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At least 559 records · Page 31

Technical Assessment of Internal Surface Smoothness and Particle Transmission to the American National Standard ANSI/HPS N13.1-2011

Clause 6.4.4 in the American National Standards Institute / Health Physics Society (ANSI/HPS) N13.1 standard, Sampling and Monitoring Releases of Airborne Radioactive Substances From the Stacks and Ducts of Nuclear Facilities, addresses the internal smoothness of sample transport lines present between the nozzle and the analyzer (or collector). This paper evaluates the appropriateness of this clause by comparing roughness length of various materials against the required relative roughness, and by conducting computational fluid dynamic modeling. The results indicate that the inclusion of numerical criteria for the relative roughness of pipe by the ANSI Standard N13.1 (Section 6.4.4) is not appropriate. Recommended alternatives would be elimination of the numerical criteria, or modification of the standard to include a variable criteria for relative roughness.

operational topics, aerosols, air sampling, atmosp↗

A 291-day Evaluation of the Performance of a Consumer-grade Temporal Radon Detector

Affordable, accurate, and robust temporal measurement devices are desirable for screening and assessment of radon levels in private homes and workplaces. This research expands upon prior research, using the RadonFTlab RadonEye device through a comparison of multiple samples of this instrument with a laboratory-grade instrument, the Saphymo AlphaGUARD, over a more extensive period than reported previously. Data were collected over 291 d in a poorly ventilated basement space in an occupied building. Environmental conditions varied naturally, changing both the radon source term and radon entry into the space approximating typically deployed conditions. The R-squared linear regression correlation coefficient and relative sensitivities of each RadonEye with the AlphaGUARD were computed. Altogether temporal and diurnal variations were also studied. The sensitivities of all RadonEyes and the AlphaGUARD agreed to within 22% throughout the entire deployment period.

47 OTHER INSTRUMENTATION↗

Subsolidus phase relations of the SrO-WO 3 -CuO system at 800 °C in air

The subsolidus phase relations of the SrO-WO 3 -CuO system were investigated in air. The samples were equilibrated at 800 °C. Under these conditions, eight binary oxides are stable. The pseudo-ternary section contains two ternary oxide phases: the previously described Sr 2 CuWO 6 phase as well as a new phase with Sr 8 CuW 3 O 18 stoichiometry. The crystal structure of this new compound was solved and refined in the R-3 space group, unit cell parameters a = 5.7202 Å and c = 28.873 Å. Sr 8 CuW 3 O 18 has a distorted perovskite type structure, where some of the Sr atoms are positioned at the B sites, and the composition may be given as: Sr 6 (Sr 2 CuW 3 )O 18 . There are indications of existence of a superstructure or stacking faults related to Cu/Sr ordering.

36 MATERIALS SCIENCE↗

Planetary Protection at Marshall Space Flight Center

Introduction: NASA Marshall Space Flight Center (MSFC) is historically known for its role in propulsion. While this is still the mainstay of MSFC’s expertise, many unique capabilities exist at MSFC which pertain to Planetary Protection (PP), including 1) identifying PP threats, and 2) developing novel methods to neutralize those threats. Furthermore, because these capabilities exist among diverse groups at MSFC, this work promotes collaboration both within and outside MSFC to expand and develop PP studies related to a full spectrum of NASA research, design, manufacture, and test interests. This abstract describes the PP research ongoing at MSFC and describes how it contributes to NASA’s overall PP objectives. Microbial Identification in Cleanrooms: One of the greatest threats to successful implementation of PP requirements is recontamination post bioburden reduction. One method to prevent recontamination is to keep the spacecraft in clean environments (i.e. cleanrooms) as much as possible during assembly and integration. However, cleanrooms are not without their own sources of contamination, which is why NASA is interested in monitoring the cleanliness of cleanrooms and characterizing the microbial species present. Such information allows a greater understanding of the resistance of these microbes to cleaning methods, as well as the risk of their contaminating the targeted planetary body of a given mission. MSFC has multiple cleanrooms of various ISO cleanliness levels onsite. We sampled the air and surfaces of three of these rooms, isolated microbes, and then sequenced the 16S rRNA gene or ITS region of the 18S rRNA gene for bacterial and fungal isolates, respectively. This has resulted in a microbial library which currently includes nearly 100 isolates. Microbial Enumeration of Spacecraft Materials: Currently, there are only a couple bioburden reduction methods approved by NASA, and often the harshness of these methods presents additional concerns or risks related to material properties. The goal of this research is to assess the microbial content of solid rocket motor (SRM) materials potentially used for lander missions. This work aims to more accurately define the risk of planetary contamination by providing empirical data associated with commonly used SRM raw materials. In this study, we pulverized nonmetallic SRM materials using a cryogenic grinder, then analyzed the resulting substrate for microbial colony forming units (CFU). We found that many SRM nonmetallic materials do not harbor detectable bioburden, though a range existed depending on the material. The results from this work provide quantitative data to potentially reduce concerns of contamination, while also providing a foundation for follow up studies into additional sterilization methods and molecular identification of contaminating microbes. Space Environmental Effects on Microbial Survival: One potential area of microbial reduction is the space environment. Understanding the survivability of hardy microbes in space-like conditions is a crucial first step in answering how space may reduce bioburden and if it can be relied upon for adherence to PP requirements. This work studied the effects of ultraviolet (UV) and ionizing radiation on survival of Bacillus atrophaeus spores. Microbes were dried on relevant polymeric materials then exposed to space environmental stressors. Coupons were submerged in water, diluted, and plated to determine survival compared with controls. We found that both UV and ionizing radiation were capable of reducing viability by nearly 99%, but there were still survivors, some with changed morphology indicating resistance mechanisms within certain cells. Manufacturing credit: Finally, given the above-mentioned limitations of the NASA-approved bioburden reduction methods, there is interest in understanding if manufacturing processes may provide enough bioburden reduction without additional PP-specific bakeouts. For instance, some material additives may be antimicrobial. Given this, we investigated the effects of several commonly used rubber additives on the growth of B. atrophaeus spores. We found that some of the materials inhibited growth of the spores, possibly supporting the use of these additives on missions with PP constraints. Future work into manufacturing credit for bioburden reduction includes inoculation of green insulation with B. atrophaeus spores, followed by a typical cure. Thermal profiles will be verified for appropriate temperature and durations to meet PP requirements, and cured samples will be analyzed using a cryogenic grinder to determine survivability of spores.

Chelsi D. Cassilly↗

Effect of pretreatment conditions on acidity and dehydration activity of CeO 2 -MeO x catalysts

A series of MeOx-modified CeO 2 (CeO 2 -MnO x , CeO 2 -ZnO, CeO 2 -MgO, CeO 2 -CaO, and CeO 2 -Na 2 O) catalysts were prepared by the impregnation of CeO 2 with corresponding metal nitrates. Acidity and oxidation state of cerium were investigated on both oxidized and reduced catalysts by employing Fourier Transform Infrared spectroscopy (FTIR) on adsorbed pyridine and in situ H 2 -Temperature Programmed Reduction/X-ray Absorption Spectroscopy (H 2 -TPR/XAS) techniques, respectively. Metal oxide addition tended to alter both type and number of acid sites on ceria. EXAFS data showed a significant difference in N Ce-O between unmodified and CeO 2 -MeO x , suggesting that added MeO x interferes with vacancy formation on ceria during reduction. Here, in comparison with air-pretreated samples, H 2 -pretreated ones under similar conversion of 1,5 pentanediol exhibited a higher selectivity towards linear alcohols. Alcohol conversion found to correlate with total acidity (i.e., Brønsted and Lewis). CeO 2 benefited from the addition of alkali (Na) or alkaline earth metals (Mg, Ca) by producing unsaturated alcohols.

1,5-Pentanediol↗

Oxidation of porous stainless steel supports for metal-supported solid oxide electrolysis cells

Oxidation behavior of porous P434L ferritic stainless steel, used for the fabrication of metal-supported solid oxide electrolysis cells (MS-SOEC), is studied under oxygen-side and steam-side conditions. The impact of oxygen content on the oxygen side and steam:hydrogen ratio on the steam side is determined at 700°C for bare, as-sintered samples. For these conditions, oxidation is more aggressive in the steam-side atmosphere. Oxygen with 3% humidification and steam:hydrogen ratio of 90:10 are selected for further assessment with pre-oxidized, catalyst-coated, and CuMn1·8O4-coated samples. The rapid oxidation at 700°C and breakaway oxidation at 600 °C observed for bare stainless steel in 90:10 steam:hydrogen is mitigated by pre-oxidizing the sample in air before exposure. In oxygen, addition of the catalyst or CuMn 1·8 O 4 coatings moderately increases the oxidation rate, due to consumption of Cr via reaction between the coatings and Cr-oxide scale. In conclusion, the results for ex-situ controlled oxidation are similar to oxidation observed after 1000h operation of a full MS-SOEC. In general, the oxidation behavior at 700°C is found to be acceptable.

08 HYDROGEN↗

Subsolidus phase relations of the SrO-SbO x -CuO system at 1140 K in air

The subsolidus phase relations of the SrO–SbOx–CuO system were investigated in air. The samples were equilibrated at 1140 K. Under these conditions, 7 binary oxide phases are stable: Sr 2 CuO 3 , SrCuO 2 , Sr 14 Cu 24 O 41-δ , CuSb 2 O 6 , SrSb 2 O 6 , Sr 2 Sb 2 O 7 and Sr 7 Sb 2 O 12 . The ternary section contains 10 three-phase regions. A new ternary oxide phase with an approximate Sr 3 Sb 2 CuO 9 composition of was identified. It structure is related to that of Sr 8 W 3 CuO 18 . This phase is not superconducting above 2 K. Instead, the magnetic susceptibility indicates onset of weak ferro- or ferrimagnetism at T ≈ 30 K.

Grivel, J. -C.↗

Structural and spectroscopic studies of Ba{sub 2}Y{sub 1−δ}UO{sub 6+x}

A combination of S-XRD and NPD demonstrate the structure of Ba{sub 2}Y{sub 0.879}UO{sub 6+x} to be monoclinic in space group I2/m. That the U is hexavalent is evident from the U L{sub 2}-edge XANES measurements. This appears to be a rare example of a double perovskite containing vacancies at the octahedral B-sites and interstitial oxygen defects, which combine to stabilise hexavalent U and appears to be a consequence of the preparation of the sample in air. The Y vacancies, coupled with anion disorder, results in a distortion of the BO{sub 6} octahedra. - Graphical abstract: The structure of Ba{sub 2}Y{sub 0.879}UO{sub 6+x} is shown to be a rare example of a double perovskite containing vacancies at the octahedral B-sites and interstitial oxygen defects. - Highlights: • Structure of Ba{sub 2}Y{sub 0.879}UO{sub 6+x} refined. • U L-edge XANES demonstrates the U is hexavalent. • Rare example of a perovskite containing vacancies at the octahedral B-site. • Y vacancies result in a distortion of the BO{sub 6} octahedra.

36 MATERIALS SCIENCE↗

Stability and phase evolution of mullite in reducing atmosphere

The aim of this study is to investigate the stability of mullite and its phase evolution when heated at 1600-1650 deg. C in reducing atmosphere created by a carbon bed. The stoichiometric mullite (3Al{sub 2}O{sub 3}.2SiO{sub 2}) was synthesized by reacting the proper precursors at 1400 deg. C in air atmosphere. Samples containing the primary mullite and graphite or carbon were prepared by pressing the mix and heated at 1600-1650 deg. C. Products were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The results showed that the stoichiometric mullite could decompose to corundum and alumina-rich mullite. During firing under reducing atmosphere, the stoichiometric mullite became richer in Al{sup 3+} cations. The gaseous SiO compound was found to be released from the sample and reacting with C to form SiC phase. Comparison of general mullite solid solution (Al{sub 4+2x}Si{sub 2-2x}O{sub 10-x}) with alumina-rich mullite obtained from decomposition revealed that x would take different values depending on temperature and atmosphere. The ultimate decomposition product was found to be corundum. - Research Highlights: {yields} This method is a new route for investigation of thermochemical stability of stoichimetric mullite under reducing condition which have done by the authors. {yields} This research has got very good results for stability of mullite at different conditions. {yields} This work has also studied the mechanism of stability of mullite under reducing atmosphere.

36 MATERIALS SCIENCE↗

Stabilizing Ir(001) Epitaxy on Yttria-Stabilized Zirconia Using a Thin Ir Seed Layer Grown by Pulsed Laser Deposition

In this paper, we demonstrate the reproducible epitaxial growth of 100 nm thick Ir(001) films on a heteroepitaxial stack consisting of 5 nm Ir and 100 nm yttria-stabilized zirconia (YSZ) grown on Si(001) substrates. It is shown that a 5 nm thick Ir layer grown by pulsed laser deposition in the same chamber as the YSZ film without breaking the vacuum is the key to stabilizing Ir(001) epitaxial growth. Growth of the Ir seed layer with pure (001) orientation occurs only in a narrow growth temperature window from 550 to 750 °C, and the fraction of Ir(111) increases at substrate temperatures outside of this window. The Ir seed layer prevents exposure of the YSZ film to air during sample transfer and enables highly reproducible Ir(001) heteroepitaxy on YSZ buffered Si(001). In contrast, if Ir is grown directly on a bare YSZ layer that was exposed to ambient conditions, the films are prone to change orientation to (111). These results reveal that preserving the chemical and structural purity of the YSZ surface is imperative for achieving Ir(001) epitaxy. The narrow range of the mosaic spread values from eight experiments demonstrates the high yield and high reproducibility of Ir(001) heteroepitaxy by this approach. Lastly, the improved Ir(001) epitaxial growth method is of great significance for integrating a variety of technologically important materials such as diamond, graphene, and functional oxides on a Si platform.

36 MATERIALS SCIENCE↗

Facile Extraction of Wheat Straw by Deep Eutectic Solvent (DES) to Produce Lignin Nanoparticles

A detailed investigation of choline chloride-lactic acid (ChCl-LA)-based deep eutectic solvent (DES) extraction of lignin nanoparticles from herbaceous biomass (wheat straw) was conducted. It was found that DES can extract high purity lignin (up to 94.8%) with a high yield (up to 81.5% from air-dried samples and 85.9% from oven-dried samples) from wheat straw. The cleavages of ether bonds in lignin, as well as the linkages between lignin and hemicelluloses during DES treatments at different conditions, were analyzed. The effects of reaction time, treatment temperature and water content in wheat straw on lignin yield, purity, and chemical structure were determined. The water content in biomass was found to affect the hydrogen bond interaction between lignin and DES, which was a key factor influencing the lignin extraction yield and chemical properties of separated lignin. The lignin extracted from wheat straw by DES consists of well-dispersed nanoparticles with a narrow size distribution peaking at 70-90 nm. The mechanism of ChCl-LA-based DES depolymerization and extraction of lignin from wheat straw is discussed.

Lou, Rui↗

Photoinduced Surface Oxidation and Its Effect on the Exciton Dynamics of CdSe Quantum Dots

With increased interest in semiconductor nanoparticles for use in quantum dot solar cells there comes a need to understand the long-term photostability of such materials. Colloidal CdSe quantum dots (QDs) were suspended in toluene and stored in combinations of light/dark and N{sub 2}/O{sub 2} to simulate four possible benchtop storage environments. CdSe QDs stored in a dark, oxygen-free environment were observed to better retain their optical properties over the course of 90 days. The excited state lifetimes, determined through femtosecond transient absorption spectroscopy, of air-equilibrated samples exposed to light exhibit a decrease in average lifetime (0.81 ns) when compared to samples stored in a nitrogen/dark environment (8.3 ns). A photoetching technique commonly used for controlled reduction of QD size was found to induce energetic trap states to CdSe QDs and accelerate the rate of electron-hole recombination. X-ray absorption near edge structure (XANES) analysis confirms surface oxidation, the extent of which is shown to be dependent on the thickness of the ligand shell.

14 SOLAR ENERGY↗

C-Term magnetic circular dichroism (MCD) spectroscopy in paramagnetic transition metal and f-element organometallic chemistry

Magnetic circular dichroism (MCD) spectroscopy is a powerful experiment used to probe the electronic structure and bonding in paramagnetic metal-based complexes. While C-term MCD spectroscopy has been utilized in many areas of chemistry, it has been underutilized in studying paramagnetic organometallic transition metal and f-element complexes. From the analysis of isolated organometallic complexes to the study of in situ generated species, MCD can provide information regarding ligand interactions, oxidation and spin state, and geometry and coordination environment of paramagnetic species. The pratical aspects of this technique, such as air-free sample preparation and cryogenic experimental temperatures, allow for the study of highly unstable species, something that is often difficult with other spectroscopic techniques. This perspective highlights MCD studies of both transition metal and f-element organometallic complexes, including in situ generated reactive intermediates, to demonstrate the utility of this technique in probing electronic structure, bonding and mechanism in paramagnetic organometallic chemistry.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

High throughput exploration of the oxidation landscape in high entropy alloys

We report high entropy alloys (HEAs) have gained interest for structural applications in extreme environments. With a potentially vast chemical and phase space, there are significant opportunities to discover superior performing alloys. Crucial for most high-temperature applications is understanding and mitigating the oxidation behavior of these chemically complex alloys. Most experimental and computational HEA studies have focused on a limited set of compositions and only a fraction these compositions have been characterized for oxidation. We present a high-throughput framework that utilizes density-functional theory (DFT) in concert with a combined machine-learning model and grand-canonical linear programming for assessing phase stability, phase-fraction, chemical activity and high-temperature survivability of arbitrary HEAs. This framework considers temperature dependent contributions to the Gibbs energy of the competing phases arising from short-range order and vibrational entropy. We demonstrate the effectiveness of the framework by assessing the thermodynamic stability, oxidation behavior, chemical activity, and phase decomposition of body-centered cubic Mo-W-Ta-Ti-Zr refractory HEAs. A total of 51 compositions were analyzed and ranked in order of their survivability based on the Pareto-front analysis. Oxidation was performed at 1373 K on fours samples in air showing the difference in oxidation behavior determined experimentally through scale thickness and their mass changes. The insights on oxidation behavior presented in this work will enable the fast assessment of technologically useful HEAs needed for future structural application in extreme conditions

36 MATERIALS SCIENCE↗

Proton conductivity of perfluorosulfonate ionomers at high temperature and high relative humidity

The proton transport properties of Nafion membranes were studied in a wide range of temperature by using an air-tight sample holder able to maintain the sample hydrated at high relative humidity. The proton conductivity of hydrated Nafion membranes continuously increased in the temperature range of 40–180 °C with relative humidity kept at RH = 100%. In the temperature range of 40–90 °C, the proton conductivity followed the Arrhenius-like thermal dependence. The calculated apparent activation energy E{sub a} values are in good agreement with proton transport via the structural diffusion in absorbed water. However, at higher measuring temperatures an upturn of the electrical conductivity was observed to be dependent on the thermal history of the sample.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

High-speed atomic force microscope based on an astigmatic detection system

High-speed atomic force microscopy (HS-AFM) enables visualizing dynamic behaviors of biological molecules under physiological conditions at a temporal resolution of 1s or shorter. A small cantilever with a high resonance frequency is crucial in increasing the scan speed. However, detecting mechanical resonances of small cantilevers is technically challenging. In this study, we constructed an atomic force microscope using a digital versatile disc (DVD) pickup head to detect cantilever deflections. In addition, a flexure-guided scanner and a sinusoidal scan method were implemented. In this work, we imaged a grating sample in air by using a regular cantilever and a small cantilever with a resonance frequency of 5.5 MHz. Poor tracking was seen at the scan rate of 50 line/s when a cantilever for regular AFM imaging was used. Using a small cantilever at the scan rate of 100 line/s revealed no significant degradation in the topographic images. The results indicate that a smaller cantilever can achieve a higher scan rate and superior force sensitivity. This work shows the potential for using a DVD pickup head in future HS-AFM technology.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗