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At least 199 records · Page 11

Obtaining Cryogenic Molecular Transport Data for Analysis

The James Webb Space Telescope (JWST) has a primary mirror, made of 18 segments, and a secondary mirror (SM) that are used to direct the light of desired targets. While on orbit, the secondary mirror assembly (SMA) was stowed for approximately 10 days and was subject to molecular contamination outgassing from the cavity of the secondary mirror support structure (SMSS) in-board hinge (IBH) which contains cables, motors, resolvers, and coatings. The main concern during this period before SMA deployment is the accumulation of ice due to the lack of a heater on the SMA. The temperature differentials between the IBH surfaces and SMA could cause redistribution of contaminants. To address this concern, single layer insulation (SLI) was used to create adequate venting and path redirection of outgassing from the IBH. Two separate thermal vacuum tests were performed to quantify this contamination: one Z307 ASTM E 1559 materials test of the radiator paint used on the motor of the IBH and a separate test on a primary mirror backplane assembly (PMBA) qualification engineering test unit (ETU) of the IBH. These tests approximately followed the predicted SMA pre-deployment thermal environment. To quantify source rates in case of a leak, the motor and resolver sides were separated and quartz crystal microbalances (QCM) were used to measure the deposition of water. The SLI redesign and implementation and outgassing measurements to understand leak effects from the IBH were essential to mitigate the deposition of contamination on the SMA. "

James Webb Space Telescope↗

Utilization of Ultrasonication as a Method of Reducing Organic and Inorganic Contamination in Post‐Consumer Plastic Film Waste

Post-consumer plastic film waste often carries organic and inorganic contaminants that challenge recycling processes and affect the quality of recycled products. An effective contaminant removal procedure through washing such single-used plastic films (SUPFs) can address environmental and waste management concerns. This study compares the efficiency of different washing techniques in reducing SUPF contamination. To evaluate the efficacy of each washing technique, film samples collected from material recovery facilities are individually exposed to friction, ultrasonic-assisted, and a combination of both washes. Thermal analysis indicates that the polymers' melting temperature, crystallization temperature, and crystallinity remain unaffected by the washing methods, demonstrating method aptness. Confocal laser scanning microscope images show that washing results in a cleaner sample surface. 91% ash reduction during the combined wash treatment indicates a high method efficiency compared to the individual friction and ultrasonic wash procedures. This is further validated by reducing characteristic contaminant IR bands (3600–3000, 1750–1600, and 1100–1000 cm −1 ). Elements of concern such as Cd, Cr, Hg, and Pb in SUPFs after each washing technique applied conform with regulations (<100 ppm) for packaging products. This research shows the novel ultrasonic washing reduces more contamination than friction with shorter wash times and no surfactants.

42 ENGINEERING↗

New shield for gamma-ray spectrometry

Gamma-ray shield that can be evacuated, refilled with a clean gas, and pressurized for exclusion of airborne radioactive contaminants effectively lowers background noise. Under working conditions, repeated evacuation and filling procedures have not adversely affected the sensitivity and resolution of the crystal detector.

Brar, S. S.↗

Proper Criteria of Nonlinear Optical Crystals for Space Laser Systems and the Possible Causes for Space Laser Failures

NASA is striving to develop a scientific understanding of the universe and the Earth-Sun System and its response to natural or human-induced changes. Space lasers are vital tools for NASA's missions to advance our understanding of space research and improving our prediction capability for climate, weather, and natural hazards. Unfortunately, several past space missions that utilized lasers proved to be short-lived and unreliable. In this paper, we are reporting the results of our investigations on several nonlinear optical crystals, which are vital components in space lasers. Examples of these investigations are: The correlation of the phase diagrams of nonlinear crystals and its durability, the effect of radiating these crystals by high-energy beams of protons and gamma on their second harmonic efficiency, and measurements of the high-energy and low-energy thresholds for each crystal before and after irradiation. A set of proper criteria for these crystals will be presented. We will also discuss the possible causes of failures in a space laser and propose a solution to a contamination problem in all future space lasers.

Abdeldayem, Hossin A.↗

Treatment of emerging contaminants in simulated wastewater via tandem photo-Fenton-like reaction and nutrient recovery

We report a tandem strategy that recovers NH 4 + and PO 4 3- nutrients from simulated wastewater in a solid form after the Fenton oxidation of emerging organic contaminants was developed. Mesoporous Cu–MgO nanoparticles were used as a photo-Fenton-like catalyst to oxidize paraoxon and tetracycline present in nutrient-rich simulated wastewater to prevent their incorporation into the struvite product. Mesoporous MgO nanoparticles were subsequently used as the Mg-source for the struvite crystallization due to the fast intraparticle diffusion and adsorption kinetics facilitated by their porosity and the high surface area. Without Fenton oxidation, 13% of paraoxon and 37% of tetracycline were incorporated into the struvite, demonstrating the clear need for the removal of hazardous contaminants before struvite synthesis. Both organic contaminants were eliminated using the Fenton oxidation reaction, with some minor non-toxic intermediate products formed. The product formed after the tandem process was shown by XRD and Raman spectroscopy to be struvite free of the emerging organic contaminants.

54 ENVIRONMENTAL SCIENCES↗

Thermocapillary flows and their stability: Effects of surface layers and contamination

The fluid mechanics and heat transfer of motions driven by surface tension gradients (Marangoni convection) were analyzed theoretically to obtain an understanding of the convection accompanying the process of growing high quality single crystals from the melt in a mu-g environment. The geometries considered include two dimensional liquid filled slots and axisymmetric float zone configurations.

Davis, S. H.↗

Use of Refractory-Volatile Element Deep Eutectic Regions to Grow Single Crystalline Intermetallic Compounds

Compounds containing both refractory and volatile elements present a unique challenge for crystal growth, given the conflicting realities of high melting temperatures and high vapor pressures. Nevertheless, the discovery of superconductivity in FeAs and FeSe based materials and a Weyl semimetal state in TaP are motivations to explore compounds containing such pairs. Here, we discuss use of the low-melting single phase liquid regions above deep M-X eutectics (M=transition metal, X=P, S) as the basis for high temperature solutions for growing intermetallic compounds containing volatile-refractory pairs. We show that Ni-P, Pd-P, Pt-P, and Pd-S compositions form single phase melts at moderate temperatures below 1000 °C and with minimal vapor pressure. We first present the simple case of growing Ni 2 P from Ni-P and next discuss the more complicated growth of RPd 3 S 4 (R=La, Ce, Nd, Eu) from a Pd-S melt. We show how frit-disc alumina crucible sets allow for contamination-free capture of decanted liquid and its reuse in subsequent experiments, demonstrating a fractionation of the CePd 3 S 4 growth to determine the optimal conditions for crystal growth. We conclude by using the single phase liquid regions above the Pt-P and Pd-P eutectics to grow single crystals of MPt 5 P (M=Mn, Fe) and MnPd 5 P. As these materials have primarily been studied in polycrystalline form, we give an overview of the magnetic and transport properties of our single crystals. The examples outlined here illustrate the utility of using the single phase liquid above deep metal-X eutectics for solution growth and materials discovery.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Friction behavior of members of the platinum metals group with gold

The adhesion and friction behavior of the platinum metals group was examined with clean surfaces and surfaces selectively contaminated with oxygen, vinyl chloride (C2H3Cl), and methyl mercaptan (CH3SH). A pin or disk specimen configuration was used with the pin being a single crystal of gold of the (111) orientation and with the platinum metal disks also being single crystals of the (111) or (0001) orientation. Loads applied ranged from 1 to 10 g and a sliding velocity of 0.7 mm/min was employed. Results indicate adhesion and transfer of gold to all of the platinum metals. Despite this observation friction differences existed among the metals in the group. These differences are related to surface chemical activity. Adsorption of various friction reducing species was selective. With some adsorbates present strong adhesive forces between metals were still observed.

Buckley, D. H.↗

Determination of contamination character of materials in space technology testing

The contamination characters of selected materials used in space technology testing. Specific materials were subjected to a thermal vacuum environment, and the outgases were collected on a cold test mirror surface. Approximately one-half of the surface of the mirror was subjected to ultraviolet irradiation while the outgases were being deposited on the mirror. The purpose of these experiments was to determine the effect of ultraviolet irradiation on the contaminative character of outgases from selected materials. The degree of contamination was measured in terms of degradation of the optical properties of the test mirror and the amount of deposit per unit area on quartz crystal microbalances placed near the test mirror, and by means of quadrupole mass spectral measurements of outgases from the test samples.

Haynes, D. L.↗

Materials of construction for silicon crystal growth

The performance of materials for construction and in contact with molten silicon for crystal growth is presented. The basis for selection considers physical compatibility, such as thermal expansion and strength, as well as chemical compatibility as indicated by contamination of the silicon. A number of new high technology materials are included as well as data on those previously used. Emphasis is placed on the sources and processing of such materials in that results are frequently dependent on the way a material is prepared as well as its intrinsic constituents.

Leipold, M. H.↗

Ambient air contamination: Characterization and detection techniques

Techniques to characterize and detect sources of ambient air contamination are described. Chemical techniques to identify indoor contaminants are outlined, they include gas chromatography, or colorimetric detection. Organics generated from indoor materials at ambient conditions and upon combustion are characterized. Piezoelectric quartz crystals are used as precision frequency determining elements in electronic oscillators.

Nulton, C. P.↗

Thermodynamics of Minerals Stable near Earth's Surface

Project “Thermodynamics of Minerals Stable Near the Earth’s Surface” uses specialized calorimetric techniques to obtain new thermochemical data for solid phases of interest in the Earth’s “critical zone”, the near surface regions of the planet most directly affecting and affected by human activity. Major activity was in three areas: manganese oxide materials, aluminum clusters which are precursors to aluminum oxyhydroxide precipitates, and zeolites. All these classes of minerals are potential carriers of heavy metals and radionuclides in the environment, both within their crystal structures and as adsorbed layers or colloids. Their thermodynamic stability, as well as the sequence of stability of competing phases, governs the aqueous solubility of contaminants (and nutrients) in soil, groundwater, and sediments. The thermodynamics of these phases is strongly affected by particle size and crystallinity, since they often occur as very fine particles which do not coarsen in the near-surface environment. Many of these materials exhibit extensive polymorphism, multicomponent solid solution, and variable hydration states. Thus, one must define and systematize important thermodynamic variables, since one cannot make measurements on each and every possible phase, particle size, and composition. A major finding of the work on manganese oxides was labile water-induced oxidation-reduction reactions. These will be studied further by a combination of thermodynamic and synchrotron-based spectroscopic methods, the latter in collaboration with Peggy O’Day at UC Merced. The adsorption of other species, including simple organics, on such redox-active surfaces will also be investigated by a combination of thermochemical and spectroscopic studies. Studies of the energetics of water adsorption on mineral surfaces will be expanded to emphasize the adsorption of CO2 and small organic molecules, relevant to soil, groundwater, and the subsurface environment. Gas adsorption calorimetry, immersion calorimetry, and solution calorimetry will be combined with appropriate analytical and spectroscopic techniques to obtain a comprehensive picture of the interactions and their energetics. The evolution of aqueous aluminum clusters to form aluminum oxyhydroxide precipitates will be studied in detail by a combination of calorimetric and structural methods applied to aqueous samples aged at room temperature. The energetics of new classes of clusters will be explored. The project addresses several common themes relevant to the broad mission of the Department of Energy. Thermochemical data for minerals stable near the Earth’s surface, though still incomplete, are essential for understanding both natural and anthropogenic processes that affect our very existence on this planet. Such data contribute to the fundamental underpinning for mitigation and management strategies for the extraction and use of energy. Fundamental thermodynamic and mechanistic understanding is required to model processes ranging from heavy metal pollution to nuclear waste disposal to climate change.

58 GEOSCIENCES↗

Three Distinctive Steps for Heterogeneous Nucleation of Tunnel-Structured Mn Oxide on Quartz under Light Exposure

Natural manganese (Mn) oxide coatings, resulting from the heterogeneous nucleation on foreign substances, have garnered interest based on their importance in the reaction with organic substances and in environmental systems. However, the heterogeneous nucleation of the natural Mn oxide coatings still remains elusive. Here, via fast photochemical oxidation of Mn 2+ (aq), we show that Mn(IV) oxide nuclei form and aggregate on quartz in three distinct successive stages: (i) a nanocrystalline film of unaligned grain forms, (ii) nanoislands develop on the film, and (iii) nanorods form on the nanoislands. Each stage has different crystalline structures and forms by aligned attachment of nanoscale precursors on the preceding surface. Crystal lattice analyses confirm the crystalline development, from the short-range order of the Mn oxide film to the long-range order of the nanorods. Also, the heterogeneous nucleation observed in this work produced groutellite-like tunnel structures of Mn oxide on quartz. Furthermore, this revealed pathway of the heterogeneous nucleation can offer a new perspective on the variety of poorly crystalline structures of natural Mn oxides found in the environment, which can affect elemental redox cycles, contaminant sequestration and removal, and soil carbon storage.

Aligned attachment↗

Investigation of the effect of structural defects from hydride precipitation on superconducting properties of high purity SRF cavity Nb using magneto-optical and electron imaging methods

Abstract Nb is an elemental superconductor with a critical temperature of 9.3 K and is widely used to fabricate superconducting radiofrequency (SRF) cavities for particle accelerators. However, microstructural defects in Nb, such as grain boundaries (GBs) and dislocations, can act as pinning centers for magnetic flux that can degrade SRF cavity performance. Hydrogen contamination is also detrimental to SRF cavity performance due to the formation of normal conducting hydrides during cool down. In this study, disc shaped Nb bi-crystals extracted from high-purity large-grain Nb slices were investigated to study the effects of GBs, hydrogen, and dislocations on superconducting properties. Grain orientation and GB misorientation were measured using Laue x-ray diffraction and electron backscattered diffraction (EBSD) analyses. Cryogenic magneto-optical imaging was used to directly observe magnetic flux penetration below T c = 9.3 K. Damage caused by low temperature precipitation of hydrides and their dissolution upon reheating after cryogenic cycles was examined using electron channeling contrast imaging, and EBSD. The relationships between hydride formation, dislocation content, GBs, cryo-cooling, heat treatment (HT), and flux penetration indicate that both GB character and hydrogen content affect magnetic flux penetration. Such flux penetration could be facilitated by dislocation structures and low angle GBs resulting from hydride precipitation and HT.

36 MATERIALS SCIENCE↗

Silicon materials task of the low-cost solar array project. Phase 4: Effects of impurities and processing on silicon solar cells

The results of the study form a basis for silicon producers, wafer manufacturers, and cell fabricators to develop appropriate cost-benefit relationships for the use of less pure, less costly solar grade silicon. Cr is highly mobile in silicon even at temperatures as low as 600 C. Contrasting with earlier data for Mo, Ti, and V, Cr concentrations vary from place to place in polycrystalline silicon wafers and the electrically-active Cr concentration in the polysilicon is more than an order of magnitude smaller than would be projected from single crystal impurity data. We hypothesize that Cr diffuses during ingot cooldown after growth, preferentially segregates to grain and becomes electrically deactivated. Accelerated aging data from Ni-contaminated silicon imply that no significant impurity-induced cell performance reduction should be expected over a twenty year device lifetime.

Hopkins, R. H.↗

Contamination control program for the Extreme Ultraviolet Explorer instruments

A contamination-control program has been instituted for the optical components of the EUV Explorer satellite, whose 80-900 A range performance is easily degraded by particulate and molecular contamination. Cleanliness requirements have been formulated for the design, fabrication, and test phases of these instruments; in addition, contamination-control steps have been taken which prominently include the isolation of sensitive components in a sealed optics cavity. Prelaunch monitoring systems encompass the use of quartz crystal microbalances, particle witness plates, direct flight hardware sampling, and optical witness sampling of EUV scattering and reflectivity.

Ray, David C.↗

Control of Meridional Flow in Circular Cylinders by a Travelling Axial Magnetic Field

Convective flow in a Bridgman or float zone configuration significantly affects the interface shape and segregation phenomena. While the primary causative factor for this flow is buoyancy induced convection in an enclosed Bridgman melt, the presence of a free surface gives rise to surface tension driven flows in the floating zone processing of melts. It is of interest to curtail these flows in order to realize near quiescent growth conditions that have shown to result in crystals with good longitudinal and radial homogeneity and thereby of better overall quality. While buoyancy effects can be reduced by careful processing in a low gravity (space) environment, the reduction of Marangoni flows due to surface tension variations is not that straight forward. Attempts have been made with some limited success with the use of external fields to affect the melt thermo-fluid behavior. The use of a static magnetic field that reduces convective contamination through the effects of a non-intrusively induced, dissipative Lorentz force in an electrically conducting melt is one such approach. Experiments have shown that axial fields of the order of 5 Tesla can significantly eliminate convection and yield close to diffusion limited crystal growth conditions. The generation and use of such high magnetic fields require substantial hardware and incur significant costs for its operation. Lately, the use of rotating magnetic fields has been tested in semiconductor crystal growth. The method is fairly well known and commonly used in metal processing but its adaptation to crystal growth of semiconductors is fairly recent. The elegance of the technique rests in its low power requirement (typically 10-20 milli-Tesla at 50-400 Hz) and its efficacy in curtailing deleterious temperature fluctuations in the melt. A rotating magnetic field imposes a rotational force and thereby induces a circulation within the melt that tends to dominate other sporadic convective effects. Thus a known low level of convective flow is introduced into the system. A new novel variation of the Lorentz force mechanism is proposed and investigated in this study. Since one of the desired process conditions in melt crystal growth is the minimization of convective effects, this investigation examines the use of an external field of magnetic origin to counteract existing convective flow within the melt. This is accomplished by utilizing a running or traveling axial magnetic wave in the system. The concept is similar to the use of vibrational means in order to induce streaming flows that oppose buoyant or surface tension driven convection in the system. The rotation direction as well as the magnitude (strength) of this circulation can be easily controlled by external inputs thus affording a direct means of controlling the developing shape of the crystallizing front (interface). The theoretical model of this technique is fully developed and presented in this paper. Results from the solution of the developed governing equations and boundary conditions are also presented. An experimental demonstration of the concept is presented through the suppression of natural convective flow in a mercury column. Implications to crystal growth systems will be fully explored in the final manuscript.

Mazuruk, K.↗

Earth Abundant Oxidation Catalysts for Removal of Contaminants of Emerging Concern from Wastewater: Homogeneous Catalytic Screening of Monomeric Complexes

Twenty novel Mn, Fe, and Cu complexes of ethylene cross-bridged tetraazamacrocycles with potentially copolymerizable allyl and benzyl pendant arms were synthesized and characterized. Multiple X-ray crystal structures demonstrate the cis-folded pseudo-octahedral geometry forced by the rigidifying ethylene cross-bridge and show that two cis coordination cites are available for interaction with substrate and oxidant. The Cu complexes were used to determine kinetic stability under harsh acidic and high-temperature conditions, which revealed that the cyclam-based ligands provide superior stabilization with half-lives of many minutes or even hours in 5 M HCl at 50–90 °C. Cyclic voltammetry studies of the Fe and Mn complexes reveal reversible redox processes indicating stabilization of Fe 2+ /Fe 3+ and Mn 2+ /Mn 3+ /Mn 4+ oxidation states, indicating the likelihood of catalytic oxidation for these complexes. Finally, dye-bleaching experiments with methylene blue, methyl orange, and rhodamine B demonstrate efficient catalytic decolorization and allow selection of the most successful monomeric catalysts for copolymerization to produce future heterogeneous water purification materials.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗