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At least 1,063 records · Page 59
All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Microstructural evolution in a precipitate-hardened (Fe 0.3 Ni 0.3 Mn 0.3 Cr 0.1 ) 94 Ti 2 Al 4 multi-principal element alloy during high-pressure torsion

Multi-principal element alloys demonstrate high strength, thermal stability, and irradiation resistance, making them excellent candidate materials for applications in nuclear reactors and other harsh environments. Some studies have examined the use of high-pressure torsion to strengthen MPEAs through grain size reduction and strain hardening. However, no studies have investigated the effect of HPT on secondary phases (precipitates) within an MPEA. Two alloys, (Fe 0.3 Ni 0.3 Mn 0.3 Cr 0.1 ) 94 Ti 2 Al 4 containing Ni(Ti, Al) B2 phase, and CrFe σ phase, and single-phase Fe 0.3 Ni 0.3 Mn 0.3 Cr 0.1 , were fabricated by casting and heat treatment. Both alloys were then processed with HPT to study microstructural evolution. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) were used to characterize the alloys before and after HPT processing. HPT processing produced a nanocrystalline structure in both alloys, but (Fe 0.3 Ni 0.3 Mn 0.3 Cr 0.1 ) 94 Ti 2 Al 4 exhibited a significantly smaller grain size and higher dislocation density than Fe 0.3 Ni 0.3 Mn 0.3 Cr 0.1 , with corresponding higher hardness. Before HPT, the (Fe 0.3 Ni 0.3 Mn 0.3 Cr 0.1 ) 94 Ti 2 Al 4 alloy consisted of large grain (~ 400 μm) and precipitates, including B2 of ~ 38 μm average size, B2 of ~ 0.7 μm average size, and small amounts of σ of ~ 1.5 μm average size. After HPT, the larger B2 precipitates were decreased in size and volume fraction, while the smaller B2 precipitates were completely dissolved; the σ precipitates appeared unaffected by HPT, likely due to their much higher hardness. Finally, observation of the B2 precipitate distribution along radial distance indicates that the strain caused the precipitates to fracture at intermediate strain (γ = 125) and dissolve at high strain (γ = 280).

36 MATERIALS SCIENCE↗
DOE OSTI2018

Spectroscopic and Theoretical Studies of Fluorescence Effects in 2-Methylamino-5-(2,4-dihydroxyphenyl)-1,3,4-thiadiazole Induced by Molecular Aggregation

The article presents the results of fluorescence analyses of 2-methylamino-5-(2,4-dihydroxyphenyl)-1,3,4-thiadiazole (MDFT) in an aqueous environment. MDFT dissolved in aqueous solutions with a pH value in the range from 1 to 4.5 yielded an interesting effect of two clearly separated fluorescence emissions. In turn, a single fluorescence was observed in MDFT dissolved in water solutions with a pH value from 4.5 to 12. As it was suggested in the previous investigations of other 1,3,4-thiadiazole compounds, these effects may be associated with conformational changes in the structure of the analysed molecule accompanied by aggregation effects. Crystallographic data showed that the effect of the two separated fluorescence emissions occurred in a conformation with the –OH group in the resorcyl ring bound on the side of the sulphur atom from the 1,3,4-thiadiazole ring. The hypothesis of aggregation as the mechanism involved in the change in the spectral properties at low pH is supported by the results of (Time-Dependent) Density Functional Theory calculations. The possibility of rapid analysis of conformational changes with the fluorescence spectroscopy technique may be rather important outcome obtained from the spectroscopic studies presented in this article. Additionally, the presented results seem to be highly important as they can be easily observed in solutions and biologically important samples.

74 ATOMIC AND MOLECULAR PHYSICS↗
DOE OSTI2019

Ce-Doping and Reduction Annealing Effects on Magnetic Properties of Pr{sub 2-x}Ce{sub x}CuO{sub 4} Nanoparticles

Magnetic properties of reduced T’-Pr{sub 2-x}Ce{sub x}CuO{sub 4} (T’-PCCO) nanoparticles with x = 0, 0.10, and 0.15 have been investigated. The T’-PCCO samples were synthesized by the chemically dissolved method with HNO{sub 3} as dissolving agents and by the succeeding calcination at 1000 °C for 15 h in air. The reduced T’-PCCO samples were obtained by the reduction annealing at 700 °C for 10 h in Argon atmosphere and at 700 °C for 12 h in vacuum. Rietveld analyses of the X-ray diffraction (XRD) patterns for all the samples have revealed dependences of the c-axis length and the crystal size on the Ce doping and the reduction annealing. XRD analyses and transmission electron microscopy (TEM) images have confirmed T’-PCCO nanoparticles with the size of around 40–100 nm. Magnetic properties of all the T’-PCCO nanoparticles were studied by a superconducting quantum interference device (SQUID) showing a dominant paramagnetic feature with very weak ferromagnetism in the as-synthesized samples at room temperature. It has changed to a pure paramagnetic feature after the reduction annealing in argon atmosphere and an enhanced ferromagnetism through vacuum annealing. This is probably due to the change in the number of oxygen vacancies through the defect recovery and the removal of excess oxygen after both reduction annealing processes, respectively.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2015

Dissolution of aerosol particles collected from nuclear facility plutonium production process

Here, a simple, robust analytical chemistry method has been developed to dissolve plutonium containing particles in a complex matrix. The aerosol particles collected on Marple cascade impactor substrates were shown to be dissolved completely with an acid mixture of 12 M HNO 3 and 0.1 M HF. A pressurized closed vessel acid digestion technique was utilized to heat the samples at 130 °C for 16 h to facilitate the digestion. The dissolution efficiency for plutonium particles was 99 %. The resulting particle digestate solution was suitable for trace elemental analysis and isotope composition determination, as well as radiochemistry measurements.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗
DOE OSTI2016

Assay Methods for 238U, 232Th, and 210Pb in Lead and Calibration of 210Bi Bremsstrahlung Emission from Lead

Assay methods for measuring 238U, 232Th, and 210Pb concentrations in refined lead are presented. The 238U and 232Th concentrations are assayed via inductively coupled plasma mass spectrometry (ICP-MS) after anion exchange column separation on dissolved lead samples. The 210Pb concentration is inferred through α-spectroscopy of a daughter isotope, 210Po, after chemical precipitation separation on dissolved lead samples. Subsequent to the 210Po α-spectroscopy assay, a method for evaluating 210Pb concentrations in solid lead samples was developed via measurement of bremsstrahlung radiation from β-decay of a daughter isotope, 210Bi, by employing a 14-crystal array of high purity germanium (HPGe) detectors. Ten sources of refined lead were assayed. The 238U concentrations were <34 microBq/kg and the 232Th concentrations ranged <0.6 – 15 microBq/kg, as determined by the ICP-MS assay method. The 210Pb concentrations ranged from ~0.1 – 75 Bq/kg, as inferred by the 210Po α-spectroscopy assay method.

Orrell, John L.↗
DOE OSTI2019

Irradiation and isolation of fission products from uranium metal–organic frameworks

Typical fission product formation experiments utilize metal or oxide target materials that must be dissolved prior to product separation. In this study, we report here a novel study using metal–organic frameworks for recovery of fission products into acidic media. We further show that the frameworks are largely preserved, such that this bulk target material could be retained for additional irradiations or characterizations. Through this approach, fission products can be separated from the actinide-based metal–organic framework using 0.01 M HNO 3 without the need to dissolve the framework itself, reducing the amount of acidic waste. Extraction yields of four frameworks with varying pore sizes are compared. In conclusion, the results suggest that it may be possible to use porous frameworks as target materials for the extraction of select fission products.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗
DOE OSTI2025

Real-time gross actinide monitoring in extreme (10 6 :1) beta-gamma background fluid streams using mini-ATMFDs

Real-time, trace alpha activity monitoring in extreme mixed radiation fields is a well-known challenge in fission product-rich streams containing mixtures of beta-gamma-alpha radiation-emitting isotopes, arising due to the extreme 10 6 :1 ratio of background beta-gamma vs. alpha radiation activity levels. This paper presents results from a novel approach to addressing this challenge, based on Tensioned Metastable Fluid Detector (TMFD) sensing technology. An acoustically driven technique was developed and tested at Purdue University (using dissolved Rn-Po and U-chain alpha emitters), and validated (with dissolved Pu) at Savannah River National Laboratory for real-time monitoring of alpha activity in the 100–10,000 dpm/mL range.

Environmental Monitoring↗
DOE OSTI2019

RDX solubility in TNT at high temperatures

The solubility of RDX (hexahydro-1,3,5-tri-nitro-1,3,5-triazine) in TNT (2,4,6-trinitrotoluene) at elevated temperatures is required to accurately predict the response of Comp-B 3 (60:40 RDX:TNT) during accidents involving fire. As the temperature increases, the TNT component melts, the RDX partially dissolves in the liquid TNT, and the remaining RDX melts (203 °C) as the Comp-B thermally ignites. In the current work, we used a differential scanning calorimeter (DSC) to estimate the solubility of RDX in TNT at the melting point of RDX. Most DSC measurements of Comp-B 3 do not show an RDX melt endotherm. The absence of an endotherm associated with the RDX melt has been interpreted as RDX being completely dissolved in TNT before reaching the melting point. Here, we have observed that the endotherm is not absent, but is masked by exothermic reactions occurring at these elevated temperatures. We have inhibited the exothermic reactions by venting our DSC samples and measuring the RDX melt endotherm in our Comp-B 3 samples at about 203 °C. Using the measured heat flow associated with the RDX melt and the latent melting enthalpy of RDX, we have approximated the solubility of RDX in TNT to be roughly 50–100 g RDX per 100 g TNT . The broad range is based on corrections for exothermic reactions occurring as the RDX melts.

42 ENGINEERING↗
DOE OSTI2018

Photochromic transformations of amphiphilic spiropyran in acetonitrile solutions and at the air/water interface

The results of a study of the photochromic properties of 1´-hexadecyl-3´,3´-dimethyl-6-nitro-1´,3´-dihydrospiro[chromene-2,2´-indole] (SP) are presented. The kinetic characteristics of photophysical processes occurring in acetonitrile solution of SP upon irradiation with UV light and during dark relaxation are determined. It is shown that spiropyran modified at the nitrogen atom by a long-chain hydrocarbon radical exhibits photochromic properties in the dissolved state, with the rate of the direct photocoloration exceeding the rate of dark relaxation by an order of magnitude. Comparative studies of SP photoreaction in dissolved and 2D states are carried out. The obtained results open up broad prospects for application of such photochromes in thin-film devices obtained using the Langmuir monolayer technique.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2011

Transport of Explosive Residue Surrogates in Saturated Porous Media

Department of Defense operational ranges may become contaminated by particles of explosives residues (ER) as a result of low-order detonations of munitions. The goal of this study was to determine the extent to which particles of ER could migrate through columns of sandy sediment, representing model aquifer materials. Transport experiments were conducted in saturated columns (2×20 cm) packed with different grain sizes of clean sand or glass beads. Fine particles (approximately 2 to 50 μm) of 2,6- dinitrotoluene (DNT) were used as a surrogate for ER. DNT particles were applied to the top 1 cm of sand or beads in the columns, and the columns were subsequently leached with artificial groundwater solutions. DNT migration occurred as both dissolved and particulate phases. Concentration differences between unfiltered and filtered samples indicate that particulate DNT accounted for up to 41% of the mass recovered in effluent samples. Proportionally, more particulate than dissolved DNT was recovered in effluent solutions from columns with larger grain sizes, while total concentrations of DNT in effluent were inversely related to grain size. Of the total DNT mass applied to the uppermost layer of the column, <3% was recovered in the effluent with the bulk remaining in the top 2 cm of the column. Our results suggest there is some potential for subsurface migration of ER particles and that most of the particles will be retained over relatively short transport distances.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2025

Dissolution of Nb(C,N) and (Ti,V)N in the Coarse-Grained Heat-Affected Zone of Electric Resistance Welded X65 Line Pipe

Nb-rich and Ti/V-rich precipitates were introduced into the X65 linepipe via thermomechanical controlled processing. Their dissolution kinetics were investigated in the coarse-grained heat-affected zone after electric resistance welding. Nb-rich precipitates were found to dissolve completely, whereas Ti/V-rich precipitates were found to dissolve partially, because of slower dissolution kinetics. In conclusion, a complete dissolution of Nb-rich precipitates was associated with significant austenite grain coarsening, which promoted bainite as a quench product, which might have reduced the impact toughness.

microstructure↗
DOE OSTI2018

Model of Inclusion Evolution During Calcium Treatment in the Ladle Furnace

Calcium treatment of steel is typically employed to modify alumina inclusions to liquid calcium aluminates. However, injected calcium also reacts with the dissolved sulfur to form calcium sulfide. The current work aims to develop a kinetic model for the evolution of oxide and sulfide inclusions in Al-killed alloyed steel during Ca treatment in the ladle refining process. The model considers dissolution of the calcium from the calcium bubbles into the steel and reduction of calcium oxide in the slag to dissolved calcium. A steel–inclusion kinetic model is used for mass transfer to the inclusion interface and diffusion within the calcium aluminate phases formed on the inclusion. The inclusion–steel kinetic model is then coupled with a previously developed steel–slag kinetic model. The coupled inclusion–steel–slag kinetic model is applied to the chemical composition changes in molten steel, slag, and evolution of inclusions in the ladle. The result of calculations is found to agree well with an industrial heat for species in the steel as well as inclusions during Ca treatment.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Manufacturing of Dysprosium-Iron Alloys by Electrolysis in Fluoride-Based Electrolytes. Electrolysis in a Laboratory-Scale Cell

Electrolytic production of light rare earth elements and rare earth alloys with transition elements takes place in a fluoride-based electrolyte using rare earth oxides as raw material. The optimization of this method, mainly in terms of the energy efficiency and environmental impact control, is rather challenging. Anode effects, evolution of fluorine-containing compounds and side cathode reactions could largely be minimized by good control of the amount of rare earth oxide species dissolved in the fluoride-based electrolyte and their dissolution rate. The Dy{sub 2}O{sub 3} feed rate needed for stable cell operation was studied by following up the anode voltage and gas analysis. On-line analysis of the cell off-gases by FTIR showed that the electrochemical reaction for the formation of Dy-Fe alloy gives mainly CO gas and that CF{sub 4} is starting to evolve gradually at anode voltages of ca. 3.25 V. The limiting current density for the discharge of the oxide ions at the graphite anode was in the range of 0.1 to 0.18 A cm{sup −2} at dissolved Dy{sub 2}O{sub 3} contents of ca. 1 wt pct. Modeling of the laboratory cell reactor was also carried out by implementing two models, i.e., an electrical model simulating the current density distribution at the electrodes and a laminal bubbly flow model that explains the electrolyte velocity induced by gas bubble production at the anode.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Dissolution Behavior of Iron and Steel Materials in Liquid Magnesium

The dissolution of metallic elements from Fe and steel materials into pure liquid Mg was investigated with the aim of improving control of impurities in Mg during processes such as Mg-alloy production and Ti smelting. Pure Mg was melted between 1073 and 1323 K (800 and 1050 °C) for 24 to 96 hours in closed crucibles made of pure Fe, low-carbon steel, or austenitic stainless steel SUS316. From the experiments using the pure Fe crucible, the relationship between the solubility of Fe in liquid Mg [C{sub sol,Fe} (mass pct)] and temperature [T (K)] was determined to be log(C{sub sol,Fe}) = − 3.67 × 10{sup 3}/T + 2.48 (± 0.06), from which the standard Gibbs energy of Fe dissolution in liquid Mg was evaluated. The amount of Fe dissolved from low-carbon steel was the same as that from pure Fe. From SUS316, not only Fe but also Cr and Ni dissolved into liquid Mg; the Fe and Cr concentrations in liquid Mg did not change significantly over time, whereas the Ni concentration increased monotonically. Preferential Ni dissolution resulted in a Ni-poor layer on the SUS316 surface. Finally, using the experimental data of Fe dissolution from low-carbon steel, the Fe contamination route in the current Ti smelting process, where a large amount of Mg is used as a reducing agent, is discussed.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Dissolution Behavior and Phase Evolution During Aluminum Oxide Dissolution in BOF Slag

Basic oxygen furnace (BOF) slag is a byproduct in the steel making process and is produced in considerable amounts. Thus, its valorization is important. Additives such as Al{sub 2}O{sub 3} can be utilized to modify the composition and mineralogy of the slag provided that a fast and effective dissolution of these additives in molten slags can be ensured. With this in mind, the dissolution of Al{sub 2}O{sub 3} particles in molten BOF slag has been investigated between 1500 and 1600 °C. In all cases, a dissolution zone forms around the dissolving particle which limits the dissolution rate in the melt under natural convection conditions. The dissolution in the current system is found to be an indirect process, wherein crystalline reaction products like CaAl{sub 4}O{sub 7} (CA{sub 2}) and CaAl{sub 2}O{sub 4} (CA) form on the surface of the particles. CA forms at 1500 °C and CA{sub 2} at 1600 °C. These reaction products form a continuous layer on the surface of the dissolving particles but the thickness of this reaction layer remains limited. The experimental data have been utilized to evaluate the dissolution paths. Near the Al{sub 2}O{sub 3}/slag interface, the inter-diffusion of Al{sub 2}O{sub 3} and CaO occurs due to which the dissolution path shifts towards the Al{sub 2}O{sub 3}-CaO binary system. A phenomenological model is presented to explain the evolution of the dissolution process in the current system, wherein the kinetics of the process is used to explain the reaction products formed at 1500 °C and 1600 °C.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Formation Mechanism of Al{sub 2}O{sub 3}-Containing Inclusions in Al-Deoxidized Spring Steel

The source, characteristics, and mechanism of Al{sub 2}O{sub 3}-containing inclusions in Al-deoxidized spring steel were investigated using electron-probe X-ray microanalysis (EPMA). Spring samples were collected during vacuum degassing (VD) refining, in a tundish ladle, and after hot rolling, respectively. Based on primary inclusion components, seven types of inclusions were observed through the manufacturing process: Al{sub 2}O{sub 3}, Al{sub 2}O{sub 3}-SiO{sub 2}, Al{sub 2}O{sub 3}-CaO, Al{sub 2}O{sub 3}-MgO, Al{sub 2}O{sub 3}-MgO-CaO, Al{sub 2}O{sub 3}-SiO{sub 2}-MnO, and Al{sub 2}O{sub 3}-SiO{sub 2}-CaO. The Al{sub 2}O{sub 3} and Al{sub 2}O{sub 3}-SiO{sub 2} inclusions were mainly attributed to deoxidization products, less than 15 μm in diameter and with liquidus temperatures exceeding 1600 °C. For Al{sub 2}O{sub 3}-CaO inclusions, which were considered to be formed by the reduction of entrapped slag by Al dissolved in the steel, the Al{sub 2}O{sub 3}/CaO ratio obviously decreased with the increase of inclusion sizes. Most Al{sub 2}O{sub 3}-SiO{sub 2}-CaO inclusions were less than 15 μm in diameter, with their composition close to that of the refining slag and a liquidus temperature near 1500 °C. The Al{sub 2}O{sub 3}-MgO and Al{sub 2}O{sub 3}-SiO{sub 2}-MnO inclusions originated from inherent reactions between dissolved [Al], [Si], [Mn], [Mg], and [O] in the steel. Al{sub 2}O{sub 3}-MgO-CaO inclusions resulted from coalescence between Al{sub 2}O{sub 3}-MgO and Al{sub 2}O{sub 3}-CaO inclusions.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Effects of Solution Treatment on Microstructure Transformation, Tensile and Exfoliation Corrosion Properties of 7136 Aluminum Alloy

The effects of solution treatment on microstructure transformation and tensile properties of 7136 aluminum alloys were investigated by means of scanning electron microscopy, electron backscatter diffraction, differential scanning calorimeter, x-ray diffraction and tensile test, electrochemical evaluations, exfoliation corrosion tests, respectively. The results indicate that solution treatment had a significant effect on the microstructure transformation and tensile properties. Soluble constituents of 7136 aluminum alloys were more likely to form the η(MgZn{sub 2}) phase rather than the S(Al{sub 2}CuMg) phase. With increasing the solution temperature, the η phase was re-dissolved into the α(Al) matrix gradually. After solution treatment of 475 °C/1 h, the η phase was completely dissolved into the matrix, with insoluble Fe-rich phases remained. The dissolution of η phase would increase the strength and the corrosion resistance of the alloys. When continuing to increase the solution temperature, the recrystallized fraction increased obviously, resulting in the decrease in the strength and the corrosion resistance. Consequently, the strength and the corrosion resistance of the alloys increased firstly and then decreased with the increase in solution temperature. After solution treatment of 475 °C/1 h, the tensile strength and yield strength of the aged alloy reached their peaks, 738 and 715 MPa, respectively. The elongation of the alloy solution treated at 475 °C/1 h reached 11.2%, and its exfoliation corrosion rating got EB level. Furthermore, after the double-stage solution treatment of 450 °C/1 h + 475 °C/1 h, the recrystallized fraction decreased, resulting in a slight increase to 12.6% of the elongation, a slight increase in the corrosion resistance and a slight decrease in the strength.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Comparison of Internal Energy Distributions of Ions Created by Electrospray Ionization and Laser Ablation-Liquid Vortex Capture-Electrospray Ionization

Recently a number of techniques have combined laser ablation with liquid capture for mass spectrometry spot sampling and imaging applications. The newly developed non-contact liquid-vortex capture probe has been used to efficiently collect 355 nm UV laser ablated material in a continuous flow solvent stream in which the captured material dissolves and then undergoes electrospray ionization. This sampling and ionization approach has produced what appear to be classic electrospray ionization spectra; however, the softness of this sampling/ionization process versus simple electrospray ionization has not been definitely determined. A series of benzlypyridinium salts, known as thermometer ions, were used to compare internal energy distributions between electrospray ionization and the UV laser ablation liquid-vortex capture probe electrospray combination. Measured internal energy distributions were identical between the two techniques, even with differences in laser fluence (0.7-3.1 J cm-2) and when using UV-absorbing or non-UV-absorbing sample substrates. This data indicates ions formed directly by UV laser ablation, if any, are likely an extremely small constituent of the total ion signal observed. Instead, neutral molecules, clusters or particulates ejected from the surface during laser ablation, subsequently captured and dissolved in the flowing solvent stream then electrosprayed are the predominant source of ion signal observed. The electrospray ionization process used controls the softness of the technique.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗