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Results for “Energy Dispersive Spectroscopy”

Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 19 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2025

Investigation of UO 2 doped with Fe 2 O 3 sintered under a reducing atmosphere

Nuclear fuel produced with trace amounts of transition metal additives is of potential interest for introducing intentional signatures for accelerating nuclear forensics. In this work, we investigate the effects on microstructure, grain size, crystal structure, and stoichiometry when trace amounts of Fe in the form of Fe 2 O 3 are added to UO 2 . Sintering of compacts with different concentrations, from 250 to 3000 ppmw, was performed under a reducing atmosphere at 1773 K. The persistence of the taggant during the fuel fabrication process as well as its impact on grain size, crystal lattice, and first-neighbor chemistry was evaluated using inductively coupled plasma–optical emission spectroscopy, powder X-ray diffraction (pXRD), Raman spectroscopy, scanning electron microscopy–backscatter electron spectroscopy, energy dispersive spectroscopy, and thermogravimetric analysis. We observed that a negligible amount of Fe was lost during sintering. Our results indicate that the feedstock, Fe 2 O 3 transforms into Fe and FeO under the test sintering conditions. For all compositions, metallic Fe precipitate was found in grain boundaries as a secondary phase. In conclusion, the potential incorporation of ionic Fe into the UO 2 unit cell was determined by pXRD and Raman spectra.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2021

Convergence of micro-geochemistry and micro-geomechanics towards understanding proppant shale rock interaction: A Caney shale case study in southern Oklahoma, USA

As a direct outcome of economic development coupled with an increase in population, global energy demand will continue to rise in the coming decades. Although renewable energy sources are increasingly investigated for optimal production, the immediate needs require focus on energy sources that are currently available and reliable, with a minimal environmental impact; the efficient exploration and production of unconventional hydrocarbon resources is bridging the energy needs and energy aspirations, during the current energy transition period. The main challenges are related to the accurate quantification of the critical rock properties that influence production, their heterogeneity and the multiscale driven physico-chemical nature of rock–fluid interactions. A key feature of shale reservoirs is their low permeability due to dominating nanoporosity of the clay-rich matrix. As a means of producing these reservoirs in a cost-effective manner, a prerequisite is creation of hydraulic fracture networks capable of the highest level of continued conductivity. Fracturing fluid chemical design, formation brine geochemical composition, and rock mineralogy all contribute to swelling-induced conductivity damage. The Caney Shale is an organic-rich, often calcareous mudrock. Many studies have examined the impact that clay has on different kinds of shale productivity but there is currently no data reported on the Caney Shale in relation to horizontal drilling; all reported data on the Caney Shale is on vertical wells which are shallow, compared to an emerging play that is at double the depth. Here, in this work we develop geochemical–geomechanical integration of rock properties at micro-and nanoscales that can provide insights into the potential proppant embedment and its mitigation. The novel methodology amalgamates the following: computed X-ray tomography, scanning electron microscopy, energy dispersive spectroscopy, micro-indentation, and Raman spectroscopy techniques. Here, our results show that due to the multiscale heterogeneity in the Caney Shale, these geochemical and structural properties translate into a variation in mechanical properties that will impact interaction between the proppant and the host shale rock.

03 NATURAL GAS↗
NASA NTRS1997

Solar Cells for Lunar Application

In this work a preliminary study of the vacuum evaporation of silicon extracted from the lunar regolith has been undertaken. An electron gun vacuum evaporation system has been adapted for this purpose. Following the calibration of the system using ultra high purity silicon deposited on Al coated glass substrates, thin films of lunar Si were evaporated on a variety of crystalline substrates as well as on glass and lightweight 1 mil (25 microns) Al foil. Extremely smooth and featureless films with essentially semiconducting properties were obtained. Optical absorption analysis sets the bandgap (about 1.1 eV) and the refractive index (n=3.5) of the deposited thin films close to that of crystalline silicon. Secondary ion mass spectroscopy and energy dispersive spectroscopy analysis indicated that these films are essentially comparable to high purity silicon and that the evaporation process resulted in a substantial reduction of impurity levels. All layers exhibited a p-type conductivity suggesting the presence of a p-type dopant in the fabricated layers. While the purity of the 'lunar waste material' is below that of the 'microelectronic-grade silicon', the vacuum evaporated material properties seems to be adequate for the fabrication of average performance Si-based devices such as thin film solar cells. Taking into account solar cell thickness requirements (greater than 10 microns) and the small quantities of lunar material available for this study, solar cell fabrication was not possible. However, the high quality of the optical and electronic properties of evaporated thin films was found to be similar to those obtained using ultra-high purity silicon suggest that thin film solar cell production on the lunar surface with in situ resource utilization may be a viable approach for electric power generation on the moon.

Freundlich, Alex↗
NASA NTRS2005

Chemically Deposited Thin-Film Solar Cell Materials

We have been working on the development of thin film photovoltaic solar cell materials that can be produced entirely by wet chemical methods on low-cost flexible substrates. P-type copper indium diselenide (CIS) absorber layers have been deposited via electrochemical deposition. Similar techniques have also allowed us to incorporate both Ga and S into the CIS structure, in order to increase its optical bandgap. The ability to deposit similar absorber layers with a variety of bandgaps is essential to our efforts to develop a multi-junction thin-film solar cell. Chemical bath deposition methods were used to deposit a cadmium sulfide (CdS) buffer layers on our CIS-based absorber layers. Window contacts were made to these CdS/CIS junctions by the electrodeposition of zinc oxide (ZnO). Structural and elemental determinations of the individual ZnO, CdS and CIS-based films via transmission spectroscopy, x-ray diffraction, x-ray photoelectron spectroscopy and energy dispersive spectroscopy will be presented. The electrical characterization of the resulting devices will be discussed.

Raffaelle, R.↗
DOE OSTI2022

Unusual flat and extended morphology of intercalated Cu under MoS 2

We report a general method was developed to intercalate metals under layered materials through a controlled density of sputtered defects. The method has already been applied to study a range of metals intercalated under graphite, and different types of morphologies were realized. In the current work, we extend the method to the study of intercalation under MoS 2 , noting that work on this system is rather limited. We use Cu as the prototype metal for comparison with Cu intercalation under graphite. Although the growth conditions needed for intercalation under graphite and MoS 2 are similar, the type of intercalated phases is very different. Each Cu island that nucleates on top of MoS 2 during Cu deposition provides material that is transferred below MoS 2 through sputtered defects under the island base; this transfer results in a uniform intercalated Cu “carpet” morphology that extends over the mesoscale. On the contrary, Cu intercalation under graphite results in well separated, compact islands formed by monomer detachment from small Cu islands on top and transfer below through defects far from the islands. The structural techniques (scanning electron microscopy and atomic force microscopy) and spectroscopic techniques (x-ray photoelectron spectroscopy and energy-dispersive spectroscopy) are used for the characterization of the intercalated Cu layer.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2020

In Situ Oxidation Studies of High-Entropy Alloy Nanoparticles

Although high-entropy alloys (HEAs) have shown tremendous potential for elevated temperature, anticorrosion, and catalysis applications, little is known on how HEA materials behave under complex service environments. Herein, we studied the high-temperature oxidation behavior of Fe 0.28 Co 0.21 Ni 0.20 Cu 0.08 Pt 0.23 HEA nanoparticles (NPs) in an atmospheric pressure dry air environment by in situ gas-cell transmission electron microscopy. It is found that the oxidation of HEA NPs is governed by Kirkendall effects with logarithmic oxidation rates rather than parabolic as predicted by Wagner's theory. Further, the HEA NPs are found to oxidize at a significantly slower rate compared to monometallic NPs. The outward diffusion of transition metals and formation of disordered oxide layer are observed in real time and confirmed through analytical energy dispersive spectroscopy, and electron energy loss spectroscopy characterizations. Localized ordered lattices are identified in the oxide, suggesting the formation of Fe 2 O 3 , CoO, NiO, and CuO crystallites in an overall disordered matrix. Hybrid Monte Carlo and molecular dynamics simulations based on first-principles energies and forces support these findings and show that the oxidation drives surface segregation of Fe, Co, Ni, and Cu, while Pt stays in the core region. The present work offers key insights into how HEA NPs behave under high-temperature oxidizing environment and sheds light on future design of highly stable alloys under complex service conditions.

36 MATERIALS SCIENCE↗
NASA NTRS2003

Defect Clustering and Nano-Phase Structure Characterization of Multi-Component Rare Earth Oxide Doped Zirconia-Yttria Thermal Barrier Coatings

Advanced oxide thermal barrier coatings have been developed by incorporating multi-component rare earth oxide dopants into zirconia-yttria to effectively promote the creation of the thermodynamically stable, immobile oxide defect clusters and/or nano-scale phases within the coating systems. The presence of these nano-sized defect clusters has found to significantly reduce the coating intrinsic thermal conductivity, improve sintering resistance, and maintain long-term high temperature stability. In this paper, the defect clusters and nano-structured phases, which were created by the addition of multi-component rare earth dopants to the plasma-sprayed and electron-beam physical vapor deposited thermal barrier coatings, were characterized by high-resolution transmission electron microscopy (TEM). The defect cluster size, distribution, crystallographic and compositional information were investigated using high-resolution TEM lattice imaging, selected area diffraction (SAD), electron energy-loss spectroscopy (EELS) and energy dispersive spectroscopy (EDS) analysis techniques. The results showed that substantial defect clusters were formed in the advanced multi-component rare earth oxide doped zirconia- yttria systems. The size of the oxide defect clusters and the cluster dopant segregation was typically ranging from 5 to 50 nm. These multi-component dopant induced defect clusters are an important factor for the coating long-term high temperature stability and excellent performance.

Zhu, Dongming↗
NASA NTRS2015

Analyses of Hubble Space Telescope Aluminized-Teflon Multilayer Insulation Blankets Retrieved After 19 Years of Space Exposure

Since its launch in April 1990, the Hubble Space Telescope (HST) has made many important observations from its vantage point in low Earth orbit (LEO). However, as seen during five servicing missions, the outer layer of multilayer insulation (MLI) has become increasingly embrittled and has cracked in many areas. In May 2009, during the 5th servicing mission (called SM4), two MLI blankets were replaced with new insulation and the space-exposed MLI blankets were retrieved for degradation analyses by teams at NASA Glenn Research Center (GRC) and NASA Goddard Space Flight Center (GSFC). The retrieved MLI blankets were from Equipment Bay 8, which received direct sunlight, and Equipment Bay 5, which received grazing sunlight. Each blanket was divided into several regions based on environmental exposure and/or physical appearance. The aluminized-Teflon (DuPont, Wilmington, DE) fluorinated ethylene propylene (Al-FEP) outer layers of the retrieved MLI blankets have been analyzed for changes in optical, physical, and mechanical properties, along with chemical and morphological changes. Pristine and as-retrieved samples (materials) were heat treated to help understand degradation mechanisms. When compared to pristine material, the analyses have shown how the Al-FEP was severely affected by the space environment. Most notably, the Al-FEP was highly embrittled, fracturing like glass at strains of 1 to 8 percent. Across all measured properties, more significant degradation was observed for Bay 8 material as compared to Bay 5 material. This paper reviews the tensile and bend-test properties, density, thickness, solar absorptance, thermal emittance, x-ray photoelectron spectroscopy (XPS) and energy dispersive spectroscopy (EDS) elemental composition measurements, surface and crack morphologies, and atomic oxygen erosion yields of the Al-FEP outer layer of the retrieved HST blankets after 19 years of space exposure.

Radiation↗
NASA NTRS1999

Analyses of Contaminated Solar Array Handrail Samples Retrieved from Mir

In January 1998 during, the STS-89 mission, an eight section Russian solar array panel was retrieved after more than ten years exposure to the orbital space environment on the Russian space station Mir. Two darkened handrail samples from the Russian solar array have been evaluated for contamination: a section of a white paint covered rigid handrail and a section of woven fabric over-wrapped around a flexible handhold. The handrail samples were evaluated using optical microscopy (OM), field emission scanning electron microscopy (FESEM) and energy dispersive spectroscopy (EDS). Optical properties were also obtained. Microscopy has shown the discolored areas to have thick layers of contaminant that has crazed and spalled off in regions. Energy dispersive spectroscopy revealed that the brown contaminant is composed of oxidized silicon. No silicon was present on the unexposed fabric over-wrap, and very small amounts were present in the white paint. Therefore, the contaminant layer on both samples is attributed to silicone contamination from other spacecraft materials that have been oxidized by atomic oxygen while in orbit. A significant source of the silicone contamination appears to be from the solar array itself.

deGroh, Kim K.↗
DOE OSTI2023

Three-dimensional atomic structure and local chemical order of medium- and high-entropy nanoalloys

Medium- and high-entropy alloys (M/HEAs) mix several principal elements with near-equiatomic composition and represent a model-shift strategy for designing previously unknown materials in metallurgy, catalysis and other fields. One of the core hypotheses of M/HEAs is lattice distortion, which has been investigated by different numerical and experimental techniques. However, determining the three-dimensional (3D) lattice distortion in M/HEAs remains a challenge. Moreover, the presumed random elemental mixing in M/HEAs has been questioned by X-ray and neutron studies, atomistic simulations, energy dispersive spectroscopy and electron diffraction, which suggest the existence of local chemical order in M/HEAs. However, direct experimental observation of the 3D local chemical order has been difficult because energy dispersive spectroscopy integrates the composition of atomic columns along the zone axes and diffuse electron reflections may originate from planar defects instead of local chemical order. Here, in this work, we determine the 3D atomic positions of M/HEA nanoparticles using atomic electron tomography and quantitatively characterize the local lattice distortion, strain tensor, twin boundaries, dislocation cores and chemical short-range order (CSRO). We find that the high-entropy alloys have larger local lattice distortion and more heterogeneous strain than the medium-entropy alloys and that strain is correlated to CSRO. We also observe CSRO-mediated twinning in the medium-entropy alloys, that is, twinning occurs in energetically unfavoured CSRO regions but not in energetically favoured CSRO ones, which represents, to our knowledge, the first experimental observation of correlating local chemical order with structural defects in any material. We expect that this work will not only expand our fundamental understanding of this important class of materials but also provide the foundation for tailoring M/HEA properties through engineering lattice distortion and local chemical order.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Understanding the Effect of Electron Beam Melting Scanning Strategies on the Aluminum Content and Materials State of Single Ti-6Al-4V Feedstock

Research on the additive manufacturing of metals often neglects any characterization of the composition of final parts, erroneously assuming a compositional homogeneity that matches the feedstock material. Here, the composition of electron-beam-melted Ti-6Al-4V produced through three distinct scanning strategies (linear raster and two point melting strategies, random fill and Dehoff fill) is characterized both locally and globally through energy-dispersive spectroscopy and quantitative chemical analysis. As a result of the different scanning strategies used, differing levels of preferential vaporization occur across the various parts, leading to distinct final compositions, with extremes of ~5.8 wt.% Al and ~4.8 wt.% Al. In addition, energy-dispersive spectroscopy composition maps reveal specific features in both the XY and XZ planes (with Z being the build direction) as a result of local inhomogeneous preferential vaporization. The subsequent change in composition significantly modifies the materials’ state of parts, wherein parts and local regions with higher aluminum contents lead to higher hardness levels (with a ~50 HV difference) and elastic property values and vice versa. While varying scan strategies and scan parameters are known to modify the microstructure and properties of a part, the effect on composition cannot, and should not, be neglected.

36 MATERIALS SCIENCE↗
DOE OSTI2021

High-Entropy 2D Carbide MXenes: TiVNbMoC 3 and TiVCrMoC 3

Two-dimensional (2D) transition metal carbides and nitrides, known as MXenes, are a fast-growing family of 2D materials. MXenes 2D flakes have n + 1 (n = 1-4) atomic layers of transition metals interleaved by carbon/nitrogen layers, but to-date remain limited in composition to one or two transition metals. In this study, by implementing four transition metals, we report the synthesis of multi-principal-element high-entropy M 4 C 3 T x MXenes. Specifically, we introduce two high-entropy MXenes, TiVNbMoC 3 T x and TiVCrMoC 3 T x , as well as their precursor TiVNbMoAlC 3 and TiVCrMoAlC 3 high-entropy MAX phases. We used a combination of real and reciprocal space characterization (X-ray diffraction, X-ray photoelectron spectroscopy, energy dispersive X-ray spectroscopy, and scanning transmission electron microscopy) to establish the structure, phase purity, and equimolar distribution of the four transition metals in high-entropy MAX and MXene phases. We use first-principles calculations to compute the formation energies and explore synthesizability of these high-entropy MAX phases. We also show that when three transition metals are used instead of four, under similar synthesis conditions to those of the four-transition-metal MAX phase, two different MAX phases can be formed (i.e., no pure single-phase forms). This finding indicates the importance of configurational entropy in stabilizing the desired single-phase high-entropy MAX over multiphases of MAX, which is essential for the synthesis of phase-pure high-entropy MXenes. The synthesis of high-entropy MXenes significantly expands the compositional variety of the MXene family to further tune their properties, including electronic, magnetic, electrochemical, catalytic, high temperature stability, and mechanical behavior.

2D materials↗
DOE OSTI2021

Structural and chemical changes from CO2 exposure to self-healing polymer cement composites for geothermal wellbores

Wellbore cement is subjected to a number of mechanical, thermal and chemical stress regimes over its lifetime. Therefore, next generation wellbore cement formulations need to be evaluated in conditions relevant to these environments. In this work, we investigate the mechanism of the alteration of a novel self-healing polymer-cement composite recently reported by our group after exposure to a CO2-rich environment by using synchrotron based X-ray Fluorescence (XRF) and X-ray absorption near edge structure (XANES) and scanning electron microscopy coupled with energy dispersive spectroscopy. Results showed that chemical alteration of the polymer-cement follows the rim carbonation mechanism, similar to conventional cement although carbonation takes place to a lesser extent in polymer-cements despite the higher porosity. Along with detailed mechanistic insights on carbonation in polymer-cement composite, the performance of these in CO2-rich environment is further studied using standard compressive strength analysis.

Elbakhshwan, Mohamed↗
NASA NTRS2015

NASA Work Experience

I have had the opportunity to support the analytical laboratories in chemical analysis of unknown samples, using Optical Microscopy (OM), Polarizing Light Microscopy (PLM), Fourier-Transform Infrared Spectroscopy (FT-IR), Scanning Electron Microscopy with Energy Dispersive Spectroscopy (SEMEDS), and X-ray Powder Diffraction (XPD). I have assisted in characterizing fibers pulled from a spacecraft, a white fibrous residue discovered in a jet refueler truck, brown residue from a plant habitat slated for delivery to the ISS (International Space Station), corrosion on a pipe from a sprinkler, and air filtration material brought back from the ISS. I also conducted my own fiber study in order to practice techniques and further my understanding of background concepts. Furthermore, I had the opportunity to participate in diverse work assignments, where I was assigned to work with other branches of the engineering department for 1-2 days each. The first was in the Materials Science branch where I participated in the construction of the plant habitat intended for use in research aboard the ISS. The second was in the Testing Design branch where I assisted with tensile and hardness testing of over 40 samples. In addition, I have had the privilege to attend multiple tours of the NASA KSC campus, including to the Astronaut Crew Quarters, the VAB (the main area, the Columbia room, and the catwalk), the Visitor Center housing the shuttle Atlantis, the Saturn-V exhibit, the Prototype laboratory, SWAMP WORKS, the Shuttle Landing Facility, the Crawler, and the Booster Fabrication Facility (BFF). Lastly, much of my coursework prepared me for this experience, including numerous laboratory courses with topics diverse as chemistry, physics, and biology.

Florida Tech↗
DOE OSTI2024

Investigation of Chemical Species in the Corrosion Barrier Layer on Thermal CO 2 Treated AZ91D Magnesium Alloy with Lithium Nitrate

A unique corrosion barrier layer, formed by thermal CO 2 treatment with LiNO 3 on AZ91D, was characterized to reveal the chemical species and their spatial distribution using the combination of scanning transmission electron microscopy (STEM), energy dispersive spectroscopy (EDS), and electron energy loss spectroscopy (EELS) techniques. Two distinct and spatially segregated phases were identified as Li compound(s) with MgCO 3 and MgO in the surface barrier layer. Finally, based on the characterization results, it is presumed that the reaction of Mg oxide/hydroxide with LiNO 3 and CO 2 occurred preferentially in some local areas where Li compound(s) with MgCO 3 were present, but the unreacted areas contained MgO in the surface barrier layer.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Surface and subsurface characterization of laser-interference structured Ti6Al4V

Ti6Al4V specimens were exposed to high-energy laser pulses of 1.24 J/cm 2 fluences per pulse using a two-beam optical configuration to attain laser-interference. In addition to the formation of periodic surface textures by laser-interference, scanning electron microscope (SEM) images demonstrated several microstructural changes on the surface processed. Moreover, the surface and subsurface of Ti6Al4V specimens were characterized for the as-received and laser-interference processed conditions using x-ray photoelectron spectroscopy (XPS) and electron energy dispersive spectroscopy (EDS). The XPS data showed that this laser technique is effective at removal of surface contaminants for Ti6Al4V. The XPS analysis also revealed the formation of an oxy-nitride layer on the laser treated material. Finally, the microstructure analysis indicates that grain refinement, dendrite and twin structures were found near the surface due to laser processing.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Oxidation of Alloy X in Subcritical, Transition, and Supercritical Water

This work investigates the oxidation of a nickel-based superalloy, namely Alloy X, in water at elevated temperatures: subcritical water at 261°C and 27 MPa, the transition between subcritical and supercritical water at 374°C and 27 MPa, and supercritical water at 380°C and 27 MPa for 100 h. The morphology of the sample surfaces were studied using scanning electron microscopy coupled with focused ion beam milling, and the surface chemistry was investigated using x-ray diffraction, Raman spectroscopy, energy dispersive x-ray spectroscopy, and x-ray photoelectron spectroscopy before and after exposure studies. Surfaces of all samples were identified to comprise of a ferrite spinel containing aluminum.

Materials Science↗
NASA NTRS2006

Ultrasonication of Bismuth Telluride Nanocrystals Fabricated by Solvothermal Method

The objective of this study is to evaluate the effect of ultrasonication on bismuth telluride nanocrystals prepared by solvothermal method. In this study, a low dimensional nanocrystal of bismuth telluride (Bi2Te3) was synthesized by a solvothermal process in an autoclave at 180 C and 200 psi. During the solvothermal reaction, organic surfactants effectively prevented unwanted aggregation of nanocrystals in a selected solvent while controlling the shape of the nanocrystal. The atomic ratio of bismuth and tellurium was determined by energy dispersive spectroscopy (EDS). The cavitational energy created by the ultrasonic probe was varied by the ultrasonication process time, while power amplitude remained constant. The nanocrystal size and its size distribution were measured by field emission scanning electron microscopy (FESEM) and a dynamic light scattering system. When the ultrasonication time increased, the average size of bismuth telluride nanocrystal gradually increased due to the direct collision of nanocrystals. The polydispersity of the nanocrystals showed a minimum when the ultrasonication was applied for 5 min. Keywords: bismuth telluride, nanocrystal, low-dimensional, ultrasonication, solvothermal

Chu, Sang-Hyon↗