Search NASA⌕ Search

SEARCH · Search NASA

Results for “X ray diffraction analysis”

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.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 1,099 records · Page 61
All sourcesNASA NTRSDOE OSTI
DOE OSTI2021

Effects of Co doping on the structure and physicochemical properties of hausmannite (Mn 3 O 4 ) and its transformation during aging

Hausmannite is a common low-valence manganese oxide mineral with a distorted spinel structure in surficial sediments. Although natural Mn oxides often contain various transition metal (TM) impurities, few studies have addressed the substitution mechanisms of TMs, such as cobalt (Co), with hausmannite and induced changes in the mineral physicochemical properties. In this study, Co-doped hausmannites with final Co/Mn molar ratios of 0.05 and 0.11 were synthesized and characterized by wet chemical analysis, powder X-ray diffraction (XRD), Fourier transformed infrared spectra (FTIR), high resolution transmission electron microscope (HRTEM), X-ray photoelectron spectroscopy (XPS) and X-ray absorption fine structure spectroscopy (XAFS). Co-doped samples have larger crystallite sizes and smaller specific surface areas than those of the hausmannite without Co. The Co cations exist in a mixed-valence of +3 and + 2. Powder XRD and acid dissolution experiments indicate that Co incorporates into the mineral structures, and increases the mineral structural stability. Co K-edge extended X-ray adsorption fine structure (EXAFS) analysis demonstrates that Co likely substitutes for lattice Mn(III). After aging at room temperature for three years, 14.1 ± 1.9% of pure hausmannite is transformed to manganite while only 2.6 ± 0.7% of manganite appears in the aged Co-doped sample with an initial Co/Mn molar ratio of 0.10. Finally, these results provide new insights into the incorporation mechanisms of TMs into low valence Mn oxides, and the stability of these minerals in natural environments.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2026

Physicochemical evolution of uranium nitride kernel microstructure with varying carbon distribution for advanced TRISO fuel forms

Uranium nitride (UN) has emerged as a fuel candidate for advanced nuclear reactor concepts due to its superior uranium density, thermal conductivity, and high melting temperature. However, the fabrication route for converting UO 2 to UN is complex and difficult to standardize. Although the chemistry of this conversion process is well-studied, more insight into the physicochemical dynamics of this conversion using advanced characterization techniques can help further our understanding of this material system. This work leveraged thermogravimetric analysis (TGA), X-ray diffraction (XRD), and nondestructive 3D X-ray computed tomography (XCT) to characterize dynamic microstructural changes in the UO 2 → UCO → UN fabrication pathway for two kernels with a varying carbon distribution in the starting composition. TGA and XRD were used to quantify changes in the mass, density, and chemical composition of the two kernels, while three-dimensional image processing and segmentation of XCT data were used to quantify the volume, surface area, and spatial distribution of features within each kernel for multiple steps along the fabrication pathway. The analysis indicates distinct differences between the two kernels that are correlated to downstream conversion efficiency. In conclusion, this work is among the first to perform 3D quantification of physicochemical evolution during UN conversion, providing quantitative correlation between processing, properties, and expected fuel performance.

Nuclear fuel↗
DOE OSTI2013

Er{sup 3+}-doped strontium lithium bismuth borate glasses for broadband 1.5 {mu}m emission - optical properties

Strontium lithium bismuth borate glasses (SLBiB) doped with various concentrations of Er{sup 3+} were prepared using conventional melt quench technique and investigated their optical properties. The amorphous nature of the prepared glass samples was confirmed by X-ray diffraction and SEM analysis. Optical properties were studied by measuring the optical absorption and near infrared luminescence spectra at room temperature. Judd-Ofelt (J-O) theory has been applied for the f.f transitions of Er{sup 3+} ions to evaluate J-O intensity parameters, {Omega}{lambda} ({lambda} = 2, 4 and 6). Using the J-O intensity parameters, radiative properties such as transition probabilities (A{sub R}), branching ratios ({beta}) and radiative lifetimes ({tau}) are estimated for certain transitions. From the emission spectra, peak emission-cross sections ({sigma}{sub p}) and products of stimulated emission cross-section and full width at half maximum ({sigma}{sub p} Multiplication-Sign FWHM) were calculated for the observed emission transition, {sup 4}I{sub 13/2}{yields}{sup 4}I{sub 15/2}.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Effect of the Fe/Ba Ratio and Sintering Temperature on Microstructure and Magnetic Properties of Barium Ferrites Prepared by Hydrothermal Method

Magnetoplumbite-type (M-type) hexagonal barium ferrite particles were synthesized by a hydrothermal method. The structure and magnetic properties of barium ferrites were investigated systematically, which indicated that the ratio of Fe/Ba (R{sub F/B}) and sintering temperature have an important effect on structure and performance. Phase composition, micro-morphology, and magnetic properties of the particles were investigated by X-ray powder diffraction (XRD) analysis, scanning electron microscopy (SEM), and vibrating sample magnetometry (VSM). When the ratio of Fe/Ba (R{sub F/B}) is even low or high, inferior images of XRD could be attained with certain impurities. When R{sub F/B} = 8, the single phase could be obtained without impurities. Micro-morphology of the particles exhibits the uniform plane hexagonal structures of nano-sized M-type ferrites when sintered at 800 °C. Saturation magnetization (M{sub s}) reaches the maximum value at R{sub F/B} = 7 (M{sub s} = 45.07 emu/g). The value of coercivity (H{sub c}) increases with the growth of R{sub F/B}, and H{sub c} is up to 6207 Oe when R{sub F/B} = 7. The effect of R{sub F/B} and temperature on magnetization (M{sub s}) and coercivity (H{sub c}) was studied in this paper.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2014

Characterization of ultrafine-grained aluminum tubes processed by Tube Cyclic Extrusion–Compression (TCEC)

Tube Cyclic Extrusion–Compression as a novel severe plastic deformation technique for tubes was utilized for processing ultrafine grained 1050 aluminum alloy for the first time. In this method, aluminum tube is fully constrained and deformed between mandrel and chamber with a small neck zone. The material deformation during Tube Cyclic Extrusion–Compression processing analyzed and the grain refinement mechanism were described. The capability of Tube Cyclic Extrusion–Compression in grain refinement of the aluminum alloy was demonstrated by transmission electron microscopy observations and X-ray diffraction line profile analysis. The micrographs of the evolved microstructure show grain size of 850 nm and 550 nm after the first and second processing cycles of Tube Cyclic Extrusion–Compression, respectively. Mechanical properties of the initial and processed specimens were extracted from ring-hoop tensile tests. The documented results confirm grain refinement by showing remarkable increase in the yield and ultimate strengths. The main increase in strength and decrease in elongation take place after the first cycle. The microhardness assessments illustrate increase from the initial value of 29 Hv to 44 and 49 Hv respectively after the first and second cycles of Tube Cyclic Extrusion–Compression. There is a good homogeneity in peripheral microhardness and microhardness across the tube thickness. - Highlights: • Tubes of AA1050 for the first time were successfully SPD processed by TCEC. • The grain size was refined to 550 nm after two cycles of TCEC. • Notable increase in the strength and decrease in the elongation were documented. • The microhardness increased to 49 Hv from the initial value of 29 Hv. • Good homogeneity in the microhardness distribution was recorded.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Study of microstress state of P91 steel using complementary mechanical Barkhausen, magnetoacoustic emission, and X-ray diffraction techniques

The paper deals with assessment of microstress state of martensite P91 steel using three complementary techniques: mechanical Barkhausen emission, magnetoacoustic emission (MAE), and X-ray diffraction (XRD) profile analysis. Magnetic coercivity Hc and microstructure were investigated with inductive magnetometry and magnetic force microscopy (MFM), respectively. Internal stress level of P91 steel was modified by heat treatment. Steel samples were austenitized, quenched, and then tempered at three temperatures (720 °C, 750 °C, and 780 °C) during increasing time (from 15 min up to 240 min). The microstrain level ε{sub i} was evaluated using Williamson–Hall method. It was revealed that during tempering microstrain systematically decreases from ε{sub i} = 2.5 × 10{sup −3} for as quenched state down to ε{sub i} = 0.3 × 10{sup −3} for well tempered samples. Both mechanical hardness (Vicker's HV) and magnetic hardness (coercivity) decrease almost linearly with decreasing microstrain while the MAE and MBE intensities strongly increase. Tempering leads to evident shift of the MeBN intensity maximum recorded for the first load towards lower applied strain values and to increase of MAE intensity. This indicates that the microstress state deduced by magnetic techniques is correlated with microstrains evaluated with XRD technique.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Graphene Oxide/Polyaniline/Manganese Oxide Ternary Nanocomposites, Facile Synthesis, Characterization, and Application for Indigo Carmine Removal

Graphene oxide/polyaniline/manganese oxide ternary nanocomposites (GO/PANI/Mn{sub 2}O{sub 3}) have been successfully synthesized in one-pot method by in situ chemical oxidative polymerization of aniline in acidic medium using MnO{sub 2} as an oxidant. The obtaining nanocomposites have been characterized by transmission electron microscope, Fourier transform infrared, X-ray powder diffraction, and thermogravimetric analysis. The adsorption isotherms of indigo carmine (IC) onto; PANI, GO/PANI, PANI/MnO{sub 2}, and GO/PANI/Mn{sub 2}O{sub 3} have been evaluated under different adsorption conditions. The adsorption isotherm models of Langmuir, Freundlich, and Temkin were applied and the fit linear was obtained with Langmuir model. It was found that adsorption capacities followed the order: GO/PANI > GO/PANI/Mn{sub 2}O{sub 3} > PANI > PANI/MnO{sub 2} with the values of 88.73, 76.40, 60.45 and 22.52 mg/g. Moreover, the kinetics of the adsorption process was investigated and fit linear was obtained with pseudo-second-order model. The adsorption process was exothermic and spontaneous as revealed from the thermodynamic studies.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Influence of magnesia-to-phosphate molar ratio on microstructures, mechanical properties and thermal conductivity of magnesium potassium phosphate cement paste with large water-to-solid ratio

This paper describes the influence of the magnesia-to-phosphate (M/P) molar ratios ranging from 4 to 12, on the properties and microstructures of magnesium potassium phosphate cement (MKPC) pastes with a large water-to-solid ratio (w/s) of 0.50. The setting behavior, compressive strength, tensile bonding strength and thermal conductivity of the MKPC pastes, were investigated. The results show that an increase in the M/P ratio can slow down the setting reaction, and clearly degrade the mechanical strengths, but clearly improve the thermal conductivity of MKPC pastes. Furthermore, micro-characterizations including X-ray diffraction, scanning electron microscopy and thermogravimetric analysis, on the MKPC pastes reveal that a lower M/P ratio can facilitate better crystallization of the resultant magnesium potassium phosphate hexahydrate (MKP) and a denser microstructure. Moreover, strong linear correlations are found between the mechanical strengths and the MKP-to-space ratio, and between thermal conductivity and the volume ratio of the unreacted magnesia to the MKP. - Highlights: • Increase of M/P molar ratio causes clear mechanical degradations on MKPC pastes. • Thermal conductivity of MKPC pastes is improved with increase of M/P molar ratio. • Lower M/P ratio leads to better MKP crystallization and denser microstructure. • Strengths of MKPC pastes are linearly correlated to the MKP-to-space ratios. • Thermal conductivity is affected by the volume ratio of unreacted magnesia to MKP.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Single-Crystal Synthesis and Characterization of Copper-Intercalated ZrTe 5

Herein is presented the synthesis and characterization of copper-intercalated zirconium pentatelluride (ZrTe 5 ). ZrTe 5 :Cu 0.05 crystals are synthesized by the chemical vapor transport method in a vacuum. X-ray diffraction and elemental analysis techniques are utilized to validate the synthesis. The results indicate that the intercalation of the layered Zr/Te structure with copper atoms causes the contraction of the unit cell along all three crystalline directions, the shrinkage of the overall volume of the unit cell, and the distortion of the unit cell. A single crystal was isolated, mechanically exfoliated, and used for the measurements of intercalation strains in a Hall bar device. Electronic transport studies indicate that an anomalous resistance drop is observed at T = 19 K. Furthermore, R xx and R xy results, respectively, indicate a probable disorder-induced localization effect and electron-type carriers.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Mechanical behavior of carbonated MgO-based Engineered Cementitious Composite (ECC) after high temperatures exposure

Carbonated MgO-based Engineered Cementitious Composite (ECC) has ultrahigh tensile ductility and tight crack width control behavior. However, the expectation of improved fire-resistant has not been confirmed. This study explored the alterations to mechanical and microstructure characteristics of this material after exposure to temperatures up to 500 °C. Material mass loss, compressive strength, tensile strength, strain capacity, and matrix fracture toughness were measured. Scanning electron microscopy, mercury intrusion porosimetry, thermogravimetric analysis, and X-ray diffraction were used to probe the degradation of the cement matrix and fibers. The effect of elevated temperature on carbonated MgO-based ECC was further assessed via examination of the micromechanical behavior of the fiber-matrix. The objective of this research was to assess the performance of carbonated MgO-based ECC exposed to fire hazards. The tensile ductility of carbonated MgO-based ECC was found to be enhanced when exposed to ~100 °C as compared with those at room temperature ~20 °C. Further increase in exposure temperature, however, posed a negative impact on the composite compressive strength, ultimate tensile strength, and ability to control crack width. Here the results provide a useful database for further investigations into carbonated MgO-based ECC for fire safety enhancement.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Study on the hydration and microstructure of Portland cement containing diethanol-isopropanolamine

Diethanol-isopropanolamine (DEIPA) is a tertiary alkanolamine used in the formulation of cement grinding-aid additives and concrete early-strength agents. In this research, isothermal calorimetry was used to study the hydration kinetics of Portland cement with DEIPA. A combination of X-ray powder diffraction (XRPD), scanning electron microscopy (SEM), differential scanning calorimetry (DSC)–thermogravimetric (TG) analysis and micro-Raman spectroscopy was used to investigate the phase development in the process of hydration. Mercury intrusion porosimetry was used to study the pore size distribution and porosity. The results indicate that DEIPA promotes the formation of ettringite (AFt) and enhances the second hydration rate of the aluminate and ferrite phases, the transformation of AFt into monosulfoaluminate (AFm) and the formation of microcrystalline portlandite (CH) at early stages. At later stages, DEIPA accelerates the hydration of alite and reduces the pore size and porosity.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Growth and characterization of metamorphic InAs/GaSb tunnel heterojunction on GaAs by molecular beam epitaxy

The structural, morphological, optical, and electrical transport characteristics of a metamorphic, broken-gap InAs/GaSb p-i-n tunnel diode structure, grown by molecular beam epitaxy on GaAs, were demonstrated. Precise shutter sequences were implemented for the strain-balanced InAs/GaSb active layer growth on GaAs, as corroborated by high-resolution X-ray analysis. Cross-sectional transmission electron microscopy and detailed micrograph analysis demonstrated strain relaxation primarily via the formation of 90° Lomer misfit dislocations (MDs) exhibiting a 5.6 nm spacing and intermittent 60° MDs at the GaSb/GaAs heterointerface, which was further supported by a minimal lattice tilt of 180 arc sec observed during X-ray analysis. Selective area diffraction and Fast Fourier Transform patterns confirmed the full relaxation of the GaSb buffer layer and quasi-ideal, strain-balanced InAs/GaSb heteroepitaxy. Temperature-dependent photoluminescence measurements demonstrated the optical band gap of the GaSb layer. Strong optical signal at room temperature from this structure supports a high-quality material synthesis. Current–voltage characteristics of fabricated InAs/GaSb p-i-n tunnel diodes measured at 77 K and 290 K demonstrated two bias-dependent transport mechanisms. The Shockley–Read–Hall generation–recombination mechanism at low bias and band-to-band tunneling transport at high bias confirmed the p-i-n tunnel diode operation. This elucidated the importance of defect control in metamorphic InAs/GaSb tunnel diodes for the implementation of low-voltage and high-performance tunnel field effect transistor applications.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2013

[Bmim][TfO] ionic liquid-assisted oriented growth of Co{sub 3}O{sub 4} nanoworms

Graphical abstract: Display Omitted Highlights: ► First time, we have used [Bmim][TfO]IL for the synthesis of Co{sub 3}O{sub 4} nanoworms. ► IL assists to form oriented growth of cubic Co{sub 3}O{sub 4} nanoworms without intermediate. ► Cubic Co{sub 3}O{sub 4} nanoworms are in the range of 20 nm width and 100–200 nm length. ► IL and oxidizing agent have not altered the Co{sub 3}O{sub 4} structural characteristics. ► Co{sub 3}O{sub 4} nanoworms exhibit crystalline domain dependent weak ferromagnetism. -- Abstract: Monodispersed worm-like structure of Co{sub 3}O{sub 4} nanocrystals of 20 nm width and 100–200 nm length are prepared directly without any intermediate product by 1-n-butyl-3-methylimidazolium trifluoromethane sulfonate ionic liquid ([Bmim][TfO] IL) assisted precipitation method. The higher concentration of [Bmim][TfO] IL in the reaction medium leads to the formation of homogeneous nanoworms. The effect of synthesis temperature and the oxidizing agent (H{sub 2}O{sub 2}) on the Co{sub 3}O{sub 4} particle's morphology and their magnetic properties are discussed. Thermogravimetric analysis (TGA), powder X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), field emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM) analysis were used to characterize the Co{sub 3}O{sub 4} monodispersed nanoworms. The magnetic property of the spinel Co{sub 3}O{sub 4} nanoworms is highly dependent on crystalline domains and exhibits weak ferromagnetic behavior with a narrow hysteresis loop opening.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Chemical and Electrochemical Characterization of Hot–Pressed Li 6 PS 5 Cl Solid State Electrolyte: Operating Pressure–Invariant High Ionic Conductivity

Sulfide solid state electrolytes (SSE) are among the most promising materials in the effort to replace liquid electrolytes, largely due to their comparable ionic conductivities. Among the sulfide SSEs, Argyrodites (Li 6 PS 5 X, X=Cl, Br, I) further stand out due to their high theoretical ionic conductivity (~1×10 –2 S cm –1 ) and interfacial stability against reactive metal anodes such as lithium. Generally, solid state electrolyte pellets are pressed from powder feedstock at room temperature, however, pellets fabricated by cold pressing consistently result in low bulk density and high porosity, facilitating interfacial degradation reactions and allowing dendrites to propagate through the pores and grain boundaries. Here, we demonstrate the mechanical and electrochemical implications of hot-pressing standalone LPSCl SSE pellets with near-theoretical ionic conductivity, superior cycling performance, and enhanced mechanical stability. X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), and x-ray diffraction spectroscopy (XRD) analysis reveal no chemical changes to the Argyrodite surface after hot pressing up to 250°C. Furthermore, we use electrochemical impedance spectroscopy (EIS) to understand mechanical stability of Argyrodite SSE pellets as a function of externally applied pressure, demonstrating for the first time pressed standalone Argyrodite pellets with near-theoretical conductivities at external pressures below 14 MPa.

25 ENERGY STORAGE↗
DOE OSTI2021

Isolation of a Cyclopentasilane from Magnesium Reduction of a Linear Hexasilane

The reductive cyclization of two linear hexasilanes is contrasted, where a methylated precursor yielded a cyclohexasilane while the tert-butyl-functionalized analog unexpectedly yielded a cyclopentasilane. A comprehensive analysis using X-ray diffraction, IR, HR, HRMS, and multinuclear (1H, 13C and 29Si) 1D and 2D NMR spectroscopy identified the 1,2-dihydrodisilane tBuPhHSi–SiHPhtBu as an additional product, which was interpreted as supportive of a mechanism involving silylene elimination. Here, the results of this study may prove informative about substituent effects in the practice of complex organosilicon molecular synthesis.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2024

Structural Distortions and Short‐Range Magnetism in a Honeycomb Iridate Cu 3 ZnIr 2 O 6

Layered honeycomb iridates receive significant attention in the materials chemistry and physics fields due to the relevance of their crystal structures to the Kitaev model of a quantum spin liquid (QSL). In quest of liquid‐like magnetic ground state signatures, first‐generation alkali metal iridates A 2 IrO 3 ≡ A 3 [AIr 2 ]O 6 (A = Li, Na) and second‐generation iridates T 3 [AIr 2 ]O 6 ( T = Cu, Ag, H) are developed. T 3 [AIr 2 ]O 6 is synthesized from A 3 [AIr 2 ]O 6 via metathesis reactions replacing alkali ions located between honeycomb layers. Herein, the next level of chemical and structural complexity is introduced by synthesizing the honeycomb iridate, Cu 3 ZnIr 2 O 6 , in which alkali ions between and within the honeycomb layers are both selectively exchanged with two different transition metals. Analysis of powder X‐Ray diffraction data reveals corrugation of the honeycomb layers in Cu 3 ZnIr 2 O 6 that hinders complete magnetic frustration and results in a spin glass behavior observed from magnetization and specific heat data. Thus, Cu 3 ZnIr 2 O 6 represents yet another model, which broadens understanding of intricate relationships between intralayer distortions and magnetism of prospective Kitaev QSL compounds.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Effect of Rare Earth Ionic Radii on Structural, Electric, Magnetic and Thermoelectric Properties of REMnO{sub 3} (RE = Dy, Gd, Eu and Sm) Manganites

In this communication, we present a systematic investigation on structural, electric, magnetic and thermoelectric power properties of REMnO{sub 3} (RE = Dy, Gd, Eu and Sm) manganites which were prepared using solid-state reaction route. The samples exhibit orthorhombic crystal structure with Pbnm space group. Rietveld analysis of x-ray diffraction (XRD) data shows that the unit cell volume increases with increase in ionic radii of the rare earth ion, r{sub RE}. The particle size was calculated from the scanning electron microscope (SEM) images. The estimated particle size is observed to decrease with increasing ionic radii of the rare earth ions. All samples exhibit insulating behaviour and display immeasurably high resistivity at low temperatures. Magnetization studies indicate that the samples display a transition in the low temperature region. Magnetization data also reveals that antiferromagnetic behaviour is observed for all samples. Thermoelectric power results show that large thermoelectric power is seen for these manganites. Thermoelectric power of high-temperature region was successfully analysed using small polaron hopping (SPH) model.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗