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DOE OSTI2016

Structure and tribological properties of steel after non-vacuum electron beam cladding of Ti, Mo and graphite powders

The non-vacuum electron beam cladding technique was used to fabricate layers alloyed with Ti, Mo and C on the surface of low-alloyed steel. Two types of experiments were carried out. In the first experiment, a mixture of Ti and graphite powders was used for cladding; in the second, a mixture of Ti, Mo and graphite powders was used for cladding. CaF{sub 2} powder or a mixture of CaF{sub 2} and LiF powders was used as flux. The thickness of the cladded layers was in the range of 2–2.2 mm. The structure of the layers was studied using optical microscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), and X-ray diffraction (XRD). The microhardness after cladding of the layers fabricated by cladding of Ti and graphite powders was 8–9 GPa, while the microhardness of layers with Mo additions reached 11–12 GPa. The highest wear resistance at sliding friction and friction in abrasive environment was reached in the samples fabricated using Ti, Mo and graphite mixture due to the higher hardness and the martensite–austenite structure of the matrix. The wear resistance against fixed abrasive particles was 2.4 times higher compared to that of carburized and quenched steel. - Highlights: • Ti, C and Mo mixture of powders was cladded using non-vacuum electron beam treatment. • The depth of the cladded layers was 2.0 … 2.2 mm. • The microhardness of layer with Mo, Ti and C additions reached ~ 11 … 12 GPa. • The hardening of the layers caused by the formation of TiC particles and martensitic matrix • Wear resistance of cladded coatings was 2.4 higher than carburized steel.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Co-transport of water and p-xylene through carbon molecular sieve membranes

Carbon molecular sieve (CMS) materials are a potential candidate for scalable and high-performance reverse osmosis membranes due to their impressive chemical and thermal stabilities. Moreover, they have the potential to enable impressive rejections of small neutral solutes from water based on their known ability to separate small organic molecules. CMS has been extensively examined for gas and organic solvent separations, but the transport of organic and aqueous mixtures through CMS microstructures is poorly understood. In this work, we investigated the sorption, diffusion, and permeation behavior of organic compounds and water in poly(vinylidene fluoride)(PVDF)-derived CMS (PVDF-CMS). Experimental observations of diffusion, sorption, and permeation shows how the properties of penetrants such as polarity and molecular size affect the transport rates and selectivity. These basic transport and sorption parameters are utilized in sorption-diffusion models to permeation rates of water-organic mixtures in CMS membranes. The transport of water and p-xylene in CMS was experimentally confirmed to follow the sorption-diffusion mechanism. The sorption-diffusion model ideal permselectivity indicates that the CMS is p-xylene selective over water. Water/p-xylene mixture permeation experiments revealed an increased selectivity of p-xylene over water, thus providing tentative evidence for a competitive sorption-selective separation mechanism. Furthermore, this work suggests that CMS membranes exhibit organic-permeable separation properties in water/organic separations. The results presented here highlight the potential for the removal of dilute organics in water via CMS pervaporation membranes.

02 PETROLEUM↗

DOE OSTI2018

Reversible adsorption of nitrogen dioxide within a robust porous metal–organic framework

Nitrogen dioxide (NO 2 ) is a major air pollutant causing significant environmental and health problems. We report reversible adsorption of NO 2 in a robust metal–organic framework. Under ambient conditions, MFM-300(Al) exhibits a reversible NO 2 isotherm uptake of 14.1 mmol g -1 , and, more importantly, exceptional selective removal of low-concentration NO 2 (5,000 to <1 ppm) from gas mixtures. Complementary experiments reveal five types of supramolecular interaction that cooperatively bind both NO 2 and N 2 O 4 molecules within MFM-300(Al). We find that the in situ equilibrium 2NO 2 ↔ N 2 O 4 within the pores is pressure-independent, whereas ex situ this equilibrium is an exemplary pressure-dependent first-order process. The coexistence of helical monomer–dimer chains of NO 2 in MFM-300(Al) could provide a foundation for the fundamental understanding of the chemical properties of guest molecules within porous hosts. Lastly, this work may pave the way for the development of future capture and conversion technologies.

36 MATERIALS SCIENCE↗

DOE OSTI2017

A Method for Identifying Prevalent Chemical Combinations in the U.S. Population

Background: Through the food and water they ingest, the air they breathe, and the consumer products with which they interact at home and at work, humans are exposed to tens of thousands of chemicals, many of which have not been evaluated to determine their potential toxicities. Furthermore, while current chemical testing tends to focus on individual chemicals, the exposures that people actually experience involve mixtures of chemicals. Unfortunately, the number of mixtures that can be formed from the thousands of environmental chemicals is enormous, and testing all of them would be impossible. Objectives: We seek to develop and demonstrate a method for identifying those mixtures that are most prevalent in humans. Methods: We applied frequent itemset mining, a technique traditionally used for market basket analysis, to biomonitoring data from the 2009–2010 cycle of the continuous National Health and Nutrition Examination Survey (NHANES) to identify combinations of chemicals that frequently co-occur in people. Results: We identified 90 chemical combinations consisting of relatively few chemicals that occur in at least 30% of the U.S. population, as well as three supercombinations consisting of relatively many chemicals that occur in a small but nonnegligible proportion of the U.S. population. Conclusions: We demonstrated how FIM can be used in conjunction with biomonitoring data to narrow a large number of possible chemical combinations down to a smaller set of prevalent chemical combinations. https://doi.org/10.1289/EHP1265

54 ENVIRONMENTAL SCIENCES↗

NASA NTRS1976

Rates of reactions ClO + ClO yields Cl2 + O2 and ClO + O yields Cl + O2 at elevated temperatures

Results are reported for an experiment in which a shock tube was employed to measure the reaction rates of chlorine-oxygen systems at high temperatures. In this experiment, a mixture of chlorine and ozone, diluted by oxygen and argon, was heated by two consecutive shock waves (primary and reflected) to produce a temperature in the range from 1000 to 1400 K and a pressure of between 3.5 and 9 atm. The reflected shock thermally decomposed the ozone; the resulting atomic oxygen reacted with molecular chlorine to produce ClO; and the variation in ClO concentration after passage of the reflected shock was observed by monitoring the intensity of 2537-A radiation passing through the test gas. The rates of the two cited reactions are deduced from the variation pattern. The rate coefficient values are found to be compatible with existing data obtained in lower pressure and temperature ranges.

Park, C.↗

NASA NTRS1977

Io's surface composition based on reflectance spectra of sulfur/salt mixtures and proton-irradiation experiments

Available full-disk reflectance spectra of Io in the range 0.3 to 2.5 microns have been used to determine a surface compositional model for Io that is consistent with Io's other known chemical and physical properties. Results indicate that the surface of Io contains abundant dehydrated salts of high Na, Mg, and Fe(3+) content such as bloedite and ferrous iron sulfate. Experiments were performed studying the irradiation damage effects from low-energy proton bombardment, since Io is immersed in Jupiter's magnetosphere.

Nash, D. B.↗

NASA NTRS1979

Interpretation of the characteristics of ocean-dumped sewage sludge related to remote sensing

Wastewater sludge characteristics in general, and characteristics of wastewater sludges generated by the City of Philadelphia in particular, were addressed. The types and sources of wastewater sludges, a description of sludge treatment and disposal processes, examination of sludge generation and management for the City of Philadelphia, and definition of characteristics for typical east coast sludges undergoing ocean disposal were discussed. Specific differences exist between the characteristics of primary and secondary wastewater sludges, especially with the nature and size distribution of the solids particles. The sludges from the City of Philadelphia monitored during remote sensing experiments were mixtures of various sludge types and lacked distinguishing characteristics. In particular, the anaerobic digestion process exerted the most significant influence on sludge characteristics for the City of Philadelphia. The sludges generated by the City of Philadelphia were found to be typical and harbor no unique features.

Pagoria, P. S.↗

NASA NTRS1984

A radiatively pumped CW CO2 laser

A proof of principle experiment to demonstrate the physics of a radiatively pumped laser has been carried out. For the first time, a blackbody cavity has optically pumped a CW CO2 laser. Results are presented from a series of experiments using mixtures of CO2, He, and Ar in which maximum output power was obtained with a 20 percent CO2-15 percent He-65 percent Ar mixture. The dependence of the output power on the blackbody temperature and the cooling gas flow rate is also discussed. By appropriately varying these parameters, continuous output powers of 8-10 mW have been achieved.

Insuik, R. J.↗

NASA NTRS1989

Diffusion and infrared properties of molecules in ice mantles

Within dense molecular clouds the formation of frozen icy mantles on interstellar dust grains is thought to be the result of various growth conditions. The molecules, which make up the ice mantles are probably completely mixed. To study the physical properties of such ice mixtures the experiments were performed on the evaporation processes and on the spectroscopic properties of CO, CO2, and CH4 in water rich ices. The decrease in concentration of volatile molecules in ice samples deposited at 10 K and subsequently heated is found to occur essentially in two steps. The first one, corresponding to an evaporation of part of the volatile molecules, starts at about 25 K for CO, 32 K for CH4, and 70 K for CO2. During the crystallization of H2O ice at temperatures greater than 120 K a second evaporation occurs leading to the complete disappearance of the volatile molecules in the solid phase. The main astrophysical implications of the diffusion and spectroscopic behaviors are presented. The possible effects of a heating source on the fraction of volatile molecules, such as CO trapped in grain mantles, are discussed.

Schmitt, Bernard↗

NASA NTRS1994

Powder agglomeration in a microgravity environment

This is the final report for NASA Grant NAG3-755 entitled 'Powder Agglomeration in a Microgravity Environment.' The research program included both two types of numerical models and two types of experiments. The numerical modeling included the use of Monte Carlo type simulations of agglomerate growth including hydrodynamic screening and molecular dynamics type simulations of the rearrangement of particles within an agglomerate under a gravitational field. Experiments included direct observation of the agglomeration of submicron alumina and indirect observation, using small angle light scattering, of the agglomeration of colloidal silica and aluminum monohydroxide. In the former class of experiments, the powders were constrained to move on a two-dimensional surface oriented to minimize the effect of gravity. In the latter, some experiments involved mixture of suspensions containing particles of opposite charge which resulted in agglomeration on a very short time scale relative to settling under gravity.

Cawley, James D.↗

NASA NTRS1999

Simulation of Unsteady Hypersonic Combustion Around Projectiles in an Expansion Tube

The temporal evolution of combustion flowfields established by the interaction between wedge-shaped bodies and explosive hydrogen-oxygen-nitrogen mixtures accelerated to hypersonic speeds in an expansion tube is investigated. The analysis is carried out using a fully implicit, time-accurate, computational fluid dynamics code that we developed recently for solving the Navier-Stokes equations for a chemically reacting gas mixture. The numerical results are compared with experimental data from the Stanford University expansion tube for two different gas mixtures at Mach numbers of 4.2 and 5.2. The experimental work showed that flow unstart occurred for the Mach 4.2 cases. These results are reproduced by our numerical simulations and, more significantly, the causes for unstart are explained. For the Mach 5.2 mixtures, the experiments and numerical simulations both produced stable combustion. However, the computations indicate that in one case the experimental data were obtained during the transient phase of the flow; that is, before steady state had been attained.

Yungster, S.↗

NASA NTRS1999

Spacelab Science Results Study: External Observations - Volume 1

Some of the 36 Spacelab missions were more or less dedicated to specific scientific disciplines, while other carried a eclectic mixture of experiments ranging from astrophysics to life sciences. However, the experiments can be logically classified into two general categories; those that make use of the Shuttle as an observing platform for external phenomena (including those which use the Shuttle in an interactive mode) and those which use the Shuttle as a microgravity laboratory. This first volume of this Spacelab Science Results study will be devoted to experiments of the first category. The disciplines included are Astrophysics, Solar Physics, Space Plasma Physics, Atmospheric Sciences, and Earth Sciences. Because of the large number of microgravity investigations, Volume 2 will be devoted to Microgravity Sciences, which includes Fluid Physics, Combustion Science, Materials Science, and Biotechnology, and Volume 3 will be devoted to Space Life Sciences, which studies the response and adaptability of living organisms to the microgravity environment.

Naumann, Robert J.↗

NASA NTRS1999

Coarsening in Solid-Liquid Mixtures Studied on the Space Shuttle

Ostwald ripening, or coarsening, is a process in which large particles in a two-phase mixture grow at the expense of small particles. It is a ubiquitous natural phenomena occurring in the late stages of virtually all phase separation processes. In addition, a large number of commercially important alloys undergo coarsening because they are composed of particles embedded in a matrix. Many of them, such as high-temperature superalloys used for turbine blade materials and low-temperature aluminum alloys, coarsen in the solid state. In addition, many alloys, such as the tungsten-heavy metal systems, coarsen in the solid-liquid state during liquid phase sintering. Numerous theories have been proposed that predict the rate at which the coarsening process occurs and the shape of the particle size distribution. Unfortunately, these theories have never been tested using a system that satisfies all the assumptions of the theory. In an effort to test these theories, NASA studied the coarsening process in a solid-liquid mixture composed of solid tin particles in a liquid lead-tin matrix. On Earth, the solid tin particles float to the surface of the sample, like ice in water. In contrast, in a microgravity environment this does not occur. The microstructures in the ground- and space-processed samples (see the photos) show clearly the effects of gravity on the coarsening process. The STS-83-processed sample (right image) shows nearly spherical uniformly dispersed solid tin particles. In contrast, the identically processed, ground-based sample (left image) shows significant density-driven, nonspherical particles, and because of the higher effective solid volume fraction, a larger particle size after the same coarsening time. The "Coarsening in Solid-Liquid Mixtures" (CSLM) experiment was conducted in the Middeck Glovebox facility (MGBX) flown aboard the shuttle in the Microgravity Science Laboratory (MSL-1/1R) on STS-83/94. The primary objective of CSLM is to measure the temporal evolution of the solid particles during coarsening.

Caruso, John J.↗

NASA NTRS2022

Flow Visualization, Heat Transfer, and Critical Heat Flux of Flow Boiling in Earth Gravity with Saturated Liquid-Vapor Mixture Inlet Conditions – In Preparation for Experiments Onboard the International Space Station

This study investigates flow boiling of n-Perfluorohexane with saturated two-phase mixture inlet in a rectangular channel of dimensions 114.6-mm heated length, 2.5-mm width, and 5 mm-height. The experiments were performed as part of the Mission Sequence Testing of the Flow Boiling and Condensation Experiment’s (FBCE) Flow Boiling Module (FBM) in the vertical upflow configuration in Earth gravity using the same experimental system that was launched to the International Space Station (ISS) in August 2021. The operating parameters varied are heating configuration (single- and double-sided), mass velocity (380 – 2400 kg/m2s), inlet quality (0.011 – 0.519), and inlet pressure (120 – 179 kPa). High-speed video photographs are presented to explain the two-phase flow patterns within the channel’s heated length. Flow patterns are constituted by low-density and high-density fronts moving along the channel, with the high-density fronts gradually reducing in length due to evaporation. Heat transfer results in terms of flow boiling curves, streamwise wall temperature profiles, streamwise heat transfer coefficient profiles, and average heat transfer coefficients are presented and trends discussed. CHF data from the present experiments are combined with prior databases to compile a consolidated FBCE-CHF database for saturated inlet to expand the ranges of operating conditions and include other flow orientations in Earth gravity. Experimental CHF trends are also discussed. The interfacial lift-off model shows a good CHF predictive accuracy evidenced by a mean absolute error of 11.97% for this consolidated database after constraining it to mass velocities greater than or equal to 500 kg/m2s. Finally, this study confirmed reliability of the upcoming ISS experiments for saturated inlet conditions and the collected Earth-gravity data will be compared to ISS microgravity data.

Flow boiling↗

DOE OSTI2016

In Memoriam: John A. Cornell (1941-2016)

This is an article in memory of John A. Cornell (1941-2016) to be published in the Journal of Quality Technology (of which John was a past editor).

Mixture experiments↗

NASA NTRS1994

Shock recovery analogs and the origin of mesosiderites

The origin of mesosiderites, which consist of approximately equal-weight proportions of Fe-Ni metal and silicates (gabbros, basalts, orthopyroxenites, dunites), remains an interesting and complex problem in meteoritics. There is general agreement that multiple impact events were probably involved in the formation of these brecciated stony-iron meteorites, but given the heterogeneity of mesosiderites, additional processes have been invoked to explain the unique and intricate textural and compositional makeup of mesosiderites. We conducted a series of shock recovery experiments to test the impact event(s) scenario. The results indicated significant similarities between the shocked analogs and many mesosiderites. We have compared our analogs with a suite of thin sections of Barea mesosiderite. I have conducted a series of flash heating experiments in which equal-weight proportions of gabbro and stainless steel (SS304) powders were compressed into small charges and heated under reducing conditions for short times. These experiments were used to bracket localized, peak postshock temperatures in our analog shots and to compare the mixing relations between the silicate and metal. The shock recovery experiments used porous metal-silicate powder starting mixtures, therefore our experiments are most analogous to an impact scenario where the target is an asteroidal regolith surface composed of a loose mixture of Fe-Ni metal and heterogeneous silicates. Analog experiments may really describe a secondary impact process similar to the late-stage, localized impact melting event. This leaves one of the crucial questions about mesosiderite genesis unanswered, namely what is the source of the Fe-Ni metal that is so intimately distributed in these meteorites?

Rowan, L. R.↗

NASA NTRS1973

Phase equilibria in molecular hydrogen-helium mixtures at high pressures

Experiments on phase behavior in hydrogen-helium mixtures have been carried out at pressures up to 9.3 kilobars, at temperatures from 26 to 100 K. Two distinct fluid phases are shown to exist at supercritical temperatures and high pressures. Both the trend of the experimental results and an analysis based on the van der Waals theory of mixtures suggest that this fluid-fluid phase separation persists at temperatures and pressures beyond the range of these experiments, perhaps even to the limits of stability of the molecular phases. The results confirm earlier predictions concerning the form of the hydrogen-helium phase diagram in the region of pressure-induced solidification of the molecular phases at supercritical temperatures. The implications of this phase diagram for planetary interiors are discussed.

Streett, W. B.↗

DOE OSTI2011

GENPLAT: an Automated Platform for Biomass Enzyme Discovery and Cocktail Optimization

The high cost of enzymes for biomass deconstruction is a major impediment to the economic conversion of lignocellulosic feedstocks to liquid transportation fuels such as ethanol. We have developed an integrated high throughput platform, called GENPLAT, for the discovery and development of novel enzymes and enzyme cocktails for the release of sugars from diverse pretreatment/biomass combinations. GENPLAT comprises four elements: individual pure enzymes, statistical design of experiments, robotic pipeting of biomass slurries and enzymes, and automated colorimeteric determination of released Glc and Xyl. Individual enzymes are produced by expression in Pichia pastoris or Trichoderma reesei, or by chromatographic purification from commercial cocktails or from extracts of novel microorganisms. Simplex lattice (fractional factorial) mixture models are designed using commercial Design of Experiment statistical software. Enzyme mixtures of high complexity are constructed using robotic pipeting into a 96-well format. The measurement of released Glc and Xyl is automated using enzyme-linked colorimetric assays. Optimized enzyme mixtures containing as many as 16 components have been tested on a variety of feedstock and pretreatment combinations. GENPLAT is adaptable to mixtures of pure enzymes, mixtures of commercial products (e.g., Accellerase 1000 and Novozyme 188), extracts of novel microbes, or combinations thereof. To make and test mixtures of ˜10 pure enzymes requires less than 100 μg of each protein and fewer than 100 total reactions, when operated at a final total loading of 15 mg protein/g glucan. We use enzymes from several sources. Enzymes can be purified from natural sources such as fungal cultures (e.g., Aspergillus niger, Cochliobolus carbonum, and Galerina marginata), or they can be made by expression of the encoding genes (obtained from the increasing number of microbial genome sequences) in hosts such as E. coli, Pichia pastoris, or a filamentous fungus such as T. reesei. Proteins can also be purified from commercial enzyme cocktails (e.g., Multifect Xylanase, Novozyme 188). An increasing number of pure enzymes, including glycosyl hydrolases, cell wall-active esterases, proteases, and lyases, are available from commercial sources, e.g., Megazyme, Inc. (www.megazyme.com), NZYTech (www.nzytech.com), and PROZOMIX (www.prozomix.com). Design-Expert software (Stat-Ease, Inc.) is used to create simplex-lattice designs and to analyze responses (in this case, Glc and Xyl release). Mixtures contain 4-20 components, which can vary in proportion between 0 and 100%. Assay points typically include the extreme vertices with a sufficient number of intervening points to generate a valid model. In the terminology of experimental design, most of our studies are "mixture" experiments, meaning that the sum of all components adds to a total fixed protein loading (expressed as mg/g glucan). The number of mixtures in the simplex-lattice depends on both the number of components in the mixture and the degree of polynomial (quadratic or cubic). For example, a 6-component experiment will entail 63 separate reactions with an augmented special cubic model, which can detect three-way interactions, whereas only 23 individual reactions are necessary with an augmented quadratic model. For mixtures containing more than eight components, a quadratic experimental design is more practical, and in our experience such models are usually statistically valid. All enzyme loadings are expressed as a percentage of the final total loading (which for our experiments is typically 15 mg protein/g glucan). For "core" enzymes, the lower percentage limit is set to 5%. This limit was derived from our experience in which yields of Glc and/or Xyl were very low if any core enzyme was present at 0%. Poor models result from too many samples showing very low Glc or Xyl yields. Setting a lower limit in turn determines an upper limit. That is, for a six-component experiment, if the lower limit for each single component is set to 5%, then the upper limit of each single component will be 75%. The lower limits of all other enzymes considered as "accessory" are set to 0%. "Core" and "accessory" are somewhat arbitrary designations and will differ depending on the substrate, but in our studies the core enzymes for release of Glc from corn stover comprise the following enzymes from T. reesei: CBH1 (also known as Cel7A), CBH2 (Cel6A), EG1(Cel7B), BG (βglucosidase), EX3 (endo-β1,4-xylanase, GH10), and BX (β-xylosidase).

09 BIOMASS FUELS↗