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All sourcesNASA NTRSDOE OSTI
NASA NTRS2013

Anti-Icing Formulas Prevent Train Delays

In the winter of 2009, Washington, DC, workers faced the prospect of a difficult commute due to record-setting snowfalls. But thousands of the city's Metrorail riders found the public transportation system fully functional, thanks in part to a NASA technology invented years before. Just like trains, an airplane must be snow- and ice-free to ensure safe travel. Traditionally, fluids containing a compound called ethylene glycol have been used to inhibit ice on planes. In 1992, however, the US Air Force banned its purchase of this ingredient due to toxicity concerns. According to the Centers for Disease Control, exposure to large amounts of ethylene glycol through air or water can damage the kidneys, nervous system, lungs, and heart. Urine samples from airport deicing workers have contained traces of the substance. At the time of the Air Force s ban, Robert Lockyer was working at NASA s Ames Research Center in the Advanced Composites Model Development Branch, where he says "we decided to pick up the gauntlet and began researching existing fluid compositions and the processes used in deicing aircraft." Along with Lockyer, in 1997 Ames researchers Leonard Haslim and John Zuk devised a nontoxic, biodegradable, and cost effective substitute for ethylene glycol. When applied to a dry surface before a snow or ice event, the solution prevented ice from forming a bond with the surface. This made it easy to wipe away any accumulation.

Source record↗
DOE OSTI2018

Handling and Treatment of Sodium-Potassium Alloy (NaK) after the Loss of Key Personnel – 19002

ABSTRACT In September 2010, during cleanup and removal efforts associated with a glovebox containing a sodium-potassium alloy (NaK) cooling system, a NaK reaction event occurred. Near the end of the evolution, which was at a Materials and Fuels Complex (MFC) research facility at the Idaho National Laboratory, a 2 to 3-ounce sample of NaK was being transferred from a metal can to a polyethylene bottle so it could be sent to the disposal outlet for verification analysis. During the transfer, a reaction of the NaK with ambient air was observed in both the metal can and sample container. The potential for a reaction was identified during the planning of this activity and mitigating steps were included in the procedures. In response, the two containers were flooded with argon, closed, and observed overnight. No additional reaction was noted. The sample container and metal can were packaged into a 10-gallon drum and transferred to a permitted storage location pending disposal. While the other containers generated from the deactivation and decommissioning activity were sent off-site for disposal, the 10-gal drum remained due to concerns by a staff specialist that the material could contain potassium superoxide (KO2) as a result of the reaction event. The intent at that time was to treat the NaK in a Resource Conservation and Recovery Act (RCRA)-permitted treatment facility at MFC, instead of sending it off-site for disposal. The container was labeled, inspected, and managed as a hazardous waste. Due to the complexities associated with safely handling and treating NaK and KO2, the container remained in storage. Treatment and disposal of the NaK and KO2 container was revisited in 2016, when researchers and chemists were consulted regarding the potential for superoxide formation and the best means to safely store and treat the container. The facility came to realize that due to the retirements of key personnel, it needed to provide current employees operational experience with the handling and treatment of NaK. An outside company was identified and contracted to provide training and consulting services. Several Battelle Energy Alliance, Inc. (BEA) personnel then attended an alkali metals safety training class. The training course provided participants with classroom and hands–on instruction associated with: • Hazards associated with handling and using sodium and NaK • Proper personal protection equipment, spill control techniques, and first aid • Common design approaches for buildings, systems, and equipment used to contain sodium and NaK • What to expect in the event of a water reaction and how to respond • How to properly prepare for a fire and contain/extinguish small metal fires • A hands-on demonstration of NaK reaction and controls. Following the training, a procedure was developed to open the container, and inspect and treat the NaK. In June 2017, facility operations personnel successfully completed the inspection and treatment of the NaK drum, eliminating the legacy liability.

99 GENERAL AND MISCELLANEOUS↗
DOE OSTI2019

Handling and Treatment of Sodium-Potassium Alloy (NaK) after the Loss of Key Personnel - 19002

In September 2010, during cleanup and removal efforts associated with a glovebox containing a sodium-potassium alloy (NaK) cooling system, a NaK reaction event occurred. Near the end of the evolution, which was at a Materials and Fuels Complex (MFC) research facility at the Idaho National Laboratory, a 2 to 3-ounce sample of NaK was being transferred from a metal can to a polyethylene bottle so it could be sent to the disposal outlet for verification analysis. During the transfer, a reaction of the NaK with ambient air was observed in both the metal can and sample container. The potential for a reaction was identified during the planning of this activity and mitigating steps were included in the procedures. In response, the two containers were flooded with argon, closed, and observed overnight. No additional reaction was noted. The sample container and metal can were packaged into a 10-gallon drum and transferred to a permitted storage location pending disposal. While the other containers generated from the deactivation and decommissioning activity were sent off-site for disposal, the 10-gal drum remained due to concerns by a staff specialist that the material could contain potassium superoxide (KO{sub 2}) as a result of the reaction event. The intent at that time was to treat the NaK in a Resource Conservation and Recovery Act (RCRA)-permitted treatment facility at MFC, instead of sending it off-site for disposal. The container was labeled, inspected, and managed as a hazardous waste. Due to the complexities associated with safely handling and treating NaK and KO{sub 2}, the container remained in storage. Treatment and disposal of the NaK and KO{sub 2} container was revisited in 2016, when researchers and chemists were consulted regarding the potential for superoxide formation and the best means to safely store and treat the container. The facility came to realize that due to the retirements of key personnel, it needed to provide current employees operational experience with the handling and treatment of NaK. An outside company was identified and contracted to provide training and consulting services. Several Battelle Energy Alliance, Inc. (BEA) personnel then attended an alkali metals safety training class. The training course provided participants with classroom and hands-on instruction associated with: - Hazards associated with handling and using sodium and NaK; - Proper personal protection equipment, spill control techniques, and first aid; - Common design approaches for buildings, systems, and equipment used to contain sodium and NaK; - What to expect in the event of a water reaction and how to respond; - How to properly prepare for a fire and contain/extinguish small metal fires; - A hands-on demonstration of NaK reaction and controls. Following the training, a procedure was developed to open the container, and inspect and treat the NaK. In June 2017, facility operations personnel successfully completed the inspection and treatment of the NaK drum, eliminating the legacy liability. (authors)

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2018

Ferromagnetism and Persistent Currents in Finely Dispersed Highly Oriented Pyrolytic Graphite Samples

Synthesis of finely dispersed graphite powders is described and results of their investigations by the methods of electron microscopy and magnetometry are presented. The samples have been prepared from crystal highly oriented pyrolytic graphite by grinding in an inert atmosphere for a long time with subsequent annealing at 400°C for 24 h in air or in vacuum. It is demonstrated that annealing of the powder in vacuum leads to a considerable increase in the ferromagnetic component associated with the formation of edge defects of zigzag type. The phenomenon of magnetic flux trapping is manifested in the samples annealed both in air and in vacuum upon cooling down to 10 K in a magnetic field that is indicative of the formation of superconducting regions in the samples.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2018

The Fifth International Workshop on Ice Nucleation phase 2 (FIN-02): laboratory intercomparison of ice nucleation measurements

Abstract. The second phase of the Fifth International Ice Nucleation Workshop (FIN-02)involved the gathering of a large number of researchers at the KarlsruheInstitute of Technology's Aerosol Interactions and Dynamics of the Atmosphere(AIDA) facility to promote characterization and understanding of icenucleation measurements made by a variety of methods used worldwide.Compared to the previous workshop in 2007, participation was doubled,reflecting a vibrant research area. Experimental methods involved sampling ofaerosol particles by direct processing ice nucleation measuring systems fromthe same volume of air in separate experiments using different ice nucleatingparticle (INP) types, and collections of aerosol particle samples ontofilters or into liquid for sharing amongst measurement techniques thatpost-process these samples. In this manner, any errors introduced bydifferences in generation methods when samples are shared across laboratorieswere mitigated. Furthermore, as much as possible, aerosol particle sizedistribution was controlled so that the size limitations of different methodswere minimized. The results presented here use data from the workshop toassess the comparability of immersion freezing measurement methods activatingINPs in bulk suspensions, methods that activate INPs in condensation and/orimmersion freezing modes as single particles on a substrate, continuous flowdiffusion chambers (CFDCs) directly sampling and processing particles wellabove water saturation to maximize immersion and subsequent freezing ofaerosol particles, and expansion cloud chamber simulations in which liquidcloud droplets were first activated on aerosol particles prior to freezing.The AIDA expansion chamber measurements are expected to be the closestrepresentation to INP activation in atmospheric cloud parcels in thesecomparisons, due to exposing particles freely to adiabatic cooling. The different particle types used as INPs included the minerals illite NX andpotassium feldspar (K-feldspar), two natural soil dusts representative of arable sandy loam(Argentina) and highly erodible sandy dryland (Tunisia) soils, respectively,and a bacterial INP (Snomax ® ). Consideredtogether, the agreement among post-processed immersion freezing measurementsof the numbers and fractions of particles active at different temperaturesfollowing bulk collection of particles into liquid was excellent, withpossible temperature uncertainties inferred to be a key factor in determiningINP uncertainties. Collection onto filters for rinsing versus directly intoliquid in impingers made little difference. For methods that activatedcollected single particles on a substrate at a controlled humidity at orabove water saturation, agreement with immersion freezing methods was good inmost cases, but was biased low in a few others for reasons that have not beenresolved, but could relate to water vapor competition effects. AmongstCFDC-style instruments, various factors requiring (variable) highersupersaturations to achieve equivalent immersion freezing activation dominatethe uncertainty between these measurements, and for comparison with bulkimmersion freezing methods. When operated above water saturation to includeassessment of immersion freezing, CFDC measurements often measured at orabove the upper bound of immersion freezing device measurements, but oftenunderestimated INP concentration in comparison to an immersion freezingmethod that first activates all particles into liquid droplets prior tocooling (the PIMCA-PINC device, or Portable Immersion Mode Cooling chAmber–Portable Ice Nucleation Chamber), and typically slightly underestimated INPnumber concentrations in comparison to cloud parcel expansions in the AIDAchamber; this can be largely mitigated when it is possible to raise therelative humidity to sufficiently high values in the CFDCs, although this isnot always possible operationally. Correspondence of measurements of INPs among direct sampling andpost-processing systems varied depending on the INP type. Agreement was bestfor Snomax ® particles in the temperature regimecolder than −10 ∘ C, where their ice nucleation activity is nearlymaximized and changes very little with temperature. At temperatures warmer than −10 ∘ C, Snomax ® INP measurements (allvia freezing of suspensions) demonstrated discrepancies consistent withprevious reports of the instability of its protein aggregates that appear tomake it less suitable as a calibration INP at these temperatures. ForArgentinian soil dust particles, there was excellent agreement across allmeasurement methods; measures ranged within 1 order of magnitude for INPnumber concentrations, active fractions and calculated active site densitiesover a 25 to 30 ∘ C range and 5 to 8 orders of correspondingmagnitude change in number concentrations. This was also the case for alltemperatures warmer than −25 ∘ C in Tunisian dust experiments. Incontrast, discrepancies in measurements of INP concentrations or active sitedensities that exceeded 2 orders of magnitude across a broad range of temperaturemeasurements found at temperatures warmer than −25 ∘ C in a previous study werereplicated for illite NX. Discrepancies also exceeded 2 orders of magnitude attemperatures of −20 to −25 ∘ C for potassium feldspar (K-feldspar), but these coincidedwith the range of temperatures at which INP concentrations increase rapidly atapproximately an order of magnitude per 2 ∘ C cooling forK-feldspar. These few discrepancies did not outweigh the overall positive outcomes of theworkshop activity, nor the future utility of this data set or future similarefforts for resolving remaining measurement issues. Measurements of the samematerials were repeatable over the time of the workshop and demonstratedstrong consistency with prior studies, as reflected by agreement of databroadly with parameterizations of different specific or general (e.g., soildust) aerosol types. The divergent measurements of the INP activity of illiteNX by direct versus post-processing methods were not repeated for otherparticle types, and the Snomax ® datademonstrated that, at least for a biological INP type, there is no expectedmeasurement bias between bulk collection and direct immediately processedfreezing methods to as warm as −10 ∘ C. Since particle size rangeswere limited for this workshop, it can be expected that for atmosphericpopulations of INPs, measurement discrepancies will appear due to thedifferent capabilities of methods for sampling the full aerosol sizedistribution, or due to limitations on achieving sufficient watersupersaturations to fully capture immersion freezing in direct processinginstruments. Overall, this workshop presents an improved picture of presentcapabilities for measuring INPs than in past workshops, and providesdirection toward addressing remaining measurement issues.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2014

A solvent replenishment solution for managing evaporation of biochemical reactions in air-matrix digital microfluidics devices

Digital microfluidics (DMF) is a powerful technique for sample preparation and analysis for a broad range of biological and chemical applications. In many cases, it is desirable to carry out DMF on an open surface, such that the matrix surrounding the droplets is ambient air. However, the utility of the air-matrix DMF format has been severely limited by problems with droplet evaporation, especially when the droplet-based biochemical reactions require high temperatures for long periods of time. We present a simple solution for managing evaporation in air-matrix DMF: just-in-time replenishment of the reaction volume using droplets of solvent. We demonstrate that this solution enables DMF-mediated execution of several different biochemical reactions (RNA fragmentation, first-strand cDNA synthesis, and PCR) over a range of temperatures (4–95 °C) and incubation times (up to 1 h or more) without use of oil, humidifying chambers, or off-chip heating modules. Reaction volumes and temperatures were maintained roughly constant over the course of each experiment, such that the reaction kinetics and products generated by the air-matrix DMF device were comparable to those of conventional benchscale reactions. As a result, this simple yet effective solution for evaporation management is an important advance in developing air-matrix DMF for a wide variety of new, high-impact applications, particularly in the biomedical sciences.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS2008

The NASA MSFC Earth Global Reference Atmospheric Model-2007 Version

Reference or standard atmospheric models have long been used for design and mission planning of various aerospace systems. The NASA/Marshall Space Flight Center (MSFC) Global Reference Atmospheric Model (GRAM) was developed in response to the need for a design reference atmosphere that provides complete global geographical variability, and complete altitude coverage (surface to orbital altitudes) as well as complete seasonal and monthly variability of the thermodynamic variables and wind components. A unique feature of GRAM is that, addition to providing the geographical, height, and monthly variation of the mean atmospheric state, it includes the ability to simulate spatial and temporal perturbations in these atmospheric parameters (e.g. fluctuations due to turbulence and other atmospheric perturbation phenomena). A summary comparing GRAM features to characteristics and features of other reference or standard atmospheric models, can be found Guide to Reference and Standard Atmosphere Models. The original GRAM has undergone a series of improvements over the years with recent additions and changes. The software program is called Earth-GRAM2007 to distinguish it from similar programs for other bodies (e.g. Mars, Venus, Neptune, and Titan). However, in order to make this Technical Memorandum (TM) more readable, the software will be referred to simply as GRAM07 or GRAM unless additional clarity is needed. Section 1 provides an overview of the basic features of GRAM07 including the newly added features. Section 2 provides a more detailed description of GRAM07 and how the model output generated. Section 3 presents sample results. Appendices A and B describe the Global Upper Air Climatic Atlas (GUACA) data and the Global Gridded Air Statistics (GGUAS) database. Appendix C provides instructions for compiling and running GRAM07. Appendix D gives a description of the required NAMELIST format input. Appendix E gives sample output. Appendix F provides a list of available parameters to enable the user to generate special output. Appendix G gives an example and guidance on incorporating GRAM07 as a subroutine in other programs such as trajectory codes or orbital propagation routines.

Leslie, F.W.↗
DOE OSTI2017

Pt-TiO{sub 2} microspheres with exposed {001} facets for degradation of formaldehyde in air: Formation mechanism and enhanced visible light photocatalytic activity

Highlights: • TiO{sub 2} microspheres with exposed {001} facets were successfully synthesized. • Pt-TiO{sub 2} catalyst combined the properties of Pt nanoparticles and TiO{sub 2} {001} facet. • The catalyst exhibited an enhanced visible-light photocatalytic activity. • The formation mechanism of TiO{sub 2} microspheres with exposed {001} facets was studied. - Abstract: In this study, TiO{sub 2} microspheres with exposed {001} facets were successfully synthesized by a low-temperature hydrothermal method without using any organic solvents as morphology controlling agent. Furthermore, an active Pt-TiO{sub 2} catalyst was prepared by impregnation and deposition-precipitation methods with reduction processes. The photocatalytic activity of the samples was evaluated by degradation of formaldehyde in air under visible light irradiation at room temperature. After modification with Pt, the optical absorption property of the Pt-TiO{sub 2} microspheres was extended to visible light range. More importantly, the Pt-TiO{sub 2} microspheres exhibited excellent photocatalytic performance for formaldehyde degradation under visible light irradiation, being superior to pure TiO{sub 2} microspheres and even Pt-P25. The formation mechanism of the TiO{sub 2} microspheres with exposed {001} facets was studied. Moreover, the proper photocatalytic mechanism was also proposed. This work provided new insight into the improvement of photocatalytic activity by special high-energy facet exposing and noble metal depositing.

36 MATERIALS SCIENCE↗
NASA NTRS1999

3-D Surface Depression Profiling Using High Frequency Focused Air-Coupled Ultrasonic Pulses

Surface topography is an important variable in the performance of many industrial components and is normally measured with diamond-tip profilometry over a small area or using optical scattering methods for larger area measurement. This article shows quantitative surface topography profiles as obtained using only high-frequency focused air-coupled ultrasonic pulses. The profiles were obtained using a profiling system developed by NASA Glenn Research Center and Sonix, Inc (via a formal cooperative agreement). (The air transducers are available as off-the-shelf items from several companies.) The method is simple and reproducible because it relies mainly on knowledge and constancy of the sound velocity through the air. The air transducer is scanned across the surface and sends pulses to the sample surface where they are reflected back from the surface along the same path as the incident wave. Time-of-flight images of the sample surface are acquired and converted to depth/surface profile images using the simple relation (d = V*t/2) between distance (d), time-of-flight (t), and the velocity of sound in air (V). The system has the ability to resolve surface depression variations as small as 25 microns, is useable over a 1.4 mm vertical depth range, and can profile large areas only limited by the scan limits of the particular ultrasonic system. (Best-case depth resolution is 0.25 microns which may be achievable with improved isolation from vibration and air currents.) The method using an optimized configuration is reasonably rapid and has all quantitative analysis facilities on-line including 2-D and 3-D visualization capability, extreme value filtering (for faulty data), and leveling capability. Air-coupled surface profilometry is applicable to plate-like and curved samples. In this article, results are shown for several proof-of-concept samples, plastic samples burned in microgravity on the STS-54 space shuttle mission, and a partially-coated cylindrical ceramic composite sample. Impressive results were obtained for all samples when compared with diamond-tip profiles and measurements from micrometers. The method is completely nondestructive, noninvasive, non-contact and does not require light-reflective surfaces.

Roth, Don J.↗
DOE OSTI2012

Relaxations in Ba{sub 2}BiTaO{sub 6} ceramics investigated by impedance and electric modulus spectroscopies

Highlights: Black-Right-Pointing-Pointer We have confirmed that the relaxation observed in Ba{sub 2}BiTaO{sub 6} is due to the conduction mechanism. Black-Right-Pointing-Pointer The conduction mechanism is the oxygen vacancies hopping. Black-Right-Pointing-Pointer We have explained because the activation energy for the Ba{sub 2}BiTaO{sub 6} is lower than observed for Ba{sub 2}BiSbO{sub 6} with basis in zero-point energy of both materials. Black-Right-Pointing-Pointer We have showed that a minor secondary phase is a minor secondary phase, which is common when the BBTO is obtained by ceramic method under air, does not change significantly the electrical properties of BBTO. -- Abstract: Impedance spectroscopy analysis of the dielectric properties of a Ba{sub 2}BiTaO{sub 6} ceramic was performed in the temperature range from room temperature to 500 K. The sample was prepared using conventional solid state synthesis under air and the X-ray diffraction shows the presence of Ba{sub 5}Ta{sub 4}O{sub 15} as a minor secondary phase (0.09%). The impedance data clearly show contributions of the grain and grain boundary. The results indicate that the conduction in Ba{sub 2}BiTaO{sub 6} is due to hopping of oxygen vacancies and that the impurities not influence the conduction mechanism.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Cu-Cu direct bonding achieved by surface method at room temperature

The metal bonding is a key technology in the processes for the microelectromechanical systems (MEMS) devices and the semiconductor devices to improve functionality and higher density integration. Strong adhesion between surfaces at the atomic level is crucial; however, it is difficult to achieve close bonding in such a system. Cu films were deposited on Si substrates by vacuum deposition, and then, two Cu films were bonded directly by means of surface activated bonding (SAB) at room temperature. The two Cu films, with the surface roughness Ra about 1.3nm, were bonded by using SAB at room temperature, however, the bonding strength was very weak in this method. In order to improve the bonding strength between the Cu films, samples were annealed at low temperatures, between 323 and 473 K, in air. As the result, the Cu-Cu bonding strength was 10 times higher than that of the original samples without annealing.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2016

Electrical properties from photoinduced charging on Cd-doped (100) surfaces of CuInSe{sub 2} epitaxial thin films

The photoresponse of Cd-doped CuInSe{sub 2} (CIS) epitaxial thin films on GaAs(100) was studied using x-ray photoelectron spectroscopy under illumination from a 532 nm laser between sample temperatures of 28–260 °C. The initial, air-exposed surface shows little to no photoresponse in the photoelectron binding energies, the Auger electron kinetic energies or peak shapes. Heating between 50 and 130 °C in the analysis chamber results in enhanced n-type doping at the surface and an increased light-induced binding energy shift, the magnitude of which persists when the samples are cooled to room temperature from 130 °C but which disappears when cooling from 260 °C. Extra negative charge trapped on the Cu and Se atoms indicates deep trap states that dissociate after cooling from 260 °C. Analysis of the Cd modified Auger parameter under illumination gives experimental verification of electron charging on Cd atoms thought to be shallow donors in CIS. The electron charging under illumination disappears at 130 °C but occurs again when the sample is cooled to room temperature.

42 ENGINEERING↗
DOE OSTI2015

Al capping layers for nondestructive x-ray photoelectron spectroscopy analyses of transition-metal nitride thin films

X-ray photoelectron spectroscopy (XPS) compositional analyses of materials that have been air exposed typically require ion etching in order to remove contaminated surface layers. However, the etching step can lead to changes in sample surface and near-surface compositions due to preferential elemental sputter ejection and forward recoil implantation; this is a particular problem for metal/gas compounds and alloys such as nitrides and oxides. Here, the authors use TiN as a model system and compare XPS analysis results from three sets of polycrystalline TiN/Si(001) films deposited by reactive magnetron sputtering in a separate vacuum chamber. The films are either (1) air-exposed for ≤10 min prior to insertion into the ultrahigh-vacuum (UHV) XPS system; (2) air-exposed and subject to ion etching, using different ion energies and beam incidence angles, in the XPS chamber prior to analysis; or (3) Al-capped in-situ in the deposition system prior to air-exposure and loading into the XPS instrument. The authors show that thin, 1.5–6.0 nm, Al capping layers provide effective barriers to oxidation and contamination of TiN surfaces, thus allowing nondestructive acquisition of high-resolution core-level spectra representative of clean samples, and, hence, correct bonding assignments. The Ti 2p and N 1s satellite features, which are sensitive to ion bombardment, exhibit high intensities comparable to those obtained from single-crystal TiN/MgO(001) films grown and analyzed in-situ in a UHV XPS system and there is no indication of Al/TiN interfacial reactions. XPS-determined N/Ti concentrations acquired from Al/TiN samples agree very well with Rutherford backscattering and elastic recoil analysis results while ion-etched air-exposed samples exhibit strong N loss due to preferential resputtering. The intensities and shapes of the Ti 2p and N 1s core level signals from Al/TiN/Si(001) samples do not change following long-term (up to 70 days) exposure to ambient conditions, indicating that the thin Al capping layers provide stable surface passivation without spallation.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Cloud condensation nuclei activity of internally mixed particle populations at a remote marine free troposphere site in the North Atlantic Ocean

Here, this study reports results from research conducted at the Observatory of Mount Pico (OMP), 2225 m above mean sea level on Pico Island in the Azores archipelago in June and July 2017. We investigated the chemical composition, mixing state, and cloud condensation nuclei (CCN) activities of long-range transported free tropospheric (FT) particles. FLEXible PARTicle Lagrangian particle dispersion model (FLEXPART) simulations reveal that most air masses that arrived at the OMP during the sampling period originated in North America and were highly aged (average plume age > 10 days). We probed size-resolved chemical composition, mixing state, and hygroscopicity parameter ($\mathcal{κ}$) of individual particles using computer-controlled scanning electron microscopy with an energy-dispersive X-ray spectrometer (CCSEM-EDX). Based on the estimated individual particle mass from elemental composition, we calculated the mixing state index, $χ$. During our study, FT particle populations were internally mixed ($χ$ of samples are between 53% and 87%), owing to the long atmospheric aging time. We used data from a miniature Cloud Condensation Nucleus Counter (miniCCNC) to derive the hygroscopicity parameter, $\mathcal{κ}$ CCNC . Combining $\mathcal{κ}$ CCNC and FLEXPART, we found that air masses recirculated above the North Atlantic Ocean with lower mean altitude had higher $\mathcal{κ}$ CCNC due to the higher contribution of sea salt particles. We used CCSEM-EDX and phase state measurements to predict single-particle $\mathcal{κ}$ ($\mathcal{κ}$ CCSEM-EDX ) values, which overlap with the lower range of $\mathcal{κ}$ CCNC measured below 0.15 % SS. Therefore, CCSEM-EDX measurements can be useful in predicting the lower bound of $\mathcal{κ}$, which can be used in climate models to predict CCN activities, especially in remote locations where online CCN measurements are unavailable.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2013

Saltstone Oxidation Study: Leaching Method

Cementitious waste forms can be designed to chemically stabilize selected contaminants, such as Tc{sup +7} and Cr{sup +6}, by chemically reduction to lower valance states, Tc{sup +4} and Cr{sup +3}, respectively, and precipitation of these species in alkaline media as low solubility solid phases. Data for oxidation of this type of cementitious waste form cured under field conditions as a function of time is required for predicting the performance of the waste form and disposal facility. The rate of oxidation (oxidation front advancement) is an important parameter for predicting performance because the solubilities of some radionuclide contaminants, e.g., technetium, are a function of the oxidation state. A non-radioactive experiment was designed for quantifying the oxidation front advancement using chromium, as an approximate redox-sensitive surrogate (Cr{sup +6} / Cr{sup +3}) for technetium (Tc{sup +7} / Tc{sup +4}). Nonradioactive cementitious waste forms were prepared in the laboratory and cured under both laboratory and ?field conditions.? Laboratory conditions were ambient temperature and sealed sample containers. Field conditions were approximated by curing samples in open containers which were placed inside a plastic container stored outdoors at SRS. The container had a lid and was instrumented with temperature and humidity probes. Subsamples as thin as 0.2 mm were taken as a function of distance from the exposed surface of the as-cast sample. The subsamples were leached and the leachates were analyzed for chromium, nitrate, nitrite and sodium. Nitrate, nitrite, and sodium concentrations were used to provide baseline data because these species are not chemically retained in the waste form matrix to any significant extent and are not redox sensitive. ?Effective? oxidation fronts for Cr were measured for samples containing 1000, 500 and 20 mg/kg Cr added as soluble sodium chromate, Na{sub 2}CrO{sub 4}. For a sample cured for 129 days under field conditions, leachable Cr (assumed to be the oxidized form, i.e., Cr{sup +6} was detected in the top 15 to 20 mm of the sample spiked with 1000 mg/kg Cr. Below about 20 mm, the Cr concentrations in leachates were below the detection limit (< 0.010 mg/L) which indicates that the oxidation as the result of exposure to air was limited to the top 20 mm of the sample after exposure for 129 days and that the bulk of the waste form was not affected, i.e., the Cr was stabilized and insoluble. For samples cured in the laboratory, leachable Cr was detected in the top 8 mm of the Cr 1000 sample cured in the laboratory for 37 days. Between 8 and 14 mm, the concentration Cr in the leachate dropped by a factor of about 20 to just above the detection limit. These depth of penetration results indicate that the rate of advancement of the oxidation front for samples spiked with 1000 mg/kg Cr cured under ?field conditions? for 129 days is less than that for the sample cured in the laboratory for 37 days, i.e., 0.156 and 0.216 mm/day, respectively. Additional data are presented for samples spiked with 500 and 20 mg/kg Cr. In summary, cementitious waste forms are porous solids with a network of interconnected pores ranging in diameter from 10E-10 m to greater than a few mm. The oxidation process is assumed to occur as the result of oxygen transport through the interconnected porosity which may be filled with air, aqueous salt solution, or both. Upon oxidation, the Cr becomes soluble and can be transported in solution through aqueous pore fluid or leachate.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2014

Dry-cleaning of graphene

Studies of the structural and electronic properties of graphene in its pristine state are hindered by hydrocarbon contamination on the surfaces. Also, in many applications, contamination reduces the performance of graphene. Contamination is introduced during sample preparation and is adsorbed also directly from air. Here, we report on the development of a simple dry-cleaning method for producing large atomically clean areas in free-standing graphene. The cleanness of graphene is proven using aberration-corrected high-resolution transmission electron microscopy and electron spectroscopy.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2013

Salt-stone Oxidation Study: Leaching Method - 13092

Cementitious waste forms can be designed to chemically stabilize selected contaminants, such as Tc{sup +7} and Cr{sup +6}, by chemically reduction to lower valance states, Tc{sup +4} and Cr{sup +3}, respectively, and precipitation of these species in alkaline media as low solubility solid phases. Data for oxidation of this type of cementitious waste form cured under field conditions as a function of time is required for predicting the performance of the waste form and disposal facility. The rate of oxidation (oxidation front advancement) is an important parameter for predicting performance because the solubilities of some radionuclide contaminants, e.g., technetium, are a function of the oxidation state. A non-radioactive experiment was designed for quantifying the oxidation front advancement using chromium, as an approximate redox-sensitive surrogate (Cr{sup +6} / Cr{sup +3}) for technetium (Tc{sup +7} / Tc{sup +4}). Nonradioactive cementitious waste forms were prepared in the laboratory and cured under both laboratory and 'field conditions'. Laboratory conditions were ambient temperature and sealed sample containers. Field conditions were approximated by curing samples in open containers which were placed inside a plastic container stored outdoors at SRS. The container had a lid and was instrumented with temperature and humidity probes. Sub-samples as thin as 0.2 mm were taken as a function of distance from the exposed surface of the as-cast sample. The sub-samples were leached and the leachates were analyzed for chromium, nitrate, nitrite and sodium. Nitrate, nitrite, and sodium concentrations were used to provide baseline data because these species are not chemically retained in the waste form matrix to any significant extent and are not redox sensitive. 'Effective' oxidation fronts for Cr were measured for samples containing 1000, 500 and 20 mg/kg Cr added as soluble sodium chromate, Na{sub 2}CrO{sub 4}. For a sample cured for 129 days under field conditions, leachable Cr (assumed to be the oxidized form, i.e., Cr{sup +6} was detected in the top 15 to 20 mm of the sample spiked with 1000 mg/kg Cr. Below about 20 mm, the Cr concentrations in leachates were below the detection limit (< 0.010 mg/L) which indicates that the oxidation as the result of exposure to air was limited to the top 20 mm of the sample after exposure for 129 days and that the bulk of the waste form was not affected, i.e., the Cr was stabilized and insoluble. For samples cured in the laboratory, leachable Cr was detected in the top 8 mm of the Cr 1000 sample cured in the laboratory for 37 days. Between 8 and 14 mm, the concentration Cr in the leachate dropped by a factor of about 20 to just above the detection limit. These depth of penetration results indicate that the rate of advancement of the oxidation front for samples spiked with 1000 mg/kg Cr cured under 'field conditions' for 129 days is less than that for the sample cured in the laboratory for 37 days, i.e., 0.156 and 0.216 mm/day, respectively. Additional data are presented for samples spiked with 500 and 20 mg/kg Cr. In summary, cementitious waste forms are porous solids with a network of interconnected pores ranging in diameter from 10 E-10 m to greater than a few mm. The oxidation process is assumed to occur as the result of oxygen transport through the interconnected porosity which may be filled with air, aqueous salt solution, or both. Upon oxidation, the Cr becomes soluble and can be transported in solution through aqueous pore fluid or leachate. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
NASA NTRS1998

Effects of Ambient High Temperature Exposure on Alumina-Titania High Emittance Surfaces for Solar Dynamic Systems

Solar dynamic (SD) space power systems require durable, high emittance surfaces on a number of critical components, such as heat receiver interior surfaces and parasitic load radiator (PLR) elements. To enhance surface characteristics, an alumina-titania coating has been applied to 500 heat receiver thermal energy containment canisters and the PLR of NASA Lewis Research Center's (LeRC) 2 kW SD ground test demonstrator (GTD). The alumina-titania coating was chosen because it had been found to maintain its high emittance under vacuum (less than or equal to 10(exp -6) torr) at high temperatures (1457 F (827 C)) for an extended period (approximately 2,700 hours). However, preflight verification of SD systems components, such as the PLR require operation at ambient pressure and high temperatures. Therefore, the purpose of this research was to evaluate the durability of the alumina-titania coating at high temperature in air. Fifteen of sixteen alumina-titania coated Incoloy samples were exposed to high temperatures (600 F (316 C) to l500 F (816 C)) for various durations (2 to 32 hours). Samples, were characterized prior to and after heat treatment for reflectance, solar absorptance, room temperature emittance and emittance at 1,200 F (649 C). Samples were also examined to detect physical defects and to determine surface chemistry using optical microscopy, scanning electron microscopy operated with an energy dispersive spectroscopy (EDS) system, and x ray photoelectron spectroscopy (XPS). Visual examination of the heat-treated samples showed a whitening of samples exposed to temperatures of 1,000 F (538 C) and above. Correspondingly, the optical properties of these samples had degraded. A sample exposed to 1,500 F (816 C) for 24 hours had whitened and the thermal emittance at 1,200 F (649 C) had decreased from the non-heat treated value of 0.94 to 0.62. The coating on this sample had become embrittled with spalling off the substrate noticeable at several locations. Based on this research it is recommended that preflight testing of SD components with alumina-titania coatings be restricted to temperatures no greater than 600 F (316 C) in air to avoid optical degradation. Moreover, components with the alumina-titania coating are likely to experience optical property degradation with direct atomic oxygen exposure in space.

deGroh, Kim K.↗