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 1,063 records · Page 59
All sourcesNASA NTRSDOE OSTI
DOE OSTI2015

Effect of thermal annealing on structure and optical band gap of Se{sub 66}Te{sub 25}In{sub 9} thin films

Thin films of a-Se{sub 66}Te{sub 25}In{sub 9} have been deposited onto a chemically cleaned glass substrate by thermal evaporation technique under vacuum. Glassy nature of the films has been ascertained by X-ray diffraction pattern. The analysis of absorption spectra, measured at normal incidence, in the spectral range 400-1100 nm has been used for the optical characterization of thin films under investigation. The effect of thermal annealing on structure and optical band gap (E{sub g}) of a-Se{sub 66}Te{sub 25}In{sub 9} have been studied.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2016

Biogenic synthesized nanoparticles and their applications

In the present scenario, there are growing concerns over the potential impacts of bioengineered nanoparticles in the health sector. However, our understanding of how bioengineered nanoparticles may affect organisms within natural ecosystems, lags far behind our rapidly increasing ability to engineer novel nanoparticles. To date, research on the biological impacts of bioengineered nanoparticles has primarily consisted of controlled lab studies of model organisms with single species in culture media. Here, we described a cost effective and environment friendly technique for green synthesis of silver nanoparticles. Silver nanoparticles were successfully synthesized from 1 mM AgNO{sub 3} via a green synthesis process using leaf extract as reducing as well as capping agent. Nanoparticles were characterized with the help of UV–vis absorption spectroscopy, X-ray diffraction and TEM analysis which revealed the size of nanoparticles of 30-40 nm size. Further the nanoparticles synthesized by green route are found highly toxic against pathogenic bacteria and plant pathogenic fungi viz. Escherichia coli, Pseudomonas syringae and Sclerotiniasclerotiorum. The most important outcome of this work will be the development of value-added products and protection of human health from pathogens viz., bacteria, virus, fungi etc.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2013

Fabrication of nano Delafossite LiCo{sub 0.5}Fe{sub 0.5}O{sub 2} as the new adsorbent in efficient removal of reactive blue 5 from aqueous solutions

Highlights: ► Fabrication of nano Delafossite LiCo{sub 0.5}Fe{sub 0.5}O{sub 2} by sol–gel method. ► Kinetic study of the adsorption properties. ► Removal of reactive blue 5 (RB5) as a reactive dye by the prepared new nanocatalyst. - Abstract: In this paper, nanoparticles of delafossite-type LiCo{sub 0.5}Fe{sub 0.5}O{sub 2} were prepared by sol–gel method in the presence of maleic acid as a chelating agent. The nanoparticles were characterized using differential thermal analysis, X-ray powder diffraction, Fourier infrared spectroscopy, transmission electron microscope, scanning electron microscopy and scanning tunneling microscopy. The nanoparticles showed the excellent adsorption properties towards reactive dye, reactive blue 5 (RB5). The adsorption studies were carried out at different pH values, various adsorbent dosages and contact time in a batch experiments. The kinetic studies indicate that the removal process obeys the second-order kinetic equation. Also, the isotherm evaluations reveal that the adsorption of RB5 by the nanoparticles follows the Freundlich model.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Analyzing the scale of the bainitic ferrite plates by XRD, SEM and TEM

Since the major strengthening mechanisms in nanocrystalline bainitic steels arise from the exceptionally small size of the bainitc ferrite plate, accurate determination of this parameter is fundamental for quantitative relating the microstructure to the mechanical properties. In this work, the thickness of the bainitic ferrite subunits obtained by different bainitic heat treatments was determined in two steels, with carbon contents of 0.3 and 0.7 wt.%, from SEM and TEM micrographs. As these measurements were made on 2D images taken from random sections, the method includes some stereological correction factors to obtain accurate information. Finally, the determined thicknesses of bainitic ferrite plates were compared with the crystallite size calculated from the analysis of X-ray diffraction peak broadening. Although in some case the values obtained for crystallite size and plate thickness can be similar, this study confirms that indeed they are two different parameters. - Highlights: •Bainitic microstructure in a nanostructured and sub-micron steel •Bainitic ferrite plate thickness measured by SEM and TEM •Crystallite size determined by X-ray analysis.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Diffused phase transitions in Pb(Zr{sub 0.65}Ti{sub 0.35})O{sub 3}-Pb(Fe{sub 2/3}W{sub 1/3})O{sub 3} multiferroics

The solid solutions of (1−x)Pb(Zr{sub 0.65}Ti{sub 0.35})O{sub 3}-xPb(Fe{sub 2/3}W{sub 1/3})O{sub 3} in different ratios were fabricated by a high-temperature solid-state reaction method using high-purity oxides for possible multi-ferroic applications. Structural analysis using x-ray diffraction powder patterns of the system by Rietveld refinement method exhibits the formation of rhombohedral phase with R3c space group. Detailed studies of dielectric permittivity as a function of temperature of the systems show that the frequency independent dielectric maximum temperature shifts toward room temperature on increasing x. In addition to this, the degree of diffuseness of the permittivity anomaly is more pronounced for higher content of Pb(Fe{sub 2/3}W{sub 1/3})O{sub 3}, implying the existence of a composition-induced diffuse phase transition for the limited range of compositional ratios. Detailed impedance spectroscopy analysis shows the contributions of grain, grain boundary, and interfacial polarizations in the resistive characteristics and conduction mechanism of the materials. The weak ferromagnetic and saturated ferroelectric loops indicate that system with x = 0.1, 0.2 have good multiferroic characteristics, and may be useful for future spintronic devices.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2019

Quantitative Analysis of Micro-structural Changes in a Bituminous Coal After Exposure to Supercritical CO{sub 2} and Water

High-volatile bituminous coal samples were reacted in deionized water with supercritical CO{sub 2} (ScCO{sub 2}–water) under simulated in situ pressure and temperature conditions (8 MPa and 40 °C) in unconfined stress state for 14 days, in order to characterize potential CO{sub 2}–water–coal reactions. Micro-structural changes were identified pre- and post-experiment using X-ray powder diffraction (XRD) analysis for powdered coal (mineralogical changes), optical microscopy and scanning electron microscopy (SEM) for polished thin sections (surface feature changes) and micro-CT scanning for a small core (porosity and permeability changes). XRD analysis revealed that carbonic acid leaches out mineral matters in coal, including carbonates (calcite) and silicate minerals (albite, illite and kaolinite). Optical microscopy, SEM and CT images confirmed that the interaction of coal with ScCO{sub 2}–water causes an abundance of micro-cracks to open or propagate in unconfined coal samples. Most micro-cracks preferably propagated along maceral–mineral and maceral–maceral interfaces, which demonstrates that the micro-cracking was caused by differential swelling of different coal lithotypes. Wormhole formation was observed in coal caused by mineral dissolution and hydrocarbon mobilization, which significantly increases coal porosity compared with swelling-induced cracking. 3-D pore network models extracted from CT images show that ScCO{sub 2}–water treatment enlarges the pore and throat size, increases the numbers of pores and throats and improves pore network connectivity. Overall, CO{sub 2}–water–coal interactions under unconfined conditions enhance coal porosity, connectivity and permeability, which can be attributed to the combined effect of micro-cracking, mineral dissolution and hydrocarbon mobilization.

58 GEOSCIENCES↗
DOE OSTI2014

Local atomic structure of K{sub x}Na{sub (1−x)}NbO{sub 3} by total x-ray diffraction

Local atomic structure of K{sub x}Na{sub (1−x)}NbO{sub 3} with 0.0 ≤ x ≤ 1.0 was studied using atomic Pair Distribution Function analysis based on x-ray diffraction. Powdered crystals were found to exhibit a re-entrant behavior by being orthorhombic (Amm2) for x < 0.42, monoclinic (Pm) for 0.42 ≤ x ≤ 0.63 and again orthorhombic (Amm2) for x > 0.63. Non-centrosymmetric structure of NaNbO{sub 3} (Amm2) was also evident in the piezoresponse force microscopy analysis revealing the presence of the ferroelectric domains and switching behavior. Lowering of the crystallographic symmetry for 0.42 ≤ x ≤ 0.63 is discussed in terms of differences in the sizes of Na{sup +} and K{sup +} ions and Na–O and K–O bond lengths. Besides being a bridging phase, as suggested by the previous studies on lead-based compositions, present study suggests that lower symmetry monoclinic phase of compositionally disordered perovskite solid solutions could also be a manifestation of the difference in the sizes of constituent ions and bond lengths.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2016

Green synthesis of ZnO nanoparticles via complex formation by using Curcuma longa extract

Synthesis of ZnO nanoparticles(NPs) were conducted via Zn(II) complex formation by using Curcuma longa extract as template. Curcuma longa extract has the ability to form zinc ions complex with curcumin as ligating agent. Study on synthesis was conducted by monitoring thermal degradation of the material. Successful formation of zinc oxide nanoparticles was confirmed by employing x-ray diffraction, surface area analysis and transmission electron microscopy(TEM) studies. From the XRD analysis it is denoted that ZnO in hexagonal wurtzite phase was formed and particle size was varied as varied temperature. The data are also confirmed by TEM analysis which shows the particle sie at the range 20-80nm. The NPs exhibited excelent photocatalytic activity for methylene blue degradation and also significant antibacterial activity for Eschericia coli. The activity in methylene blue degradation was also confirmed from fast chemical oxygen demand (COD) reduction.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2018

Reducibility of PbO in Lead Silicate Glasses

X-ray diffraction data and X-ray fluorescence analysis data for microchannel plates are presented. From X-ray diffraction patterns, one can estimate the amount of reduced lead in microchannel plates and make sure of the presence of both metallic lead and semiconducting PbO{sub x} with a variable oxygen content.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2022

Radiation-induced Alteration of Meta-chert

Concrete aggregate identified as “meta-chert” was irradiated with gamma-rays and neutrons. To identify the volume expansion of the aggregate under neutron irradiation, herein the following analyses were performed for pristine and irradiated α-quartz and meta-chert: X-ray diffraction (XRD)/Rietveld analysis, dimension change, water pycnometry, He-pycnometry, light optical microscopy (LOM), and scanning electron microscopy (SEM). From the difference of volume expansion observed from dimension change and water / helium pycnometry, the crack opening inside the aggregate subjected to irradiation was elucidated, and this was confirmed by LOM and SEM analysis. The crack contribution to the expansion of the aggregate was significant for neutron fluence > 6.99 × 1019 n/cm 2 , for E ≥ 0.01 MeV. Based on the XRD analysis, changes in lattice parameters were identified and the cell volume expansion was compared with the data by helium pycnometry. Based on the density change calculation and phase calculation data, the density of X-ray amorphous phase was consistent with that of expanded crystal α-quartz.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Obtaining aluminas from the thermal decomposition of their different precursors: An {sup 27}Al MAS NMR and X-ray powder diffraction studies

Graphical abstract: - Highlights: • We synthesized three precursors of alumina from different methods. • The calcination of the precursors generated several alumina polymorphs. • XRD and NMR were used for structural investigation of the polymorphs. • The synthesis route determines the structural and textural properties of the solids. - Abstract: A commercial sample of Boehmite was used as precursor of alumina polymorphs. For comparison, three other precursors were synthesized from different methods. Particularly, the use of excess of urea promoted a very crystalline form of basic aluminum carbonate. The characteristics of the four precursors were investigated by thermal, vibrational and X-ray powder diffraction (XRD) analysis. Additionally, the nuclear magnetic resonance, with magic angle spinning ({sup 27}Al MAS NMR), was used to verify the coordination of aluminum cations. Each precursor was calcined at various temperatures generating alumina polymorphs, which were structurally analyzed by XRD and {sup 27}Al MAS NMR. Due to interest in catalysis supports, special attention was given to the γ-Al{sub 2}O{sub 3} phase, which in addition to structural investigation was subjected to textural analysis. The results showed that, from different synthesis procedures and common route of calcination, one can obtain materials with the same composition but with different structural and textural properties, which in turn can significantly influence the performance of a supported catalyst.

36 MATERIALS SCIENCE↗
DOE OSTI2016

The effect of acid treatment on the reactivity of natural zeolites used as supplementary cementitious materials

This work investigated the use of acid treatment as a method for increasing the reactivity of natural zeolite used as a supplementary cementitious material. The effects of treating a natural clinoptilolite zeolite with nine acid solutions, 0.1 M, 0.5 M, or 1 M hydrochloric or nitric acid or 0.1 M, 0.5 M, or 0.87 M acetic acid, were measured using x-ray diffraction, particle size analysis, pore size distribution and surface area analysis. The zeolite pozzolanic reactivity was determined by measuring the quantity of portlandite in hydrated zeolite-cement paste after 28 and 90 days. Results showed that acid treatment increased zeolite surface area, resulting in increased zeolite pozzolanic reactivity, independent of the solution concentration used. Cement hydration was also increased, evidenced by greater rates of heat evolution from cement-zeolite pastes. Additionally, although reductions of portlandite occurred most quickly in pastes with zeolites treated with strong acids, by 90 days the zeolites treated with acetic acid solutions showed comparable portlandite reductions.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Phosphate-passivated mordenite for tandem-catalytic conversion of syngas to ethanol or acetic acid

Selective and stable production of C 2 oxygenates from syngas is enabled by a phosphate-passivated mordenite catalyst used in tandem with a commercial Cu/ZnO/AlMgO x catalyst. Unmodified mordenite used in this arrangement is accompanied by substantial hydrocarbon formation and carbon deposition. Therefore, phosphate groups are used to remove or significantly reduce Brønsted acidity in mordenite by capping aluminum sites. Such groups are stable to calcination and catalyst regeneration. Here, trimethylphosphite is used as a phosphate precursor because it is able to enter the 12 membered-ring pores of mordenite where hydrocarbon formation occurs, but not enter the 8 membered-ring sidepockets, where methanol carbonylation occurs selectively. The catalyst was characterized using X-ray fluorescence, X-ray diffraction, and thermal gravimetric analysis. Optionally, a third bed of Cu/ZnO/AlMgO x catalyst is able to hydrodeoxygenate acetic acid to ethanol. The C 2 oxygenate selectivity is over 96% and among the best reported in a single reactor with a syngas feed.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2016

Dielectric relaxation of alkyl chains in graphite oxide and n-alkylammonium halides

The dynamic of n-alkylammonium halides and n-alkylammonium cations (n = 12, 14, 16, 18) intercalated in graphite oxide (GO) have been investigated with complex impedance spectroscopy. X-ray diffraction, X-ray photoelectron spectroscopy, Fourier-transform infrared spectroscopy, elemental analysis and thermogravimetry served to characterize the materials. The intercalated alkylammonium cations distributes as monolayers (when n = 12, 14 or 16) or bilayers (when n = 18), with their long axis parallel to GO layers, and with cations of headgroups bonded ionically to C-O{sup -} groups of GO; backbones of the confined molecules remain free. All halides and intercalation compounds suffer dielectric loss at low temperature. Arrhenius plots of the thermal dependence of the loss peaks, which are asymmetric, produce apparent activation energies that rise with increasing n. Ngai’s correlated-state model helps to correct for effects of dipole-dipole interaction, leading to virtually identical values for actual activation energy of 110 meV ± 5%; the values are also almost the same as the barrier energy for internal rotation in the alkyl macromolecule. We conclude that the relaxation of the alkylammonium cations arises not from C{sub 3} reorientation of the CH{sub 3} at its headgroup, but from small-angle wobbling around its major axis, an intrinsic motion.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2018

Size-dependent structural phase transitions and their correlation with photoluminescence and optical absorption behavior of annealed Zn0.45Cd0.55S quantum dots

Highlights: • Thermal Induced Structural Phase transition in nanostructured Zn{sub 0.45}Cd{sub 0.55}S. • Low temperature structural phase transition from cubic to hexagonal structure. • Thermal annealing effect on FTIR and Raman Spectra. • Thermal annealing effect on optical absorption of Zn{sub 0.45}Cd{sub 0.55}S nanoparticles. • Excitation-wavelength dependent photoluminescence emission spectra. - Abstract: In this paper, we investigate the effect of thermally induced structural phase transitions on the photoluminescence (PL) and optical absorption behaviour of Zn{sub 0.45}Cd{sub 0.55}S nanoparticles (NPs). Analysis of X-ray diffraction (XRD) patterns and high-resolution electron microscope (HRTEM) images reveal that the as-synthesized sample possesses zinc-blende-type cubic structure. In addition, at annealing temperature (T{sub a}) 400 °C, the cubic structure transforms completely into the wurtzite-type hexagonal structure. Furthermore, the second phase transition of the as-synthesized sample has observed at 700 °C, where the cubic structure has transformed into mixed polycrystalline phases of hexagonal ZnO, cubic CdO, monoclinic CdSO{sub 3}, and orthorhombic ZnSO{sub 4} structures. These new phases have also confirmed from the analysis of Raman and FTIR spectra. Analysis of UV–visible optical absorption spectra demonstrates that Increasing T{sub a} results in the decrease of optical band gap due the improvement in crystallinity accompanied by the increase in the particle size. The PL emission bands at an excitation energy of 3.818 eV exhibit redshift and a decrease in the intensity with increasing T{sub a} up to 500 °C. Meanwhile, further increase in T{sub a} up to 700 °C results in the enhancement of green emission intensity. On the other hand, PL emission spectra at 3.354 eV and T{sub a} 700 °C, reveal a dramatic increase in the emission intensity nearly by one-order of magnitude with respect to its value of the as-synthesized sample. This behaviour is ascribed to the incorporation of oxygen-related defects via thermal annealing in air, which act as additive radiative centers. Also, we have interpreted the observed spectral blue shift of PL emission spectrum with increasing excitation energy.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2017

New Diphosphopentamolybdate K{sub 5}[HP{sub 2}Mo{sub 5}O{sub 23}] · 10H{sub 2}O: Synthesis, Structure, and Characterization

A new diphosphopentamolybdate(VI) K{sub 5}[HP{sub 2}Mo{sub 5}O{sub 23}] · 10H{sub 2}O has been prepared employing solution method and characterized by single crystal X-ray diffraction, energy dispersive analysis, infrared spectroscopy, thermal stability analysis, cyclic voltammetry analysis, and ultraviolet visible spectroscopy. The compound crystallizes in the orthorhombic sp. gr. Pcab: a = 15.9661(10) Å, b = 19.0832(10) Å, c = 20.0970(9) Å, V = 6123.27(10) Å3, Z = 8. The crystal structure contains the polyanion units [HP{sub 2}Mo{sub 5}O{sub 23}]{sup 5–} around the potassium cations and lattice water. The [HP{sub 2}Mo{sub 5}O{sub 23}]{sup 5–} subunits are connected together through K−O−Mo bridges and hydrogen bonds. The crystal shape morphology was simulated using the Bravais–Friedel–Donnay–Harker model.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Assessment of lead tellurite glass for immobilizing electrochemical salt wastes from used nuclear fuel reprocessing

This paper provides an overview of research evaluating the use of lead tellurite glass as a waste form for salt wastes from electrochemical reprocessing of used nuclear fuel. The efficacy of using lead tellurite glass to immobilize three different salt compositions was evaluated: a LiCl-Li2O oxide reduction salt containing fission products from oxide fuel, a LiCl-KCl eutectic salt containing fission products from metallic fuel, and SrCl2. Physical and chemical properties of glasses made with these salts were characterized with X-ray diffraction, bulk density measurements, differential thermal analysis, chemical durability tests, scanning and transmission electron microscopies, and energy-dispersive X-ray spectroscopy. These glasses were found to accommodate high salt concentrations and have high densities, but further development is needed to improve chemical durability. (C) 2017 Published by Elsevier B.V.

Riley, Brian J.↗
DOE OSTI2016

Synthesis and photoluminescence properties of LiSrPO{sub 4}:Eu{sup 2+} phosphor for solid state lighting

A novel method to prepare orthophosphate LiSrPO{sub 4}: Eu{sup 2+} phosphor for white light-emitting diodes (w-LEDs) is given in this paper. Phosphor was successfully synthesized by Pechini (citrate gel) method which is efficient than conventional high temperature solid state reaction. X-ray powder diffraction (XRD) analysis confirmed the single phase formation of LiSrPO{sub 4}:Eu{sup 2+} with monoclinic crystal structure. Luminescence results showed that the phosphor could be efficiently excited by near UV and exhibited bright blue emission at λ{sub em} = 420 nm corresponding to 5d– 4f transition of Eu{sup 2+}. The phosphor exhibits blue emission bands under 350 nm excitation. This mercury-free excitation is useful for solid state lighting and light-emitting diode (LED). Hence it could be useful for solid state lighting and light-emitting diode (LED) application.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗