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At least 1,153 records · Page 64
All sourcesNASA NTRSDOE OSTI
DOE OSTI2021

Fischer-Tropsch Synthesis: The Characterization and Testing of Pt-Co/SiO 2 Catalysts Prepared with Alternative Cobalt Precursors

Different low-cost cobalt precursors (acetate, chloride) and thermal treatments (air calcination/H 2 reduction versus direct H 2 -activation) were investigated to alter the interaction between cobalt and silica. H 2 -activated catalysts prepared from cobalt chloride had large Co 0 particles (XRD, chemisorption) formed by weak interactions between cobalt chloride and silica (temperature programmed reduction (TPR), TPR with mass spectrometry (TPR-MS), TPR with extended X-ray absorption fine structure (EXAFS) and X-ray absorption near edge spectroscopy (XANES) techniques) and retained Cl-blocked active sites, resulting in poor activity. In contrast, unpromoted Co/SiO 2 catalysts derived from cobalt acetate had strong interactions between Co species and silica (TPR/TPR-MS, TPR-EXAFS/XANES); adding Pt increased the extent of the Co reduction. For these Pt-promoted catalysts, the reduction of uncalcined catalysts was faster, resulting in larger Co 0 clusters (19.5 nm) in comparison with the air-calcined/H 2 -activated catalyst (7.8 nm). Both catalysts had CO conversions 25% higher than that of the Pt-promoted catalyst prepared in the traditional manner (air calcination/H 2 reduction using cobalt nitrate) and three times higher than that of the traditional unpromoted Co/silica catalyst. The retention of residual cobalt carbide (observed in XANES) from cobalt acetate decomposition impacted performance, resulting in a higher C 1 –C 4 selectivity (32.2% for air-calcined and 38.7% for uncalcined) than that of traditional catalysts (17.5–18.6%). The residual carbide also lowered the α-value and olefin/paraffin ratio. Future work will focus on improving selectivity through oxidation–reduction cycles.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2020

Bismuth Subcarbonate Decorated Reduced Graphene Oxide Nanocomposite for the Sensitive Stripping Voltammetry Analysis of Pb(II) and Cd(II) in Water

In this paper, bismuth subcarbonate (BiO)2CO3-reduced graphene oxide nanocomposite incorporated in Nafion matrix ((BiO)2CO3-rGO-Nafion) was synthesized and further applied, for the first time, in the sensitive detection of Pb(II) and Cd(II) by square-wave anodic stripping voltammetry (SWASV). The as-synthesized nanocomposites were characterized by energy-dispersive spectroscopy (EDS), Raman spectroscopy, scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), cyclic voltammetry (CV), and electrochemical impedance spectroscopy (EIS). (BiO)2CO3 composite plays a key role in the improvement of the detection sensitivity, which can form multicomponent alloy with cadmium and lead. Additionally, the unique structure of rGO can enlarge the surface area and provide abundant active sites. Moreover, Nafion incorporation in the nanocomposite can effectively increase the adhesion and mechanical strength of the film, and further improve the preconcetration ability due to the cation-exchange capacity of its abundant sulfonate groups. As expected, the (BiO)2CO3-rGO/Nafion nanocomposite-modified glassy carbon electrode ((BiO)2CO3-rGO-Nafion/GCE) achieved low detection limits of 0.24 μg/L for Pb(II) and 0.16 μg/L for Cd(II), in the linear range of 1.0–60 μg/L, and showed some excellent performance, such as high stability, good selectivity, and sensitivity. Finally, synthetic water samples were prepared and further used to verify the practicability of the (BiO)2CO3-rGO-Nafion/GCE with satisfactory results.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2021

Linker-Free Magnetite-Decorated Gold Nanoparticles (Fe3O4-Au): Synthesis, Characterization, and Application for Electrochemical Detection of Arsenic (III)

Linker-free magnetite nanoparticles (Fe3O4NPs)-decorated gold nanoparticles (AuNPs) were grown using a new protocol that can be used as a new platform for synthesis of other intact metal–metal oxide nanocomposites without the need for linkers. This minimizes the distance between the metal and metal oxide nanoparticles and ensures the optimum combined effects between the two material interfaces. X-ray diffraction (XRD) and Fourier transform infrared (FTIR) spectroscopy confirmed the successful synthesis of the Fe3O4-Au nanocomposite, without any change in the magnetite phase. Characterization, using transmission electron microscopy (TEM), scanning electron microscopy (SEM) and energy dispersive X-ray (EDX) spectroscopy, revealed the composite to consist of AuNPs of 70 ± 10 nm diameter decorated with tiny 10 ± 3 nm diameter Fe3O4NPs in Au:Fe mass ratio of 5:1. The prepared Fe3O4-Au nanocomposite was embedded in ionic liquid (IL) and applied for the modification of glassy carbon electrode (GCE) for the electrochemical detection of As(III) in water. By combining the excellent catalytic properties of the AuNPs with the high adsorption capacity of the tiny Fe3O4NPs towards As(III), as well as the good conductivity of IL, the Fe3O4-Au-IL nanocomposite showed excellent performance in the square wave anodic stripping voltammetry detection of As(III). Under the optimized conditions, a linear range of 1 to 100 μg/L was achieved with a detection limit of 0.22 μg/L (S/N = 3), and no interference from 100-fold higher concentrations of a wide variety of cations and anions found in water. A very low residual standard deviation of 1.16% confirmed the high precision/reproducibility of As(III) analysis and the reliability of the Fe3O4-Au-IL sensing interface. Finally, this proposed sensing interface was successfully applied to analyzing synthetic river and wastewater samples with a 95–101% recovery, demonstrating excellent accuracy, even in complex synthetic river and wastewater samples containing high concentrations of humic acid without any sample pretreatments.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

A Sustainable and Environmentally Friendly Concrete for Structural Applications

The purpose of this study is to utilize waste products—precipitated calcium carbonate (PCC) and upcycled recycled concrete aggregate (upcycled RCA or UCA)—in civil works projects. To do so, tests must be performed to determine the engineering properties of the materials in which PCC and UCA are sequestered. PCC is a fine to coarse grain waste product generated during the production of sugar from sugar beets. UCA is produced from demolished and returned concrete by the extraction of primarily calcium and alkalinity. The study also includes the use of both PCC and UCA in the same concrete mix design. The test results on PCC alone show that the optimum content to achieve a minimum 28 MPa (4000 psi) compressive strength is 25% and 30%. The corresponding compressive strength of mixes in which conventional aggregate was replaced by UCA is about 48 MPa (7000 psi) to 55 MPa (8000 psi) at the same water: cement ratio (0.44) by weight. The compressive strength of concrete with 25% to 30% cement replaced by PCC and varying aggregates replaced with UCA ranges from 19.3 to 40 MPa (2800 to 5800 psi). Other tests on PCC and UCA include tensile strength of 2 to 3 MPa (293 to 423 psi) and flexural strength of 1.3 to 1.9 MPa (183 to 279 psi). Analytical techniques such as X-ray diffraction (XRD), energy-dispersive X-ray spectrometry (EDX), and scanning electron microscopy (SEM) were used to identify the constituent elements and chemical compounds present in PCC, including calcium carbonate and silica. Based on the test results, the composition of PCC by weight indicates 45.9% calcium, 39.4% oxygen, and 9.2% carbon. Based on the results of this study, we can expect to reduce carbon emissions in the production of cement and aggregates, as well as utilize waste products in the civil engineering field.

42 ENGINEERING↗
DOE OSTI2023

CO 2 /Brine/Rock Interactions in the Cedar Keys-Lawson Formation

It has been reported that among the various geologic storage options, deep saline aquifers have the largest estimated capacity for CO 2 storage. Obtaining knowledge of possible artificially geochemically induced changes to the permeability and porosity of host CO 2 storage deposits will enable us to gain insight on long-term reservoir behavior under CO 2 storage conditions. An experimental study of the interaction of CO 2 /brine/rock on saline formations was conducted in a static system under CO 2 storage conditions. Chemical interactions in the Cedar Keys-Lawson Formation carbonate during exposure to CO 2 and brine under sequestration conditions were studied. Samples were exposed to the simulated in-situ reaction conditions for one and six months. The samples were exposed to a model brine at 55 °C and CO 2 pressure of 23.8 MPa (3,500 psig). Computed tomography (CT), x-ray diffraction (XRD), scanning electron microscopy (SEM)-energy dispersive x-ray spectroscopy (EDS), brine composition, core porosity, and core permeability analyses were conducted prior to and after the exposure experiments. Preliminary permeability measurements obtained from the core samples showed changes after they were exposed to CO 2 -saturated brine for one and six months. This observation suggests that mineral dissolution and mineral precipitation could occur in the host deposit altering its characteristics for CO 2 storage over time. The 3D images of the pore space clearly illustrate the degree of dissolution that occurred during exposure. It is noted that the dissolution that occurred during the six-month exposure could have enhanced the connectivity between voids. This may contribute the increase of permeability after the CO 2 /brine exposure. In addition, the primary minerals comprising the core are dolomite and gypsum. Both minerals could dissolve in the CO 2 /brine environment resulting in the increase of permeability after the six-month exposure.

58 GEOSCIENCES↗
DOE OSTI2023

Electrical and Magnetic Properties of FeGa 3 with Antisite Disorder

We investigated the electronic and magnetic ground states of the cage compound FeGa 3 under the presence of Fe antisite disorder (namely as Fe 0.258 Ga 0.742 ) by x-ray diffraction (XRD), Mössbauer spectroscopy (MS), magnetization and electrical resistivity. Our results show that approximately 4.5 (5)% Fe antisite occupying one of the two non-equivalent Ga sites changes significantly the electronic and magnetic ground states of the pristine compound. We uncover that Fe 0.258 Ga 0.742 undergoes two magnetic transitions, T 1 ≈ 60 K and T 2 ≈ 15 K, the latter associated with the suppression of semiconducting behavior. We focus our discussion on the role that in-gap impurity states and spin disorder play across semiconducting-metal and paramagnetic-magnetic transitions.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Code to map Xray reflectivity data from real space to reciprocal space

Code to map X-ray reflectivity data from real space to reciprocal space. The code is written as a Jupyter notebook. Example data are included as a separate file (example_data.csv). These data were collected on a Panalytical XRD system. As a first step, run all cells in the notebook. Opportunities are identified for users to make their own choices for choosing the boundaries of the region of interest to estimate background. A simple algorithm is used to estimate background from the outer regions of the data collection region, interpolating the result inside the region of interest. The background is removed and then the data mapped to Qx-Qz (reciprocal space) coordinates. The results are written as NumPy binary and Matlab formatted files.

Fitzsimmons, Michael [Oak Ridge National Lab. (ORN↗
DOE OSTI2025

Data for: Climatic Imprint on Interfacially-Controlled Platinum-Palladium Resources

Data package for manuscript "Climatic Imprint on Interfacially-Controlled Platinum-Palladium Resources" by Emily G. Wright, Ivey Wang, Yihang Fang, Elaine D. Flynn, and Jeffrey G. Catalano. This dataset contains adsorption results from experiments designed to investigate the effect of chloride on Pd(II) adsorption to goethite and Pt(II) adsorption to hematite and goethite, including lab experiments, X-ray absorption fine structure spectroscopy, and models of retention within a laterite. See the associated manuscript for full methods information. The file "Wright2025_PtAds_data.csv" contains the target starting Pt concentration (uM), final aqueous Pt and associated error (in uM), calculated adsorbed Pt and associated error (in umol/m2), target and measured aqueous chloride (mM), target aqueous nitrate (mM), final pH, and mineral concentration/loading (g/L). Associated mineral-free controls (mineral loading = 0 g/L) are included; the aqueous Pd error was not calculated and chloride was not measured in every sample. These data appear in Figures 1, S3, S4, S5, S20, and S22 in the associated manuscript. The file "Wright2025_PdAds_data.csv" contains the target starting Pd concentration (uM), final aqueous Pd and associated error (in uM), calculated adsorbed Pd and associated error (in umol/m2), target and measured aqueous chloride (mM), and mineral concentration/loading (g/L). Associated mineral-free controls (mineral loading = 0 g/L) are included; the aqueous Pd error was not calculated and chloride was not measured in every sample. These data appear in Figures 1, S3, S4, S5, and S20 in the associated manuscript. The file "Wright2025_MineralBatches_data.csv" contains the mineral identity and BET specific surface area (m2/g) for every mineral batch synthesized and used in experiments. The annealing time used is listed for hydrothermally annealed goethite. These data appear in Table S2 in the associated manuscript. The file "Wright2025_XRD_data.csv" contains the XRD patterns for every mineral batch synthesized as the counts as a function of two theta (in degrees). See "Wright2025_MineralBatches_data.csv" for more details on specific mineral batches. These data appear in Figure S2 in the associated manuscript. The file "Wright 2025_ZetaPotential_data.csv" contains the measured zeta potentials for samples of goethite (batch G2) at pH 4 the presence of varying amounts of sodium chloride. These data appear in Table S3 in the associated manuscript. The file "Wright2025_XAFSSamples_data.csv" contains the specific mineral batch, measured final aqueous Pd or Pt (uM), measured final aqueous chloride (mM), and estimated adsorbed Pd or Pt (umol/m2) of all XAFS samples. These data appear in Tables S4, S7, S8, and S10 in the associated manuscript. The files "Wright2025_PdXAFS_data.csv" and "Wright2025_PtXAFS_data.csv" contain the normalized spectra of Pd and Pt, respectively, adsorbed to minerals at varying chloride concentrations. See "Wright2025_XAFSSamples_data.csv" for a guide to sample names. Note that "05" in a sample name is equivalent to "0.5". These data appear in Figures 2, S6, S7, S8, S12, S13, and S14 in the associated manuscript. The file "Wright2025_LateriteProfileProfileModelParameters_data.csv" include the ratio of hematite to hematite and goethite in two synthetic, modeled profiles, as well as the modeled surface areas of goethite and hematite as a function of relative depth within the modeled weathering zone. These data were used, in conjunction with equations presented in the paper, to calculate the theoretical concentrations of Pd and Pt (and the resulting Pt/Pd ratio) within the profiles. These data appear in Figure 3 in the associated manuscript. The file "Wright2025_Imagery_data.zip" is a zipped folder containing the TEM and STEM images appear in Figures S18 and S19. Individual files are labeled as either STEM (Fig. S18) or TEM (Fig. S19) with a letter representing the part of the multipart figure.

58 GEOSCIENCES↗
DOE OSTI2021

Pressure-Induced Insulator–Metal Transition in Two-Dimensional Mott Insulator NiPS 3

The pressure-induced insulator to metal transition (IMT) of layered magnetic nickel phosphorous tri-sulfide NiPS 3 was studied in-situ under quasi-uniaxial conditions by means of electrical resistance (R) and X-ray diffraction (XRD) measurements. This sluggish transition is shown to occur at 35 GPa. Transport measurements show no evidence of superconductivity to the lowest measured temperature (~2 K). The structure results presented here differ from earlier in-situ work that subjected the sample to a different pressure state, suggesting that in NiPS 3 the phase stability fields are highly dependent on strain. Furthermore, it is suggested that careful control of the strain is essential when studying the electronic and magnetic properties of layered van der Waals solids.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Characterizing x-ray transmission through filters used in high energy density physics diagnostics

We report on the design and implementation of a new system used to characterize the energy-dependent x-ray transmission curve, Θ(E), through filters used in high-energy density physics diagnostics. Using an Amptek X-123-CdTe x-ray spectrometer together with a partially depleted silicon surface barrier detector, both the energy spectrum and total emission of an x-ray source have been accurately measured. By coupling these detectors with a custom PROTO-XRD x-ray source with interchangeable cathodes, accurate characterizations of Θ(E) for filters of varying materials and thicknesses have been obtained. The validity of the technique has been confirmed by accurately reproducing areal densities for high-purity filters with known x-ray transmission properties. In this paper, the experimental setup is described and the results of absorption calibrations performed on a variety of different filters are presented.

Pearcy, J.↗
NASA NTRS1981

Autothermal reforming of sulfur-free and sulfur-containing hydrocarbon liquids

The mechanisms by which various fuel component hydrocarbons related to both heavy petroleum and coal-derived liquids are converted to hydrogen without forming carbon were investigated. Reactive differences between paraffins and aromatics in autothermal reforming (ATR) were shown to be responsible for the observed fuel-specific carbon formation characteristics. The types of carbon formed in the reformer were identified by SEM and XRD analyses of catalyst samples and carbon deposits. From tests with both light and heavy paraffins and aromatics, it is concluded that high boiling point hydrocarbons and polynuclear aromatics enhance the propensity for carbon formation. The effects of propylene addition on the ATR performance of benzene are described. In ATR tests with mixtures of paraffins and aromatics, synergistic effects on conversion characteristics were identified. Indications that the sulfur content of the fuel may be the limiting factor for efficient ATR operation were found. The conversion and degradation effects of the sulfur additive (thiophene) were examined.

Source record↗
NASA NTRS1982

A study of fiber materials for use in temperature resistant fiber reinforced composites

This study has been directed at characterizing the micro-properties of candidate ceramics and glasses for use in making fibers used in fiber reinforced material composites. Particular emphasis has been given into developing techniques to guide the optimization of fiber properties. The Scanning Electron Microscope (SEM) and X-ray Diffractometer (XRD) have been used to help collate the method of synthesis, crystal structure and surface morphology with physical performance parameters. As a result, progress has been made in characterizing such materials. This increased understanding makes the previous research worthy of further study.

Bachowsky, M. J.↗
NASA NTRS1986

Adequacy of surface analytical tools for studying the tribology of ceramics

Surface analytical tools are very beneficial in tribological studies of ceramics. Traditional methods of optical microscopy, XRD, XRF, and SEM should be combined with newer surface sensitive techniques especially AES and XPS. ISS and SIMS can also be useful in providing additional compositon details. Tunneling microscopy and electron energy loss spectroscopy are less known techniques that may also prove useful.

Sliney, H. E.↗
NASA NTRS1986

Characterization of the tribological coating composition 77 wt % CaF2 - 23 wt % Li F fused to IN-750 alloy

A coating composed of 77 wt % CaF2 - 23 wt % LiF fused on IN-750 nickel-based alloy was studied using SEM, XRD, EDX, and optical microscopic methods. The surfaces examined were the as-fused coating with no subsequent treatment, the coating after ultrasonic cleaning in water, and the uncoated polished and etched metal. It was found that the coating reacts during fusion with Ti and Nb rich inclusions in the alloy. Numerous small rectangular crystallites of Ca(Ti,Nb) oxide are formed beneath an overlay of fused fluoride composition. These crystallines are stubby and appear to be embedded in the metal substrate surface. It is known from previous studies that this coating-alloy system has good tribological properties in extreme conditions, such as liquid fluorine. It has been concluded from the present study that the short firmly embedded crystalline protuberances contribute to the coating adherence and thereby to enhanced coating wear life.

Deadmore, D. L.↗
NASA NTRS1987

Morphology of zirconia particles exposed to D.C. arc plasma jet

Zirconia particles were sprayed into water with an arc plasma gun in order to determine the effect of various gun operating parameters on their morphology. The collected particles were examined by XRD and SEM techniques. A correlation was established between the content of spherical (molten) particles and the operating parameters by visual inspection and regression analysis. It was determined that the composition of the arc gas and the power input were the predominant parameters that affected the melting of zirconia particles.

Zaplatynsky, Isidor↗
NASA NTRS1987

Nature and origin of mineral coatings on volcanic rocks of the Black Mountain, Stonewall Mountain and Kane Springs wash volcanic centers, southern Nevada

Mineral coatings, including desert varnish on volcanic rocks of the semi-arid Basin and Range province are composted of amorphous, translucent films of Fe, Mn, Si, and Al rich compounds. Coatings are chiefly thin films that impregnate intergranularly to depths of about 0.1 to 0.3 mm, rarely deeper. Sixteen coating sections and subsurface interiors were probed by SEM; 20 samples were scanned by infrated spectrometry; 10 samples were scanned for visible-near IR spectra; inductin coupling plasma analyses were collected on 34 samples; 2 desert varnish surgaces were investigated by optical density slice imagery; a few XRD analyses were conducted in addition to the 50 reported in the last period; thin section observation continued; and imagery processing focused on classification techniques. In late May, approximately 10 field days were spent at the Stonewall and Black Mountain study sited conducting more detailed mapping and observation base on imagery results and collecting spectra with the Collins Field Spectrometer. Approximately 100 spectral analyses were collected and are currently being processed.

Taranik, James V.↗
NASA NTRS1986

High-temperature oxidation of a rapidly solidified amorphous Ta-Ir alloy

The oxidation products formed at 500 and 700 C on an amorphous Ta-44.5 at. pct Ir alloy in an Ar-0.1 percent O2 gas mixture were characterized using SEM, XRD, EPMA, TEM, STEM, AES, and XPS. Initially, a thin (3-4 nm) layer of Ta2O5 formed at the surface of the alloy. Continued growth of the Ta2O5, which occurred very rapidly, involved diffusion of oxygen anions from the Ta2O5/gas interface to the alloy/Ta2O5 interface, where tantalum was selectively oxidized. Because the oxide grew more quickly than iridium could diffuse back into the alloy, the iridium coalesced into platelets of crystalline iridium-rich alloy that were oriented approximately parallel to the oxide/alloy interface, and which became embedded in a matrix of Ta2O5. The unoxidized core remained in the glassy state. The oxidation process and/or the dissolution of oxygen into the unoxidized alloy caused the alloy to become embrittled.

Cotell, Catherine M.↗
NASA NTRS1987

Phase purity of NiCo2O4, a catalyst candidate for electrolysis of water

NiCo2O4 is shown to be difficult to obtain as a pure phase, and may never have been so obtained. High resolution x-ray diffractometry is required for its precise characterization. Film XRD is not likely to show the asymmetry in the spinel diffraction lines, caused by poorly crystallized NiO, as seen in diffractometer traces. The Co3O4 which is expected to accompany NiO as an impurity in NiCo2O4 syntheses has the same diffraction pattern as the binary oxide. Firings of the co-precipitated hydroxides at 300, 350, and 400 C, including one in pure O2, failed to produce single phase cobaltate. Scanning electron microscopy showed all the sintered products to range over several orders of magnitude in agglomerate/particle size. Surface areas by BET were all in the range 40 to 110 m sq/g, equivalent to particles of 200 to 100 Angstrom diameter. The spinel diffraction line breadths were compatible with those approximate dimensions.

Singer, J.↗