indicative of an exogenic contribution. In addition, it may be possible to directly search for mineral phases common in meteorites. An understanding of the formation and evolution of the martian soil would not be complete without addressing the unusual reactivity discovered by the Viking Landers The presence of an inorganic oxidant, possibly one produced as a results of photochemical processes, is the most widely accepted explanation of the Viking results. Are these chemical species simply adsorbed on soil grains, or have they reacted with the metal oxide substrates and altered the mineral structures? Could a completely different (non-photochemical) process be responsible for the soil reactivity? The various ideas for the nature of this putative oxidant could be constrained by a measurement of the change in reactivity with depth. Different compositions will have different lifetimes and mobilities and thus will have different vertical profiles. Because the oxidizing compounds are believed to actively destroy organic molecules, determination of the reactivity gradient also has significant implications for the search for life on Mars. A DS2-based microprobe system can be instrumented for a 2003 micromission to investigate the origin and reactivity of the martian soil. These measurements would provide invaluable information regarding the climate history and exobiological potential of the planet. The NMR, X ray and chemiresistor measurement approach described embodies a highly synergistic and general set of soil interrogation methods for elements, compounds, and crystal structures and can also be applied to other geologic questions of interest. For example, if the capability for precise targeting of the probes is available, then in-situ investigations of suspected evaporite and hydrothermal deposits would be possible with the same set of instruments. Additional information is contained in the original.

Yen, Albert S.↗

Impacts of PV Module Connector Failures on Cost and Performance of Utility Scale Photovoltaic Systems

The reliability, cost and performance of electrical connectors are a concern in all types of electrical systems, and demands on connectors used on photovoltaic (PV) systems include that connectors maintain electrical conductivity and physical strength, endure ultraviolet sunlight and high ambient temperature, and resist moisture and chemical intrusion over a very long (>25 year) performance period. Connector failures increase operation and maintenance (O&M) costs and reduce plant production, but connector failure can also cause safety and liability problems, which are of greater concern. This work results from a three-year collaboration between Sandia National Laboratories (SNL), the Electric Power Research Institute (EPRI), and the National Renewable Energy Laboratory (NREL) and funded by the U.S. Department of Energy (DOE) Solar Energy Technology Office (SETO) under Agreements #39035 and #38531 "Connector Reliability Across the US Solar Sector." a multi-pronged investigation of PV connector health across the US (see https://energy.sandia.gov/pvconnectors/). This report presents derivation of a Techno-Economic Analysis (TEA) that models failure modes and frequencies (how often failure occurs), estimates O&M costs and lost production associated with connector failures, and then calculates the effect that PV module connectors can have on Levelized Cost of Energy (LCOE). The model is informed with initial data from quantitative assessment of failure rates, root causes and mechanisms, in-situ diagnostics and data collection, lab-based forensics, and interviews with PV connector manufacturers and plant operators. SNL conducted site inspections at multiple utility-scale sites in different climates and subjected field samples of new, used, and degraded connectors to visual and electrical characterization. EPRI conducted metallurgical analysis of the pin and sleeve conductors to study failure-induced morphological and compositional changes. There is in general a shortage of statistically valid data, but data from PVROM database maintained by SNL was sufficient to ascertain failure rates and lost production as well as provide qualitative insight in its curated maintenance records. This report details the structure of the mathematical model but the sources of data to inform the model will continue to evolve. Analysis of a 100 MW PV plant is provided as an example of the use of the model, with results indicating that connectors are responsible for Annualized O&M Costs of $\$$71,933/year; Annualized Unit O&M Costs of $\$$0.72/kW/year; that a Reserve Account of $\$$187,220 should be available to fund repairs related to connectors; that connectors add $\$$1,494,004 to the Net Present Value of the O&M Costs (project life); and that O&M related to connectors adds about $\$$0.00088/kWh to the Levelized Cost of Energy. The impact of this model is to provide a tool to make the US solar sector more robust by quantifying and monetizing the reliability risks to utility-scale PV systems posed by poorly installed, mismatched and/or poorly designed and manufactured connectors. The TEA provides a model incorporating failure statistics, O&M cost data, and lost production into a single figure of merit, informing decisions and enabling practitioners to optimize cost and performance trade-offs. Stakeholders include connector manufacturers, system designers and equipment specifiers, standards bodies, installers and O&M providers, investors and insurance underwriters. This report supports continued growth of PV predicated on assurances that properly installed and maintained PV system connectors are safe and reliable. The project team is proposing future work including accelerated testing of connectors and expanding the approach taken here to other PV system components, such as TEA for rapid shut-down devices.

14 SOLAR ENERGY↗

The ePIC dual-radiator RICH detector

The dual radiator Ring Imaging Cherenkov (dRICH) detector is required to provide continuous hadron identification from ≈3 GeV/c up to ≈50 GeV/c, and to supplement electron and positron identification from a few hundred MeV/c up to about 15 GeV/c, in the forward (ion-side) end-cap of the ePIC experiment. Such an extended momentum range imposes the use of two radiators, gas and aerogel. The common imaging system, that ensures compactness and cost-effectiveness, is based on SiPM sensors to work in a high non-uniform magnetic field. During the R&D phase, the dual radiator principle and the single component performance have been validated. A status overview of the project is presented. The design and technological choices are discussed together with the results obtained from laboratory characterization of the component demonstrators and beam tests of the evolving prototypes.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗

Multiscale investigation of thermomechanical and compositional developments in Ni alloy 718 under laser processing

Laser processing has been widely employed in various applications due to its exceptional spatial resolution. However, the rapid temperature gradients generated in localized areas present significant challenges for experimental characterization using conventional instruments. To characterize Ni alloy 718 during laser processing, we employed in-situ synchrotron X-ray diffraction with a high-speed detector, a method particularly well-suited for probing processes with high temporal and spatial resolution. Through a series of in-situ experiments, we investigated the local variations in the evolution of microstructures and thermomechanical behaviors within a keyhole mode melt pool. The in situ macroscopic thermomechanical behaviors were quantified using an empirical model derived from diffraction patterns, with experimental results showing reasonable agreement with finite element analysis. Various laser parameters were tested to assess their influences on the residual strains in the melt pools. The results revealed that the residual strain in the keyhole mode melt pool is relatively insensitive to variations in the parameters and is smaller than that in the melt pool created under conduction mode laser scanning. Additionally, we analyzed the shapes of individual diffraction spots, providing insights into the plastic behaviors and compositional developments in the resolidified alloy. The analysis confirmed that compositional variations in a dendritic microstructure manifest as asymmetric broadening of the diffraction spots.

Ni alloy 718↗

In-Situ Visualization of a Growing Brittle Crack in Aluminum Oxynitride Using Synchrotron X-Rays and the Double-Cleavage Drilled Compression Geometry

Brittle fracture is difficult to study in situ due to the speed of a growing crack and the often-catastrophic nature of failure in brittle materials. As a result, the influence of microstructural considerations, such as orientation, grain boundary locations, and strain field, on the crack path remains poorly understood. Presented in this study is a method addressing this knowledge gap, which utilizes the double-cleavage drilled compression geometry to achieve quasi-stable fracture in aluminum oxynitride (AlON). Synchrotron X-ray micro-computed tomography is used to characterize the crack shape and length, while high-energy diffraction microscopy provides information on the strains, orientations, and shapes of grains in the microstructure surrounding the crack tip. During testing, the crack grew in discrete and irregular jumps while the fracture toughness falls within reported ranges. The crack in AlON is found to have no greater tendency to crack intergranularly as compared to transgranularly, and grains which are cracked transgranularly do not display a trend in orientation or stress when compared to those around which the crack followed a grain boundary. The high resolution of the crack path and microstructural data provides a path forward for modeling and understanding 3D brittle fracture.

Gorske, Sara F.↗

Spatiotemporally Registered In-Situ and Ex-Situ Datasets for Laser-based Blown Powder Directed Energy Deposition

This dataset is comprised of in situ sensing data collected during laser-based, blown powder directed energy deposition (DED) of Inconel 718 representing eight different printing conditions: (1) nominal, (2) +15% scan speed, (3) +12% laser power, (4) +42% powder feed rate, (5) +100% jerk limit, (6) +10% layer height, (7) +20% hatch spacing, (8) +20% carrier gas flow. All eight DED builds constructed an identical test coupon geometry consisting of geometric features representative of industrial print requirements (e.g., bulk deposition, thin walls, overhangs). In situ data consists of xyz-coordinates (100 Hz) and on-axis melt pool camera video (60 Hz), both of which have been temporally synchronized to spatially map the melt pool camera data. In addition, post-build X-ray computed tomography (XCT) data for each of the eight test geometries have been spatially registered to the recorded xyz-coordinates, allowing for comparisons between melt pool camera data and flaws identified in the XCT data.

additive manufacturing↗

Degradation science: Integrating modeling and experiments to predict localized corrosion processes (Annual Progress Report)

Additively manufactured (AM) eutectic high-entropy alloys (EHEAs), such as nano-lamellar AlCoCrFeNi 2.1 , have excellent strength, ductility, and wear resistance even at elevated temperatures, but their corrosion behavior in aggressive acids at different length scales remain poorly understood. This work investigates the corrosion behavior of laser powder bed–fused (L-PBF) AlCoCrFeNi 2.1 as a function of annealing temperatures, probing degradation mechanisms from nanoscopic to macroscopic length scales. The alloy is dual phase consisting of a ductile FCC L1 2 phase and a high-strength BCC B2 phase. Rapid solidification during L-PBF produces a far-from-equilibrium nano-lamellar structure with nearly homogeneous elemental distribution, which tends to evolve upon annealing toward Cr/Co/Fe-enriched FCC and Al/Ni-enriched B2. Three conditions were studied: as-printed, 600 °C/5 h, and 1000 °C/1 h, over which B2 lamellae coarsen, lamellar spacing increases, and elemental segregation becomes more prominent. Microstructure and chemistry were characterized by scanning electron microscopy (SEM) and energy-dispersive spectroscopy (EDS), while in-situ electrochemical atomic force microscopy (EC-AFM) was used to link early (<5 h) local dissolution to microstructure after exposure in sulfuric acid. EC-AFM highlights preferential dissolution of the BCC/B2 phase where the surrounding matrix is Cr-depleted and directly quantifies the dissolution rates within individual phases, tracks the transition from early nano-scale attack to partial repassivation, to correlate height differences with current and impedance responses. To monitor longer-term behavior (up to 96 h), ex-situ AFM, SEM, and confocal imaging were combined with conventional bulk electrochemical tests, bridging nanoscale observations to micro/meso-scale damage morphologies. At the meso-scale, the deepest dissolution channels align with the build-direction lamellae and melt-pool boundaries, indicating that printing directionality guides the propagation of these localized corrosion sites. Annealing modifies corrosion by restructuring BCC/FCC phase fractions, lamellar spacing, and Cr/Al segregation, thereby changing the cathode/anode ratio and passive film stability. The results clarify how as-printed and annealed nano-lamellar architectures differ in their susceptibility to selective dissolution; how elemental segregation competes with residual stresses along the build direction. With these insights, future work will use CALPHAD-guided alloy modification to stabilize higher Cr contents in the B2 phase while retaining a dominant FCC+B2/BCC microstructure, with the goal of designing mechanically robust, corrosion-resistant EHEAs for safety-critical applications to leverage the LLNL’s broader national and global security mission.

36 MATERIALS SCIENCE↗

Multiscale and Machine Learning Modeling for Process-informed Microstructure Prediction in Additively Manufactured Materials using MALAMUTE

The Advanced Materials and Manufacturing Technologies (AMMT) program under the Department of Energy Office of Nuclear Energy aims to develop and qualify additively manufactured materials for nuclear applications. One key challenge to this is the microstructural variability observed in the additively manufactured products and their impact on the properties and performance of the material in extreme environments. AMMT is using a combination of high-throughput experimental and modeling techniques to accelerate qualification. Conventionally, in-situ and ex-situ characterizations and testing are performed to correlate different aspects of the additive manufacturing process to the final product and its performance. However, adopting a trial-and-error approach to experimentally evaluate the vast range of process parameters required to capture microstructural variability is cost-prohibitive. Modeling and simulation provide a comparatively inexpensive way to understand and correlate the microstructural evolution to the processing conditions. The modeling and simulation work-packages within the AMMT program aims to use physics-based and machine learning models to develop a digital twin for additive manufacturing that can correlate the process conditions to the final product and establish a process-structure-property-performance (PSPP) correlation. The melting and subsequent solidification that occurs during the additive process is a complex phenomenon that requires multiscale multiphysics analysis. This work package focuses on understanding the role of process variabilities on the unique microstructural characteristics of additively manufactured materials. Microstructural features at the subgrain level, such as compositional micro-heterogeneity and dislocation cells, are of particular interest here since they can influence the creep properties and radiation performance. Idaho National Laboratory’s Multiphysics Object-Oriented Simulation Environment (MOOSE), specifically the MOOSE Application Library for Advanced Manufacturing UTilitiEs (MALAMUTE) software, provides an ideal platform for developing the multiphysics multiscale model to explore the intricacies of the microstructural evolution during the AM processes within a single framework. Furthermore, given that such full-fidelity simulations can be computationally intensive, reduced order models are necessary to explore the PSPP space for additively manufactured materials in an efficient, reliable, and cost-effective way. This work focuses on capturing the microstructural variabilities at the subgrain level that are often missing in the part-scale models. In fiscal year 2025, we significantly advanced upon our work in the last fiscal year, in terms of the predictive capabilities of the physics-based and ML models, by adding the capabilities to capture subgrain-level micro-segregation during solidification using phase-field model and to predict the time-dependent dynamics of the AM process through the MOGPAR model. The alloy solidification model in MOOSE incorporates the thermodynamic properties and free energy relevant to 316 stainless steel. The model demonstrates the Cr and Ni segregation that occurs during solidification, including that the rate of solidification. The microstructural evolution model is connected to the process conditions via the surrogate model developed in this work. This enables predictions of the final microstructure in conjunctions with the manufacturing process. This work supports AMMT's rapid qualification goals by laying the foundation for an efficient and cost-effective model establishing the PSPP correlation for AM. The generated microstructures and predicted micro-segregation can be used by other work packages under AMMT to evaluate the properties and environmental response of the material at the mesoscale. Thus, this work helps to identify the key microstructural features at the subgrain level that are significant in property and performance predictions of additively manufactured components. This work will also provide inputs to the large-scale process variability models to reevaluate and validate assumptions and simplifications made in the part-scale models. Furthermore, through active learning this work can help identify the data need from both modeling and experimental sides for development of a robust digital twin for additive manufacturing and accelerate the AMMT's qualification efforts.

36 - MATERIALS SCIENCE↗

Low Earth orbital atomic oxygen environmental simulation facility for space materials evaluation

Simulation of low Earth orbit atomic oxygen for accelerated exposure in ground-based facilities is necessary for the durability evaluation of space power system component materials for Space Station Freedom (SSF) and future missions. A facility developed at the National Aeronautics and Space Administrations's (NASA) Lewis Research Center provides accelerated rates of exposure to a directed or scattered oxygen beam, vacuum ultraviolet (VUV) radiation, and offers in-situ optical characterization. The facility utilizes an electron-cyclotron resonance (ECR) plasma source to generate a low energy oxygen beam. Total hemispherical spectral reflectance of samples can be measured in situ over the wavelength range of 250 to 2500 nm. Deuterium lamps provide VUV radiation intensity levels in the 115 to 200 nm range of three to five equivalent suns. Retarding potential analyses show distributed ion energies below 30 electron volts (eV) for the operating conditions most suited for high flux, low energy testing. Peak ion energies are below the sputter threshold energy (approximately 30 eV) of the protective coatings on polymers that are evaluated in the facility, thus allowing long duration exposure without sputter erosion. Neutral species are expected to be at thermal energies of approximately .04 eV to .1 eV. The maximum effective flux level based on polyimide Kapton mass loss is 4.4 x 10 exp 6 atoms/((sq. cm)*s), thus providing a highly accelerated testing capability.

Stidham, Curtis R.↗

Balloon profiles of stratospheric NO2 and HNO3 for testing the heterogeneous hydrolysis of N2O5 on sulfate aerosols

Simultaneous in situ measurements of stratospheric NO2, HNO3, HCl, and CH4 from 34 to 24 km were made in August 1992 from Palestine, Texas, using the Balloon-borne Laser In-Situ Sensor (BLISS) tunable diode laser spectrometer. Although the measurements of NO2, HNO3, and NO2/HNO3 agree well with gas-phase model calculations near 34 km where Stratospheric Aerosol and Gas Experiment (SAGE) 2 data show little sulfate aerosol, this is not true at the lower altitudes where SAGE 2 shows high aerosol loadings. At 24 km the BLISS NO2 and HNO3 measurements are 70% lower and 50% higher, respectively, than the gas phase model predictions, with a measured NO2/HNO3 ratio 5 times smaller. When the heterogeneous hydrolysis of N2O5 and ClONO2 on sulfate aerosol of surface area densities matching the SAGE 2 measurements is added to the model, good agreement with the BLISS measurements is found over the whole altitude range.

Webster, C. R.↗