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All sources NASA NTRS DOE OSTI

DOE OSTI2018

The Performance of CH3NH3PbI3 - Nanoparticles based – Perovskite Solar Cells Fabricated by Facile Powder press Technique

Highlights: • Perovskite nanoparticles (PNs) were prepared using simple solid-state technique. • Perovskite layer has been deposited by facile powder press technique - a solution cum vacuum-free. • Fabricated device structure: FTO/c-TiO{sub 2}/mp-TiO{sub 2}/Perovskite/CuI/Cr/Pt-coated FTO. • 1:3 M ratio of PbI{sub 2} in MAI resulted in achieving a PCE of 3.90%. • From the stability test, it is inferred that deterioration in ‘η’ and ‘V{sub OC}’ was by 27.87% and 29.23% respectively. - Abstract: Here, we have introduced a facile solid-state route assisted method to prepare CH{sub 3}NH{sub 3}PbI{sub 3} perovskite nanoparticles (PNs) and together with a facile - powder press technique, for the deposition of prepared PNs - a solution cum vacuum-free route. The perovskite layer was prepared using different lead iodide (PbI{sub 2}) precursor molar concentrations (0.5, 1, 1.5, 2 mmol) and the PbI{sub 2} concentration was found to have a significant impact on the structural, optical, morphological and electrical properties. The sample prepared using molar ratio PbI{sub 2}: MAI at 1:3 shows the optimal bandgap value (∼1.51 eV), broader band edge peak at 755 nm and found have good optical property for photovoltaic (PV) applications. The J–V performance of the fabricated perovskite device with FTO/c-TiO{sub 2}/mp-TiO{sub 2}/Perovskite/CuI/ Cr/Pt-coated FTO counter electrode has been studied. The device fabricated using the concentration at PbI{sub 2}:MAI 1:3 achieved a PCE of 3.9% and resulted in better long-term stability with deterioration in η and V{sub OC} by 27.87% and 29.23% after 15 days.

14 SOLAR ENERGY↗

NASA NTRS2009

A Data Matrix Method for Improving the Quantification of Element Percentages of SEM/EDX Analysis

A simple 2D M N matrix involving sample preparation enables the microanalyst to peer below the noise floor of element percentages reported by the SEM/EDX (scanning electron microscopy/ energy dispersive x-ray) analysis, thus yielding more meaningful data. Using the example of a 2 3 sample set, there are M = 2 concentration levels of the original mix under test: 10 percent ilmenite (90 percent silica) and 20 percent ilmenite (80 percent silica). For each of these M samples, N = 3 separate SEM/EDX samples were drawn. In this test, ilmenite is the element of interest. By plotting the linear trend of the M sample s known concentration versus the average of the N samples, a much higher resolution of elemental analysis can be performed. The resulting trend also shows how the noise is affecting the data, and at what point (of smaller concentrations) is it impractical to try to extract any further useful data.

Lane, John↗

DOE OSTI2022

Interlaboratory Reproducibility of Contour Method Data in a High Strength Aluminum Alloy

The contour method for residual stress measurement has seen significant development, but an experimental reproducibility study utilizing physical samples has not been published. A double-blind reproducibly study is reported, having scope beginning with EDM cutting and ending with residual stress calculation. A reinforced I-beam sample geometry is identified for its unique residual stress profile when extracted from residual stress bearing quenched aluminum bar (7050-T74). Contour measurements are prescribed on a midplane of symmetry with dimensions 24.0 mm by 50.0 mm. Fourteen identically prepared samples are fabricated from a single long bar with well characterized and uniform residual stress. Five samples throughout the bar are identified for planning measurements to validate sample uniformity and overall suitability of the residual stress field. The planning measurements employ a range of techniques: contour method, neutron diffraction, and hole-drilling. Eight samples are distributed to an international group of participants to execute their standard measurement practice. A double-blind process is followed to provide anonymity. Results are provided by eight participants: six being self-similar and two being quite different, the latter set aside as outliers. An average residual stress field is established from non-outlying results and the spatial distribution of reproducibility standard deviation is determined. The average stress field ranges from -60 to 70 MPa and the reproducibility standard deviation averages 8.1 MPa on the measurement plane. The average reproducibility standard deviation is about 3 × larger for points within 1.0 mm of plane boundaries (17.6 MPa) than for the remaining points (6.1 MPa). Reproducibility standard deviation (among different labs) for contour method residual stress measurement is found to be very similar to repeatability standard deviation (in a single lab) reported in prior work. The reproducibility observed here, for the entire measurement process, is also similar to that found in a prior reproducibility study limited to contour method data analysis.

36 MATERIALS SCIENCE↗

DOE OSTI2014

Near surface silicide formation after off-normal Fe-implantation of Si(001) surfaces

We report on formation of non-crystalline Fe-silicides of various stoichiometries below the amorphized surface of crystalline Si(001) after irradiation with 5 keV Fe{sup +} ions under off-normal incidence. We examined samples prepared with ion fluences of 0.1 × 10{sup 17} and 5 × 10{sup 17} ions cm{sup −2} exhibiting a flat and patterned surface morphology, respectively. Whereas the iron silicides are found across the whole surface of the flat sample, they are concentrated at the top of ridges at the rippled surface. A depth resolved analysis of the chemical states of Si and Fe atoms in the near surface region was performed by combining X-ray photoelectron spectroscopy and X-ray absorption spectroscopy (XAS) using synchrotron radiation. The chemical shift and the line shape of the Si 2p core levels and valence bands were measured and associated with the formation of silicide bonds of different stoichiometric composition changing from an Fe-rich silicides (Fe{sub 3}Si) close to the surface into a Si-rich silicide (FeSi{sub 2}) towards the inner interface to the Si(001) substrate. This finding is supported by XAS analysis at the Fe K-edge which shows changes of the chemical environment and the near order atomic coordination of the Fe atoms in the region close to surface. Because a similar Fe depth profile has been found for samples co-sputtered with Fe during Kr{sup +} ion irradiation, our results suggest the importance of chemically bonded Fe in the surface region for the process of ripple formation.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2016

Field application of pathogen detection technologies

Over the last 10 years there has been a significant increase in commercial products designed for field-based detection of microbial pathogens. This is due, in part, to the anthrax attacks in the United States in 2001, and the need for first responders to quickly identify the composition of suspected white powders and other potential biothreats. Demand for rapid detection is also driven by the need to ensure safe food, water, and environmental systems. From a technology perspective, rapid identification methods have largely capitalized on PCR and other molecular recognition techniques that can be deployed as robust field instrumentation. Examples of the relevant needs include the ability to: 1) declare a water distribution system free of microbial pathogens after a pipe/main break repair; 2) assess risks of contamination such as when produce production and processing plants are located near concentrated animal feeing operations; 3) evaluate the safety of ready-to-eat products; 4) determine the extent of potential serious disease outbreaks in remote and/or disaster stricken areas where access to clinical laboratories is not an immediate option; and 5) quickly assess credible biological terrorism events. Many of the principles underlying rapid detection methods are derived from methods for environmental microbiology, but there is a dearth of literature describing and evaluating field-based detection systems. Thus, the aims of this chapter are to: 1) summarize the different kinds of commercially available sampling kits and field-based biological detectors; 2) highlight some of the continued challenges of sample preparation to stimulate new research towards minimizing the impact of inhibitors on PCR-based detection systems; 3) describe our general rationale and statistically-based approach for instrument evaluation; 4) provide statistical and spatial guidelines for developing valid sampling plans; and 5) summarize some current needs and emerging technologies. This information is presented both to highlight the state of the field, and to also highlight major questions that students may wish to consider investigating further. Where possible we will cite studies that have been conducted and published either in traditional peer-reviewed or other literature (e.g., AOAC International Methods).

Straub, Tim M.↗

DOE OSTI2022

Fluid Induced Elemental and Mineralogy Alterations of Caney Shale

ABSTRACT: Studies were conducted on cores and rock cuttings recovered from two wells drilled in Caney shale in the Southern Oklahoma. Mineralogical compositions of these samples were obtained by X-Ray Diffraction (XRD) measurements using two methods of sample preparation: conventional powder (by crushing and grinding of rock fragments) and spray-drying of micronized rock powder method. Microstructure and microanalysis were acquired by Scanning Electron Microscopy/Energy Dispersive Spectroscopy (SEM/EDS). Batch experiments were then conducted using selected rock samples and fracturing fluid whilst deionized water was used as control sample for fluid/rock interaction. These were conducted at 95°C and ambient pressure for various time periods to assess the geochemical reactivity of the Caney shale. The rock samples were subsequently recovered from fluid, dried and analysis repeated using identical XRD and SEM/EDS measurements, following the same conditions. Preliminary experimental results show rock mineralogical compositions are predominantly quartz with relatively high clay content. The clay minerals are mainly illite. Carbonate content is less than 10% by weight for most samples, with other non-clay minerals pyrite, albite, dolomite, and some apatite. In general, sprayed samples showed more intense peaks and less full width at half maxima (FWHM) relative to conventional rock-powder samples. Post-experimental mineralogical changes were observed in samples with clay portions breaking down to amorphous entities. As expected, dissolution of carbonates (calcite and dolomite) was observed and newly detected dissolution of biogenic micro quartz resulted in formation of amorphous silica. 1.0 INTRODUCTION Formation of sedimentary rocks involves processes where rock sediments are emplaced with fluids starting interactions that persist over long periods. During the lithification process, sediments and fluids react and attain equilibrium state. This equilibrium is disturbed during drilling, completion, hydraulic fracturing and other operations that involve the introduction of engineered fluids into the subsurface. To return to equilibrium, dissolution and precipitation of minerals may occur. These reactions have implications on the petrophysical properties of the reservoir. Whiles dissolution and precipitation of minerals can enhance porosity and permeability, the reverse can also be true. For example, when acidic fluids are introduced into formations with high carbonate contents, carbonate minerals dissolve into solution thus increasing the porosity and permeability of the formation. In contrast, when alkaline fluids with pH above 11 are introduced into an illite-rich shale formation, the rock-fluid interaction leads to de-flocculation of illite platelets causing substantial increase in clay fines migration, consequently significant reduction in permeability (Salles et al., 2008).

Awejori, G.↗

DOE OSTI2012

Preparation of {l_brace}0 1 0{r_brace}-faceted anatase TiO{sub 2} nanocuboids from peroxotitanium complex solution

{l_brace}0 1 0{r_brace}-faceted anatase TiO{sub 2} nanocuboids have been fabricated by hydrothermal route using peroxotitanium complex solution as precursor. The effects of reaction time, the amount of urea and temperature on the formation of {l_brace}0 1 0{r_brace}-faceted anatase TiO{sub 2} were characterized by XRD, FESEM and TEM. The growth mechanism of nanocuboids was proposed that the nanocuboids were formed by the transition from H{sub 2}Ti{sub 2}O{sub 5}{center_dot}H{sub 2}O phase to anatase TiO{sub 2} in the basic condition. The photocatalytic performance of the prepared samples was tested in the degradation of Rhodamine B and the anatase nanocuboids exhibited enhanced photocatalytic activity compared with the standard P25 powders. - Graphical abstract: Anatase TiO{sub 2} nanocuboids with exposed {l_brace}0 1 0{r_brace} facets prepared by a hydrothermal method exhibit superior photocatalytic activity for degradation Rhodamine B to P25. Highlights: Black-Right-Pointing-Pointer One-step route to prepare {l_brace}0 1 0{r_brace}-faceted anatase TiO{sub 2} nanocrystal is developed. Black-Right-Pointing-Pointer Control synthesis of {l_brace}0 1 0{r_brace}-faceted anatase nanocuboids. Black-Right-Pointing-Pointer Mechanism on formation of anatase nanocuboids under hydrothermal condition. Black-Right-Pointing-Pointer The enhanced photocatalytic reactivity of nanocuboids is attributed to reactive facets.

36 MATERIALS SCIENCE↗

DOE OSTI2013

Intrinsic magnetic, structural and resistivity properties of ferromagnetic Mn{sub 0.5}Zn{sub 0.5}Al{sub x}Fe{sub 2−x}O{sub 4} nanoparticles

Highlights: ► Al{sup 3+} ion substituted Mn–Zn ferrite nanoparticles. ► Single phase cubic spinel structure changes with Al{sup 3+} substitution. ► Magnetization and coercivity decreased with increasing Al{sup 3+}. ► Resistivity increased with Al{sup 3+} substitution. - Abstract: In this work the nano-structural, magnetic and resistivity properties of Al{sup 3+} substituted Mn–Zn ferrites powders were investigated. Mn{sub 0.5}Zn{sub 0.5}Al{sub x}Fe{sub 2−x}O{sub 4} powders, where x = 0.0, 0.1, 0.2, 0.3, 0.4 and 0.5 were obtained by the sol–gel auto-combustion method. X-ray diffraction data indicate that, after substitution, all the samples consisted of the main spinel phase in combination with a small amount of a foreign Al{sub 2}O{sub 3} phase. The addition of Al{sup 3+} resulted in a reduction of particle size and density of the prepared samples. Cation distribution in the present study was estimated by using X-ray diffraction data. The tetrahedral site radii initially increased with Al{sup 3+} content while the octahedral site radii decreased with the Al{sup 3+} substitution. FTIR spectra show two strong absorption bands at 529–548 cm{sup −1} and 445–452 cm{sup −1} which are the typical bands for the cubic spinel crystal structure. The magnetic properties were measured by employing a vibrating sample magnetometer. It was observed that the saturation magnetization, coercivity and anisotropy field decreased with the increase of Al{sup 3+} substitution. Introduction of Al{sup 3+} ions into the Mn–Zn ferrite increased the values of the resistivity, especially in the lower temperature range.

36 MATERIALS SCIENCE↗

DOE OSTI2014

Synthesis of polyaniline/SnO{sub 2} nanocomposite and its improved electrochemical performance

Highlights: • Supercapacitors based on PANI/SnO{sub 2} nanocomposite were reported. • Supercapacitors using this material gave a specific capacitance of 501 F g{sup −1}. • Capacitance retention was 85.8% over 2000 charge–discharge cycles. - Abstract: SnO{sub 2} was prepared by the hydrothermal route. Aniline monomer was polymerized in the suspension of SnO{sub 2} to form inorganic–organic nanocomposite materials, in which SnO{sub 2} particles were embedded within polyaniline (PANI). Morphological and structural characterizations of the prepared samples were carried out using scanning electron microscope; transmission electron microscope; power X-ray diffraction and Fourier transform infrared spectroscopy. Their electrochemical properties were also investigated using cyclic voltammetry, galvanostatic charge–discharge and electrochemical impedance spectroscopy. The as-prepared nanocomposites had excellent properties in the capacitance, and its specific capacitance was up to 501 F g{sup −1} with a specific energy density of 66.8 W h kg{sup −1} at a power density of 960.6 W kg{sup −1}. The device fulfilled the requirement of long durability necessary for an energy storage system, since after 2000 galvanostatic charge–discharge cycles, retention of 85.8% in capacitance was observed. These results indicated that the PANI/SnO{sub 2} had a synergistic effect of the complementary properties of both components.

36 MATERIALS SCIENCE↗

DOE OSTI2014

Magnetic properties of Zn doped Co{sub 2}Y hexaferrite by using high-field Mössbauer spectroscopy

The polycrystalline samples of Ba{sub 2}Co{sub 2−x}Zn{sub x}Fe{sub 12}O{sub 22} (x = 0.5, 1.0, 1.5) were synthesized by using solid-state-reaction method. From the XRD patterns, analyzed by Rietveld refinement, the prepared samples are found to be single-phased with rhombohedral structure (R-3m). The magnetic properties of samples were investigated with vibrating sample magnetometer, and high-field Mössbauer spectrometer. From the zero-field-cooled curves under 100 Oe between 4.2 and 740 K, we observe that the samples show spin transition from helicalmagnetic to ferrimagnetic order. With increasing Zn ion concentration, the spin transition temperature (T{sub s}) and Curie temperature (T{sub C}) decrease linearly. We have obtained Zero-field Mössbauer spectra of all samples at various temperatures ranging from 4.2 to 650 K, and analyzed the spectra below T{sub C} as six-sextets for Fe sites. From the temperature dependence of hyperfine field (H{sub hf}), we have noticed an abrupt change in H{sub hf} at T{sub s}. In addition, Mössbauer spectra of all samples at 4.2 K were taken with applied field ranging from 0 to 50 kOe, indicating the canting angle between applied field and H{sub hf} decreased with increasing Zn concentration.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2025

Determining the complex second-order optical susceptibility in macroscale van der Waals heterobilayers

In this work, we report on the experimental characterization of the second-order susceptibility in MoSe 2 /WS 2 heterobilayers, including their hidden complex phases. To this end, we developed a heterodyne-detection scheme for second-harmonic generation and applied it to macroscale heterobilayer samples prepared using the gold-tape exfoliation method. The heterodyne scheme enabled us to distinguish the relative orientation of the crystal domains, and furthermore, it allowed us to characterize the complex phases of the susceptibility relative to a reference quartz sample. By comparing the results from the monolayer regions and the heterobilayer region over several hundred microns of the sample area, we determined that the contribution of interlayer effects to second-harmonic generation is within the experimental uncertainty arising from the sample inhomogeneity. The results here provide fundamental quantitative information necessary for the precise design of nanophotonic systems based on stacking engineering.

2D materials↗

DOE OSTI2023

Jahn–Teller-driven phase segregation in Mn x Co 3–x O 4 spinel thin films

Transition metal spinel oxides comprised of earth-abundant Mn and Co have long been explored for their use in catalytic reactions and energy storage. However, understanding functional properties can be challenging due to differences in sample preparation and the ultimate structural properties of the materials. Epitaxial thin film synthesis provides a novel means of producing precisely controlled materials to explore the variations reported in the literature. In this work, Mn x Co 3–x O 4 samples from x = 0 to x = 1.28 were synthesized through molecular beam epitaxy and characterized to develop a material properties map as a function of stoichiometry. Here, films were characterized via in situ x-ray photoelectron spectroscopy, x-ray diffraction, scanning transmission electron microscopy, and polarized K-edge x-ray absorption spectroscopy. Mn cations within this range were found to be octahedrally coordinated, in line with an inverse spinel structure. Samples largely show mixed Mn 3+ and Mn 4+ character with evidence of phase segregation tendencies with the increasing Mn content and increasing Mn 3+ formal charge. Phase segregation may occur due to structural incompatibility between cubic and tetragonal crystal structures associated with Mn 4+ and Jahn–Teller active Mn 3+ octahedra, respectively. Our results help in explaining the reported differences across samples in these promising materials for renewable energy technologies.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

DOE OSTI2017

New approaches for metabolomics by mass spectrometry

Small molecules constitute a large part of the world around us, including fossil and some renewable energy sources. Solar energy harvested by plants and bacteria is converted into energy rich small molecules on a massive scale. Some of the worst contaminants of the environment and compounds of interest for national security also fall in the category of small molecules. The development of large scale metabolomic analysis methods lags behind the state of the art established for genomics and proteomics. This is commonly attributed to the diversity of molecular classes included in a metabolome. Unlike nucleic acids and proteins, metabolites do not have standard building blocks, and, as a result, their molecular properties exhibit a wide spectrum. This impedes the development of dedicated separation and spectroscopic methods. Mass spectrometry (MS) is a strong contender in the quest for a quantitative analytical tool with extensive metabolite coverage. Although various MS-based techniques are emerging for metabolomics, many of these approaches include extensive sample preparation that make large scale studies resource intensive and slow. New ionization methods are redefining the range of analytical problems that can be solved using MS. This project developed new approaches for the direct analysis of small molecules in unprocessed samples, as well as pushed the limits of ultratrace analysis in volume limited complex samples. The projects resulted in techniques that enabled metabolomics investigations with enhanced molecular coverage, as well as the study of cellular response to stimuli on a single cell level. Effectively individual cells became reaction vessels, where we followed the response of a complex biological system to external perturbation. We established two new analytical platforms for the direct study of metabolic changes in cells and tissues following external perturbation. For this purpose we developed a novel technique, laser ablation electrospray ionization (LAESI), for metabolite profiling of functioning cells and tissues. The technique was based on microscopic sampling of biological specimens by mid-infrared laser ablation followed by electrospray ionization of the plume and MS analysis. The two main shortcomings of this technique had been limited specificity due to the lack of a separation step, and limited molecular coverage, especially for nonpolar chemical species. To improve specificity and the coverage of the metabolome, we implemented the LAESI ion source on a mass spectrometer with ion mobility separation (IMS). In this system, the gas phase ions produced by the LAESI source were first sorted according to their collisional cross sections in a mobility cell. These separated ion packets were then subjected to MS analysis. By combining the atmospheric pressure ionization with IMS, we improved the metabolite coverage. Further enhancement of the non-polar metabolite coverage resulted from the combination of laser ablation with vacuum UV irradiation of the ablation plume. Our results indicated that this new ionization modality provided improved detection for neutral and non-polar compounds. Based on rapid progress in photonics, we had introduced another novel ion source that utilized the interaction of a laser pulse with silicon nanopost arrays (NAPA). In these nanophotonic ion sources, the structural features were commensurate with the wavelength of the laser light. The enhanced interaction resulted in high ion yields. This ultrasensitive analytical platform enabled the MS analysis of single yeast cells. We extended these NAPA studies from yeast to other microorganisms, including green algae (Chlamydomonas reinhardtii) that captured energy from sunlight on a massive scale. Combining cellular perturbations, e.g., through environmental changes, with the newly developed single cell analysis methods enabled us to follow dynamic changes induced in the cells. In effect, we were able to use individual cells as a “laboratory,” and approached the long-standing goal of establishing a “lab-in-a-cell.” Model systems for these studies included cells of cyanobacteria (Anabaena), yeast (Saccharomyces cerevisiae), green algae (C. reinhardtii) and Arabidopsis thaliana.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS1998

"CHON" particles: The interstellar component of cometary dust

Interstellar dust is characterized by strong absorption in the ultraviolet and the mid-IR. Current models of interstellar dust are based on three chemically distinct components: a form of carbon (usually graphite), a silicate, and a blend of polycyclic aromatic hydrocarbons or other carbonaceous material. Previous work using effective medium theories to understand the optical properties of cometary dust suggested that an amalgam of materials could reproduce the observed interstellar and cometary dust features. Recently, Lawler and Brownlee (1992) re-analyzed the PIA and PUMA-1 data sets from the Giotto flyby of P/Halley and discovered that the so-called "CHON" particles were actually composed of a blend of carbon-bearing and silicon-bearing materials. Based on effective medium theories, the absorption spectrum of such a material would display the spectral features of each of the components - strong UV absorption from the carbonaceous component and strong absorption in the IR from the silicate component. To test this idea, vapor-deposited samples were created using two different deposition techniques: sputtering with an argon RF magnetron and deposition from an argon plasma torch. Two different compositions were tested: a blend of graphite and silica in a 7:1 ratio and an amalgam of materials whose approximate composition matches the "CHON"-silicate abundances for the uncompressed PIA data set of Lawler and Brownlee: graphite, iron oxide, magnesium oxide, ammonium sulfate, calcium carbonate, and silica in mass ratios of 6:4.3:4:2.2:1:9. The samples were finely ground and pressed into 2" diameter disks using a 40 ton press. In all, four different experiments were performed: one with each of the compositions (C:SiO and "CHON") in both the RF magnetron and the plasma torch chambers. The RF magnetron created a uniform dark thin film on the substrate surface, and the plasma torch created a coating of small (<100 micron) diameter grey particles. The spectra of all four samples show a strong, broad absorption feature at around 220 nm as well as a strong but narrower absorption peak near 10 microns. The RF magnetron sputtered samples showed some sub-structure in the UV, and the peak of the absorption was shifted toward longer wavelengths. The UV absorption in the plasma torch deposited samples have no sub-structure, and the peak absorption is very near 220 nm. Strong absorption near 9 microns is seen in the spectra from both sample preparation techniques, and is consistent with the IR spectra of some terrestrial silicates. Other features, particularly at 6.2 and 8.6 microns, are seen in the interstellar medium. A strong feature near 2 microns is due to absorbed water in the sample. Based on the results of these experiments, there is evidence that a material with a composition similar to that detected in "CHON" particles in the coma of P/Halley have a spectral signature which reproduces the main absorption features of interstellar dust. This suggests that the "CHON" particles could be the interstellar component of cometary dust.

Lien, David J.↗

DOE OSTI2015

In-vitro study of copper doped SiO{sub 2}-CaO-P{sub 2}O{sub 5} system for bioactivity and antimicrobial properties

Samples of the xCuO-(45-x)CaO-10P{sub 2}O{sub 5}-45SiO{sub 2} system (x varies from 0 to 4 mole%) have been synthesized for application as biomaterials to slow or inhibit the growth of living organisms (fungi and other pathogenic microorganisms) by the combination of sol-gel and co-precipitation processes. Prepared samples have been characterized by X-Ray Diffraction, Fourier Transform Infra-Red and Field Emission Scanning Electron Microscopy techniques before and after immersion in simulated body fluid. Antimicrobial activity of samples has been investigated against Staphylococcus aureus. Releasing of Cu{sup 2+}and other ions in the simulated body fluid has been determined by Atomic Absorption Spectroscopy to ensure the use of prepared material as biomaterial with good antibacterial properties.

36 MATERIALS SCIENCE↗

DOE OSTI2017

Structure and Properties of VT6 Alloy Obtained by Layered Selective Sintering of a Powder

This paper is focused on a clarification and analysis of the regularities of formation of the structure and properties of samples of the titanium-based alloy VT6, obtained by methods of conventional metallurgy and formed by layered selective electron-beam sintering in vacuum (using the Arcam A2X (3D printer) system (Arcam, Sweden)) of VT6 titanium powder with particle size 40–100 μm. Additional modification of the samples was realized by irradiating the surface with an intense pulsed electron beam (15 keV, 45 J/cm{sup 2}, 200 μs, 10 pulses, 0.3 s{sup –1}, 3.5·10{sup –2} Pa). It is shown that the action of a pulsed electron beam on the surface of samples formed by layered selective electron-beam sintering leads to a significant reduction in the porosity of the surface layer of the material and formation in the surface layer of a polycrystalline structure (grain size 15–60 μm) with a substructure in the form of crystallization cells (cell size 0.5–1.2 μm). Electron-beam processing of samples prepared by methods of conventional metallurgy for the indicated electron-beam parameters leads to the formation in the surface layer of a polycrystalline structure (grain size 50–800 μm) with a laminar intragrain substructure. Mechanical tests, performed by stretching flat samples, showed that the highest combination of mechanical strength and plasticity is possessed by samples obtained by layered selective electron-beam sintering with subsequent irradiation by an intense pulsed electron beam.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Water Migration and Swelling in Engineered Barrier Materials for Radioactive Waste Disposal

Deep, underground repositories are needed to isolate radioactive waste from the biosphere. Because bentonite is an integral component of many multibarrier repository systems, information on the hydraulic behavior of bentonite is crucial for modeling the long-term viability of such systems. In this paper the hydraulic behavior of bentonite samples was analyzed as a function of aggregate size, and samples were subjected to hydrothermal treatments involving contact with NaCl, KCl, and deionized water. Neutron and X-ray imaging were used to quantify water sorption into packed bentonite samples and bentonite swelling into the water column. The distance between the original clay-water interface and the wetting front was determined as a function of time. Average water uptake exhibited a square-root-of-time dependence in freshly prepared samples, but more variable rates were observed for samples previously in contact with water. The radiography was supported by small-angle neutron scattering analysis and ultra-small-angle neutron scattering analysis of aggregate size distributions and by inelastic neutron scattering to understand the physicochemical environment of the sorbed water. Results showed that hydrothermal treatment with KCl had the greatest effect of increased water transport in the bentonite, possibly as a result of the interaction of K + with smectite layers in the clay.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2020

W-ZrC composites prepared by reactive melt infiltration of Zr 2 Cu alloy into binder jet 3D printed WC preforms

W-ZrC composites were successfully prepared by reactive melt infiltration (RMI) of stoichiometric and excess amounts of Zr 2 Cu into sintered and un-sintered WC preforms made from binder jet 3D printing. The focus of this work was to study the conversion of reactant powders and liquid infiltrant with varying preform density and infiltrant amount by controlling the processing time to reach high conversion yield while understanding the phase composition, microstructure, and hardness. To investigate the effect of time, the reactive melt infiltration was conducted at 1400 °C for 2, 4 and 8 h in a furnace with 96% Ar - 4% H2 gas atmosphere. The increase in reaction time from 2 to 8 h increased the W and W 2 C phase contents and decreased the ZrC phase content when using sintered WC preforms. Samples prepared from un-sintered WC preforms exhibited improved reactive melt infiltration compared to sintered samples, and there was no detectable W 2 C phase and nearly full consumption of WC. Similar to sintered WC samples, the content of W and ZrC phases increased with the increase in time from 2 to 8 h. The interfaces and phases at reaction interfaces were investigated using electron diffraction analysis and S/TEM-EDS to understand material stability; the phases were identified and consistent with XRD analysis. Additionally, there was no Cu present at the interfaces. Increasing the amount of infiltrant led to better reactive melt infiltration. In general, the hardness increased with reaction time and the highest Vickers hardness was found in the W-ZrC sample formed from sintered WC reacted with excess Zr 2 Cu. Finally, this research addresses the critical comparison of sintering and RMI time and shows that by using un-sintered samples for 8 h we are able to achieve W-ZrC composites with fewer undesired phases.

36 MATERIALS SCIENCE↗