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Materials science research in microgravity

There are several important attributes of an extended duration microgravity environment that offer a new dimension in the control of the microstructure, processing, and properties of materials. First, when gravitational effects are minimized, buoyancy driven convection flows are also minimized. The flows due to density differences, brought about either by composition or temperature gradients will then be reduced or eliminated to permit a more precise control of the temperature and the composition of a melt which is critical in achieving high quality crystal growth of electronic materials or alloy structures. Secondly, body force effects such as sedimentation, hydrostatic pressure, and deformation are similarly reduced. These effects may interfere with attempts to produce uniformly dispersed or aligned second phases during melt solidification. Thirdly, operating in a microgravity environment will facilitate the containerless processing of melts to eliminate the limitations of containment for reactive melts. The noncontacting forces such as those developed from electromagnet, electrostatic, or acoustic fields can be used to position samples. With this mode of operation, contamination can be minimized to enable the study of reactive melts and to eliminate extraneous crystal nucleation so that novel crystalline structures and new glass compositions may be produced. In order to take advantage of the microgravity environment for materials research, it has become clear that reliable processing models based on a sound ground based experimental experience and an established thermophysical property data base are essential.

Perepezko, John H.↗

Study of surfaces using near infrared optical fiber spectrometry

The measurement and control of cleanliness for critical surfaces during manufacturing and in service provides a unique challenge for fulfillment of environmentally benign operations. Of particular interest has been work performed in maintaining quality in the production of bondline surfaces in propulsion systems and the identification of possible contaminants. This work requires an in-depth study of the possible sources of contamination, methodologies to identify contaminants, discrimination between contaminants and chemical species caused by environment, and the effect of particular contaminants on the bondline integrity of the critical surfaces. This presentation will provide an introduction to the use of optical fiber spectrometry in a nondestructive measurement system for process monitoring and how it can be used to help clarify issues concerning surface chemistry. Correlation of the Near Infrared (NIR) spectroscopic results with Optical Stimulated Electron Emission (OSEE) and ellipsometry will also be presented.

Workman, G. L.↗

An OSEE Based Portable Surface Contamination Monitor

Many industrial and aerospace processes involving the joining of materials, require sufficient surface cleanliness to insure proper bonding. Processes as diverse as painting, welding, or the soldering of electronic circuits will be compromised if prior inspection and removal of surface contaminants is inadequate. As process requirements become more stringent and the number of different materials and identified contaminants increases, various instruments and techniques have been developed for improved inspection. One such technique based on the principle of Optically Stimulated Electron Emission (OSEE) has been explored for a number of years as a tool for surface contamination monitoring. Some of the benefits of OSEE are: it's non-contacting; requires little operator training; and has very high contamination sensitivity. This paper describes the development of a portable OSEE based surface contamination monitor. The instrument is suitable for both hand-held and robotic inspections with either manual or automated control of instrument operation. In addition, instrument output data is visually displayed to the operator and may be output to an external computer for archiving or analysis.

Perey, Daniel F.↗

A Portable Surface Contamination Monitor Based on the Principle of Optically Stimulated Electron Emission (OSEE)

Many industrial and aerospace processes involving the joining of materials, require sufficient surface cleanliness to insure proper bonding. Processes as diverse as painting, welding, or the soldering of electronic circuits will be compromised if prior inspection and removal of surface contaminants is inadequate. As process requirements become more stringent and the number of different materials and identified contaminants increases, various instruments and techniques have been developed for improved inspection. One such technique, based on the principle of Optically Stimulated Electron Emission (OSEE), has been explored for a number of years as a tool for surface contamination monitoring. Some of the benefits of OSEE are: it is non-contacting; requires little operator training; and has very high contamination sensitivity. This paper describes the development of a portable OSEE based surface contamination monitor. The instrument is suitable for both hand-held and robotic inspections with either manual or automated control of instrument operation. In addition, instrument output data is visually displayed to the operator and may be sent to an external computer for archiving or analysis.

Perey, D. F.↗

Genesis Solar Wind – Capture, Return, Curate and Analyze: Looking Backward and Creating a Timeline

Introduction: In 1997 NASA’S Discovery Program selected the Genesis mission proposal to return solar wind samples to Earth for laboratory analyses. Principal Investigator Donald S. Burnett and the science team defined the purity of collector materials and ability to analyze solar wind composition to the precision required for planetary science. As a small mission, focused on a well-defined science goal, yet needing careful attention to engineering details, the communication among scientists and engineers, nurtured by Don Burnett, was exceptional. Genesis Mission and Curation Legacy: Genesis, as the first U. S. spacecraft to return astromaterial samples since Apollo, not only integrated the mission planning and flight teams, but also the science and sample curation teams during the mission development period. Since Genesis is a sample return mission, the Science Team was essential in certifying the collectors (sample containers for solar atoms). From inception, Genesis established mission funding for returned sample curation. JSC was lead in contamination control during mission preparation, including establishment of an ISO 4 cleanroom facility and use of ultrapure water (UPW) for cleaning flight hardware (and, as it turned out, for cleaning collectors after the mishap). Reliable, fast communication among scientists, engineers and curators at the hands-on level established deep respect among team members and efficient decision-making. JSC’s 50-years of astromaterial sample curation provided experienced sample processors onsite during recovery in Utah (a deep bench for emergency response). Post-recovery curation included iterative collaboration with science sample users to clean or verify cleanliness of samples. The science legacy from Genesis is addressed by Burnett and Jurewicz, this volume. In The Beginning: After Apollo sample return, Burnett and Marcia Neugebauer at JPL began discussing a solar wind sample return, with Neugebauer arguing that separate collection of solar wind regimes was essential science. By 1992 a solar wind sample return mission was presented at a workshop, and by 1994 a mission was proposed named Suess-Urey. The mission was re-proposed under a new name GENESIS and selected in 1997. Susan Niebur captured the Genesis mission history and stories, from high level management documents and from many interviews with participants [2]. Her account lets readers glimpse personality of participants in quotations from interviews. Need and Scope for Detailed Technical Timeline: A timeline constructed from lower level task documents has been initiated to document the resources and skills actually used, as well as task sequence or concurrency. Timelines for high level mission events are captured in two documents [1] [2] and for detailed re-entry events in [3]. A detailed technical timeline for Genesis mission and curation activities will provide data points for lower level tasks, such as ISO 4 curation facility construction time, preparation for nominal sample field recovery, mishap recovery, and UPW expansion. Changes in technology context 1990-2024: Semiconductor technologies were easily accessible in the U.S.A. (1990-1999), and the Genesis team used those resources for cleanroom design and UPW system expansion. Image documentation was changing from film to digital during cleanroom construction and payload cleaning (1997-2001). Engineering design was done using computer aided design proprietary software, making more difficult the archiving of payload configuration and materials. Email of documents, tracked delivery service and virtual meeting capability greatly improved communication efficiency. Information sources – Pre-launch mission preparation: Examples of mission science, engineering and contamination control are collector purity testing, payload design/fabrication and ISO 4 cleanroom construction. Information on timing of these activities comes from facility readiness reviews, management reviews, shipping documents, procurement documents, test reports, travel documents, laboratory logs, Quality Assurance documents, dates on images, participant notebooks and emails. Information sources – Sample return re-entry and field recovery activities: Information comes from event timelines produced by Mid-Air Recovery team, Lockheed team lead notes and from chase video, JPL Quality Assurance. Information also comes from images and logbooks from UTTR cleanroom operations and from curatorial documents. Information sources – Resulting science and sample cleaning processes: Agendas from the annual gatherings of the science team initially trace testing for collector purity/cleanliness, and after sample recovery, include collector cleaning and cleanliness assessment. Post-recovery documents include curatorial orders and procedures, sample allocation documents and LPSC abstracts. Timeline Objectives: A simple spreadsheet timeline with headers DATE, EVENT, PEOPLE, COMMENT, INFORMATION SOURCE has been initiated and currently has over 90 entries. While this is not definitive historical research, it is a quick look at the evolution of Genesis curation with pointers to documents or people with information. Engineers for future missions may find useful points of comparison for development of facilities. References:[1] Genesis Mission Reference Document, (2011) JPL D-62382.[2] Niebur S. M., edited by Brown D. W. (2023) NASA’s Discovery Program: The First 20 Years of Competitive Planetary Exploration, NASA-SP-2023-4238.[3] Genesis Mishap Investigation Board Report, Vol. 1 (July 2005).

solar wind↗

Does Collection Time Bias the Ecology of Cleanroom Air Samples?

Microbial monitoring of astromaterials collections has taken on increased importance with the return of biologically sensitive samples from the asteroids Ryugu and Bennu and the initiation of the Mars Sample Return Program. Terrestrial bacteria and fungi can alter the mineralogy and organic composition of our collections causing irreversible contamination of pristine samples and increasing the risk of false positives for life detection measurements. NASA has conducted routine microbial monitoring of its existing collections since 20181. Initial monitoring focused on surface samples collected with foam swabs. Although, airborne microbiology is often decoupled from surface microbiology in the built environment2 culture-based air sampling techniques like impactors were not compliant with existing contamination control requirements. Bringing organic rich media, gelatin or liquids into curation cleanrooms presents an unacceptable risk to pristine samples. In 2022 NASA purchased a materials complaint air sampler and began collecting air samples from the cleanrooms in addition to surface samples3. The new instrument uses an electret filter to collect samples that are suitable for cultivating organisms or for direct DNA sequencing. Preliminary DNA sequencing results appeared to indicate that longer sampling times biased the microbial community in favor of hearty, spore-forming bacteria3. We present the results of a study comparing overnight sampling (17 hours) to short (1 hour) sampling of unoccupied curation cleanrooms. The results will help us optimize our monitoring protocols and develop a more detailed inventory of the ecology of astromaterials curation cleanrooms. Methods: We analyzed 72 paired air samples from six different cleanrooms including the meteorite processing lab (ISO 7 equivalent, 16 samples), the lunar lab (ISO 6 equivalent, 10 samples), the stardust lab (ISO 5 equivalent 14 samples), the OSIRIS-REx lab (ISO 5 equivalent, 12 samples), the Hayabusa2 lab (ISO 5 equivalent, 14 samples), and the Genesis lab (ISO 4 equivalent, 6 samples). All the samples were collected with an InnovaPrep Bobcat air sampler operating at a sampling rate of 200 L/min. The sampler operates for 5 minutes out of every 20 minute period. Half of the samples were collected by filtering 3,000L (15 min. of active sampling) of air across an electret filter for one hour. The rest of the samples were collected by filtering approximately 51,000 L air across the filter overnight (~17 hours, 255 min. of active sampling). Cells were eluted from the filter using 6-7 ml of pressurized 0.15% tween 20 in PBS (phosphate buffered saline). This liquid was used to cultivate bacteria according to previously published methods1,4,5 and for DNA extraction and next generation sequencing. DNA was extracted with a Qiagen MagAttract PowerMicrobiome kit6. To identify bacteria and archaea, the 16S rRNA gene was amplified using Earth Microbiome primers for the V4 region 7. The amplified DNA was sequenced on an Illumina MiSeq using a V3 reagent kit. The resulting sequences were processed using DADA2 and QIIME2 as implemented on the EDGE bioinformatics platform8–10. Results: Only two of the 72 samples had no amplifiable DNA. Amplified DNA concentrations ranged from 2.67 – 0.272 ng/µl. The median concentration of amplified DNA for the 1 hour samples was 0.770 ± 0.368 ng/µl. The median concentration of amplified DNA for the overnight samples was 0.877 ± 0.434 ng/µl. On average the overnight samples had slightly more sequences (58,960 vs. 59,456) and ASV’s (amplicon sequence variants) (60 vs 64.5) than the one hour samples, but these differences are not statistically significant. The most abundant ASV in every sample mapped to the genus Cupravidus. ASV’s mapping to the genuses Bacillus, Schlegelella, Thermus, and Staphylococcus were also common. Discussion and Future Work: Alpha diversity statistics like Shannon Entropy and Faith Phylogenetic Diversity are used to describe the diversity of organisms in a single sample. If a longer sampling time was biasing the data, we would expect to see a change in these diversity statistics vs. sample time. However, we did not observe this in our data. The median Shannon entropy was slightly higher for the overnight samples (3.773 vs 3.611) as was the Faith Phylogenetic Diversity (4.042 vs 3.596), but both values were within a standard deviation of each other for the two sampling times (Fig. 1). It is unlikely, that the longer sampling time is introducing bias into our data. We do observe a significant decrease in diversity when comparing the air samples by lab. The Genesis lab (ISO 4 equivalent) has a lower median number of ASV’s (45.5) than the other labs (62). Median values for Shannon Entropy (3.717 vs. 3.430) and Faith Phylogenetic Diversity (3.796 vs. 3.548) are also lower for Genesis, but those values are with one standard deviation of each other for the different sampling times. This is consistent with previous culture-based results suggesting that the environment in cleanrooms tends to select for a core group of organisms capable of surviving under dry, low nutrient, conditions. The presence of the ASV’s mapping to Cupravidus and Thermus in our sequencing blanks and controls suggests that several of the most common organisms in our samples represent contaminants from the reagents used to perform the DNA extractions and sequencing. Further work is needed to identify these contaminants, remove them from our data and recalculate the diversity statistics. This is a systematic error. Therefore, we do not expect removing the sequencing contaminants to change our conclusions. Longer air sample collection times appear to result in slightly higher diversity and do not bias the results towards “hardy” bacteria like spore-formers. Based on these preliminary results we conclude that sampling at least 3,000 liters of air is sufficient to capture the microbial diversity of cleanrooms, and that air samples can also be collected overnight without negatively impacting diversity. These results allow us to be flexible when designing microbial monitoring plans so that they do not interfere with routine lab activity. References: 1. Regberg, A. B. et al. 49th Lunar and Planetary Science Conference (2018). 2. The United States Pharmacopeial Convention. USP General Chapter <1116> (2013). 3. Regberg, A. B., et al. 54th Lunar and Planetary Science Conference (2023). 4. Regberg, A. B. et al. 53rd Lunar and Planetary Science Conference ( 2022). 5. Davis, R. E.,et al. 50th Lunar and Planetary Science Conference (2019). 6. Qiagen. MagAttract® PowerMicrobiome® DNA/RNA EP Kit Handbook. (2018). 7. Walters, W. et al. mSystems 1, (2015). 8. Callahan, B. J. et al. Nat. Methods 13, 581–583 (2016). 9. Hall, M. & Beiko, R. G. Microbiome Analysis: Methods and Protocols113–129 (Springer, 2018). 10. Philipson, C. et al. Bio-Protoc. 7, e2622 (2017).

A. B. Regberg↗

Observations of thermal ion influxes about the space shuttle

Ion mass spectrometer measurements made as part of the University of Iowa's Plasma Diagnostic Package on the STS-3 and Spacelab 2 Space Shuttle missions sampled a variety of ion composition and collected ion current responses to gas emissions from the vehicle. The only other shuttle ion measurements were made by an Air Force Geophysics Laboratory (AFGL) quadrupole spectrometer flown on STS-4. Gas emissions change the distribution of the incoming plasma through scattering and charge transfer processes. A background flux of contaminant ion species (mostly relating to water) always exists in the near vicinity of the shuttle with a magnitude which is dependent on the look direction of the spectrometer but which varies differently with changes in the angle of attack than that of the ambient ions. There is a near shuttle wake cavity in the contaminant ion distributions which has a different spatial configuration than the wake of the ambient ions. Although water dumps produce the most persistent ion perturbations, the sources for ion current modification were best delineated from measurements made when only one or two of the Reaction Control System thrusters fired for a relatively long duration. Contaminant ion perturbations associated with such firings were observed to persist for the order of a second after the cessation of the firings. The dense thruster plumes are efficient collisional, charge exchange barriers to the passage of ambient ions. Collected ion current perturbations were more evident for firings of the rear verniers, whose plumes scatter off projecting surfaces, than for the nose thrusters. The effect of the Vernier firings was found to depend not only on the location and attitude of the spectrometer with respect to the shuttle and thruster plume direction, but also on the orientation of the local magnetic field with respect to the shuttle velocity.

Grebowsky, Joe M.↗

Zeolite crystal growth in space

The growth of large, uniform zeolite crystals in high yield in space can have a major impact on the chemical process industry. Large zeolite crystals will be used to improve basic understanding of adsorption and catalytic mechanisms, and to make zeolite membranes. To grow large zeolites in microgravity, it is necessary to control the nucleation event and fluid motion, and to enhance nutrient transfer. Data is presented that suggests nucleation can be controlled using chemical compounds (e.g., Triethanolamine, for zeolite A), while not adversely effecting growth rate. A three-zone furnace has been designed to perform multiple syntheses concurrently. The operating range of the furnace is 295 K to 473 K. Teflon-lined autoclaves (10 ml liquid volume) have been designed to minimize contamination, reduce wall nucleation, and control mixing of pre-gel solutions on orbit. Zeolite synthesis experiments will be performed on USML-1 in 1992.

Sacco, Albert, Jr.↗

Automated Cryocooler Monitor and Control System

A system was designed to automate cryogenically cooled low-noise amplifier systems used in the NASA Deep Space Network. It automates the entire operation of the system including cool-down, warm-up, and performance monitoring. The system is based on a single-board computer with custom software and hardware to monitor and control the cryogenic operation of the system. The system provides local display and control, and can be operated remotely via a Web interface. The system controller is based on a commercial single-board computer with onboard data acquisition capability. The commercial hardware includes a microprocessor, an LCD (liquid crystal display), seven LED (light emitting diode) displays, a seven-key keypad, an Ethernet interface, 40 digital I/O (input/output) ports, 11 A/D (analog to digital) inputs, four D/A (digital to analog) outputs, and an external relay board to control the high-current devices. The temperature sensors used are commercial silicon diode devices that provide a non-linear voltage output proportional to temperature. The devices are excited with a 10-microamp bias current. The system is capable of monitoring and displaying three temperatures. The vacuum sensors are commercial thermistor devices. The output of the sensors is a non-linear voltage proportional to vacuum pressure in the 1-Torr to 1-millitorr range. Two sensors are used. One measures the vacuum pressure in the cryocooler and the other the pressure at the input to the vacuum pump. The helium pressure sensor is a commercial device that provides a linear voltage output from 1 to 5 volts, corresponding to a gas pressure from 0 to 3.5 MPa (approx. = 500 psig). Control of the vacuum process is accomplished with a commercial electrically operated solenoid valve. A commercial motor starter is used to control the input power of the compressor. The warm-up heaters are commercial power resistors sized to provide the appropriate power for the thermal mass of the particular system, and typically provide 50 watts of heat. There are four basic operating modes. "Cool " mode commands the system to cool to normal operating temperature. "Heat " mode is used to warm the device to a set temperature near room temperature. "Pump " mode is a maintenance function that allows the vacuum system to be operated alone to remove accumulated contaminants from the vacuum area. In "Off " mode, no power is applied to the system.

Britcliffe, Michael J.↗

Microbial reduction of low-crystallinity tripuhyite (FeSbO 4 ): Implications for Sb(V) cycling in contaminated environments

Tripuhyite (FeSbO 4 ) is an important antimony (Sb)-bearing mineral that controls Sb mobility in contaminated environments, yet its structural stability during microbial reduction remains unresolved. Understanding how FeSbO 4 behaves under anoxic conditions is therefore necessary to predict natural Sb cycling. Here, this study examined how an anaerobic microbial community interacts with FeSbO 4 and alters its structural and redox behavior. Across all conditions, FeSbO 4 released measurable Sb(V), demonstrating that the mineral undergoes partial dissolution in anoxic environment even without microbial activity. However, when extensive microbial Fe(III) reduction occurred in the presence of the electron shuttle anthraquinone-2,6-disulfonate (AQDS), the released Sb was re-immobilized. This indicates that microbial reduction processes modulate Sb mobility. Microbial community analysis showed the enrichment of acetate-utilizing Fe(III)-reducing bacteria as key drivers of Fe reduction. Although secondary Fe minerals were not detected, X-ray absorption fine structure measurements and scanning electron microscopy images revealed the formation of an Sb(III)-bearing phase consistent with valentinite (Sb 2 O 3 ) in the AQDS-amended treatment. This transformation suggests that AQDS not only enhances Fe(III) reduction but is also linked to Sb(V) reduction, and facilitates the immobilization of reduced Sb(III) as Sb 2 O 3 . Overall, this work provides the first evidence that FeSbO 4 is susceptible to microbially mediated redox transformations, and that these processes can significantly alter the mobility and speciation of Sb in reducing environments.

Electron transfer mediator↗

Quality Control Algorithms for the Kennedy Space Center 50-Megahertz Doppler Radar Wind Profiler Winds Database

This paper presents the process used by the Marshall Space Flight Center Natural Environments Branch (EV44) to quality control (QC) data from the Kennedy Space Center's 50-MHz Doppler Radar Wind Profiler for use in vehicle wind loads and steering commands. The database has been built to mitigate limitations of using the currently archived databases from weather balloons. The DRWP database contains wind measurements from approximately 2.7-18.6 km altitude at roughly five minute intervals for the August 1997 to December 2009 period of record, and the extensive QC process was designed to remove spurious data from various forms of atmospheric and non-atmospheric artifacts. The QC process is largely based on DRWP literature, but two new algorithms have been developed to remove data contaminated by convection and excessive first guess propagations from the Median Filter First Guess Algorithm. In addition to describing the automated and manual QC process in detail, this paper describes the extent of the data retained. Roughly 58% of all possible wind observations exist in the database, with approximately 100 times as many complete profile sets existing relative to the EV44 balloon databases. This increased sample of near-continuous wind profile measurements may help increase launch availability by reducing the uncertainty of wind changes during launch countdown

Barbre, Robert E., Jr.↗

The Development of Catalysts for Upgrading of Pyrolysis Vapor for Refinery Feedstocks and Intermediates (CRADA Final Report)

Catalytic fast pyrolysis (CFP) is a versatile technology platform to convert biomass into fungible hydrocarbon transportation fuels and chemical co-products. Key technical barriers to reaching this goal include increasing the product yields and achieving the desired fuel properties for gasoline, diesel, and jet range fuels or blendstocks that would be suitable for introduction into existing refinery unit operations. Overcoming these barriers will require durable catalysts that are effective at upgrading and stabilizing biomass pyrolysis vapors. Towards these goals, this CRADA leveraged NREL experience as a leader in biomass pyrolysis research and Johnson Matthey's (JM) experience as a leader in the production of advanced catalytic materials. The scope spanned CFP catalyst development, characterization, multi-scale reaction testing, and computational modeling. CRADA benefits to DOE, Participant, and U.S. Taxpayer: Assists laboratory in achieving programmatic scope, Uses the laboratory’s core competencies. The purpose of this CRADA was to develop and deploy catalysts for biomass CFP to help achieve cost-competitive biofuels and bio-based products. This was accomplished through a close collaboration between biomass conversion researchers at NREL and catalyst development researchers at JM. Summary of Research Results: Focus Area 1. Foundational research on catalytic conversion and deactivation: Key interactions between pyrolysis vapors and heterogeneous catalysts were probed through catalyst characterization, model compound reaction testing, and atomistic-scale computational modeling. Catalyst development focused on multifunctional materials, which include zeolites, oxides, carbides, and nitrides. Computational modeling identified reaction mechanisms and elucidated surface chemistry to test hypotheses regarding mechanisms of deoxygenation, coupling, cracking, dehydration, coke formation, hydrogen transfer, and aromatic ring reactions. This information was used to design multifunctional catalysts to increase product yields, control product selectivity, and reduce deactivation during CFP and downstream processing steps. The results served to increase fundamental understanding of key catalyst attributes and durability features for the upgrading of biomass pyrolysis vapors. Model compound experiments confirmed the importance of metal-acid bifunctionality for the deoxygenation of lignin-derived phenolic species under hydrodeoxygenation conditions. This insight led to the development of catalysts such as Pt/TiO2 and Mo2C, which were confirmed as high-performing materials during subsequent bench-scale experiments using biomass-derived pyrolysis vapors. This focus area also led to the identification of important catalyst deactivation mechanisms associated with the deposition of inorganic contaminants such as potassium. The molecular-level insight from model compound experiments and computational modeling, shown in Figure 1, informed the development of regeneration procedures that have been shown to be effective for restoration of > 90% of initial catalyst activity. This understanding has subsequently been translated to other catalyst systems, including zeolite materials that can be operated without requirements for co-fed hydrogen.

09 BIOMASS FUELS↗

Extrapolation of space weathering processes to other small solar system bodies

A diverse range of processes were invoked as the dominant factor or as important contributory factors in the modification of the optical surface and regolith of the moon. These include impact vitrification by large and small projectiles, solar wind implantation and the reduction of oxidized iron during energetic events, sputtering and crystal lattice damage by energetic cosmic rays, shock metamorphism of minerals, mixing of diverse lithologies by impacts, and contamination by external materials. These processes are also potentially important on the rocky surfaces of other small solar system bodies. For icy bodies, several additional processes are also possible, including formation of complex organic compounds from methane and ammonia-bearing ices by ultraviolet irradiation and the condensation of vapor species to form frost layers in the polar or cooler regions of objects at appropriate heliocentric distances. The lunar case, even when completely understood, will not extend in a simple linear fashion to other small rocky objects, nor will the optical surfaces of those objects all be affected to the same degree by each process. The major factors that will control the relative efficacy of a possible mechanism include the efficiency of ejecta retention and the degree to which the regolith materials experience multiple events (primarily a function of body size, escape velocity, and impactor velocities); the mean duration of typical regolith particle exposure at the optical surface and within reach of the micrometeorite, cosmic ray, solar wind, or UV fluxes (a function of the rate and scale of regolith mixing, production, and removal processes); the incident flux of solar (low energy) cosmic rays, solar wind, or UV radiation (inverse square of heliocentric distance) or of galactic (high energy) cosmic rays (slowly increasing flux with heliocentric distance); and the compositional and mineralogical nature of the surface being affected. In general, those processes that depend upon either the retention of impact ejecta or on the presence of multigenerational regoliths should be substantially less effective on smaller bodies with lower escape velocities. However, there are important exceptions to this generalization. For example, a process that involves the hypervelocity impact of small particles into a fine-grained regolith may be able to effectively retain highly shocked or melted material due to the nature of shock wave propagation in such a heterogeneous material.

Gaffey, M. J.↗

Crossflow membrane filtration system for operando fouling characterization using transmission x-ray scattering

Membrane-based separations are widely used for wastewater treatment due to their low cost and efficiency. However, membrane fouling, which is the unwanted deposition or attachment of contaminants on membrane surfaces and/or within membrane pores, remains a major challenge as it increases the mass transfer resistance and reduces membrane productivity. Membrane fouling is typically probed by macroscopic performance metrics, such as flux decline, and ex situ characterization. However, this does not capture the membrane and fouling layer evolution under operating conditions, potentially masking important mechanisms and nonequilibrium pathways that impact fouling. Here, we present a remotely controlled crossflow membrane system and a custom membrane cell for operando fouling characterization using transmission small/wide angle x-ray scattering (SAXS/WAXS). This approach allows direct observation of the nanoscale changes occurring at the membrane surface during pressurized water treatment processes, enabling a new way to understand the connections between dynamic fouling behaviors and membrane performance. Nanoparticle fouling of porous membranes during ultrafiltration was investigated using operando SAXS, and mineral scaling of reverse osmosis membranes was investigated using operando WAXS. Furthermore, this system allows for tracking membrane fouling in real time and under realistic conditions, providing fundamental physical insights into how water chemistry and operating conditions affect macroscopic membrane performance. Moreover, this system opens the door for future in situ and operando studies, and it serves as a testbed for evaluating novel materials/processes for membrane-based separations.

36 MATERIALS SCIENCE↗

Instrumentation for Examining Microbial Response to Changes In Environmental Pressures

The Automated Adaptive Directed Evolution Chamber (AADEC) is a device that allows operators to generate a micro-scale analog of real world systems that can be used to model the local-scale effects of climate change on microbial ecosystems. The AADEC uses an artificial environment to expose cultures of micro-organisms to environmental pressures, such as UV-C radiation, chemical toxins, and temperature. The AADEC autonomously exposes micro-organisms to selection pressures. This improves upon standard manual laboratory techniques: the process can take place over a longer period of time, involve more stressors, implement real-time adjustments based on the state of the population, and minimize the risk of contamination. We currently use UV-C radiation as the main selection pressure, UV-C is well studied both for its cell and DNA damaging effects as a type of selection pressure and for its related effectiveness as a mutagen; having these functions united makes it a good choice for a proof of concept. The AADEC roadmap includes expansion to different selection pressures, including heavy metal toxicity, temperature, and other forms of radiation.The AADEC uses closed-loop control to feedback the current state of the culture to the AADEC controller that modifies selection pressure intensity during experimentation, in this case culture density and growth rate. Culture density and growth rate are determined by measuring the optical density of the culture using 600 nm light. An array of 600 nm LEDs illuminate the culture and photodiodes are used to measure the shadow on the opposite side of the chamber.Previous experiments showed that we can produce a million fold increase to UV-C radiation over seven iterations. The most recent implements a microfluidic system that can expose cultures to multiple different selection pressures, perform non-survival based selection, and autonomously perform hundreds of exposure cycles. A scalable pump system gives the ability to pump in various different growth media to individual cultures and introduce chemical toxins during experimentation; AADEC can perform freeze and thaw cycles. We improved our baseline characterization by building a custom UV-C exposure hood, a shutter operates on a preset timer allowing the user to set exposure intensity consistently for multiple iterations.

Environment↗

Spaceflight Effect on White Matter Structural Integrity

Recent reports of elevated brain white matter hyperintensity (WMH) counts and volume in postflight astronaut MRIs suggest that further examination of spaceflight's impact on the microstructure of brain white matter is warranted. To this end, retrospective longitudinal diffusion-weighted MRI scans obtained from 15 astronauts were evaluated. In light of the recent reports of microgravity-induced cephalad fluid shift and gray matter atrophy seen in astronauts, we applied a technique to estimate diffusion tensor imaging (DTI) metrics corrected for free water contamination. This approach enabled the analysis of white matter tissue-specific alterations that are unrelated to fluid shifts, occurring from before spaceflight to after landing. After spaceflight, decreased fractional anisotropy (FA) values were detected in an area encompassing the superior and inferior longitudinal fasciculi and the inferior fronto-occipital fasciculus. Increased radial diffusivity (RD) and decreased axial diffusivity (AD) were also detected within overlapping regions. In addition, FA values in the corticospinal tract decreased and RD measures in the precentral gyrus white matter increased from before to after flight. The results show disrupted structural connectivity of white matter in tracts involved in visuospatial processing, vestibular function, and movement control as a result of spaceflight. The findings may help us understand the structural underpinnings of the extensive spaceflight-induced sensorimotor remodeling. Prospective longitudinal assessment of the white matter integrity in astronauts is needed to characterize the evolution of white matter microstructural changes associated with spaceflight, their behavioral consequences, and the time course of recovery. Supported by a grant from the National Space Biomedical Research Institute, NASA NCC 9-58.

Lee, Jessica K.↗

Major Effects of Nonmetallic Inclusions on the Fatigue Life of Disk Superalloy Demonstrated

The fatigue properties of modern powder metallurgy disk alloys can vary because of the different steps of materials and component processing and machining. Among these variables, the effects of nonmetallic inclusions introduced during the powder atomization and handling processes have been shown to significantly degrade low-cycle fatigue life. The levels of inclusion contamination have, therefore, been reduced to less than 1 part per million in state-of-the-art nickel disk powder-processing facilities. Yet the large quantities of compressor and turbine disks weighing from 100 to over 1000 lb have enough total volume and surface area for these rare inclusions to still be present and limit fatigue life. The objective of this study was to investigate the effects on fatigue life of these inclusions, as part of the Crack Resistant Disk Materials task within the Ultra Safe Propulsion Project. Inclusions were carefully introduced at elevated levels in a nickel-base disk superalloy, U720, produced using powder metallurgy processing. Multiple strain-controlled fatigue tests were then performed on extracted test specimens at 650 C. Analyses were performed to compare the low-cycle fatigue lives and failure initiation sites as functions of inclusion content and fatigue conditions. Powder of the nickel-base superalloy U720 was atomized in argon at Special Metals Corporation, Inc., using production-scale high-cleanliness powder-processing facilities and handling practices. The powder was then passed through a 270-mesh screen. One portion of this powder was set aside for subsequent consolidation without introduced inclusions. Two other portions of this powder were seeded with alumina inclusions. Small, polycrystalline soft (Type 2) inclusions of about 50 mm diameter were carefully prepared and blended into one powder lot, and larger hard (Type 1) inclusions of about 150 mm mean diameter were introduced into the other seeded portion of powder. All three portions of powder were then sealed in separate containers, hot isostatically pressurized, extruded, forged into subscale disks, and heat treated. Low-cycle-fatigue specimens were then extracted, machined, and tested. Fatigue tests were performed at 650 C in closed-loop servohydraulic testing machines using induction heating and axial extensometers. All tests were continued to failure, and fractographic evaluations were performed on all specimens to determine the crack initiation sites. A large majority of the failures in specimens with introduced inclusions occurred at cracks initiating from inclusions at the specimen surface, as shown for each type of inclusion in the following bar chart. The inclusions significantly reduced fatigue life from unseeded material levels, as shown in the bar chart. These effects were found to depend on the strain range, strain ratio, and inclusion size. Tests at lower strain ranges and higher strain ratios resulted in larger effects of inclusions on life. Inclusion effects on life were thereby maximized in tests at the lowest strain range of 0.6 percent and the most positive strain ratio of 0.5. Under these conditions, small Type 2 inclusions reduced life substantially-- about 20 times, whereas large Type 1 inclusions dramatically reduced life 100 times. These results clearly demonstrate that it is essential to include the effects of inclusions for realistic predictions of disk fatigue life. Important issues, including temperature dependence, crack initiation versus propagation, surface treatments, realistic disk features and machining, and realistic disk spin testing will be addressed to accurately model inclusion effects on disk fatigue life. Fatigue life varied from well over 105 cycles for no inclusions to a little over 103 cycles for 100-micrometer inclusions. A single crack initiating at a surface-connected seeded inclusion caused failure in each case.

Gabb, Timothy P.↗

Uncooled tunneling infrared sensor

An uncooled infrared tunneling sensor in which the only moving part is a diaphragm which is deflected into contact with a micromachined silicon tip electrode prepared by a novel lithographic process. Similarly prepared deflection electrodes employ electrostatic force to control the deflection of a silicon nitride, flat diaphragm membrane. The diaphragm exhibits a high resonant frequency which reduces the sensor's sensitivity to vibration. A high bandwidth feedback circuit controls the tunneling current by adjusting the deflection voltage to maintain a constant deflection of the membrane. The resulting infrared sensor can be miniaturized to pixel dimensions smaller than 100 .mu.m. An alternative embodiment is implemented using a corrugated membrane to permit large deflection without complicated clamping and high deflection voltages. The alternative embodiment also employs a pinhole aperture in a membrane to accommodate environmental temperature variation and a sealed chamber to eliminate environmental contamination of the tunneling electrodes and undesireable accoustic coupling to the sensor.

Kenny, Thomas W.↗