Risk and benefit of diffraction in Energy Dispersive X-ray fluorescence mapping

NASA Astrophysics Data System (ADS)

Nikonow, Wilhelm; Rammlmair, Dieter

2016-11-01

Energy dispersive X-ray fluorescence mapping (μ-EDXRF) is a fast and non-destructive method for chemical quantification and therefore used in many scientific fields. The combination of spatial and chemical information is highly valuable for understanding geological processes. Problems occur with crystalline samples due to diffraction, which appears according to Bragg's law, depending on the energy of the X-ray beam, the incident angle and the crystal parameters. In the spectra these peaks can overlap with element peaks suggesting higher element concentrations. The aim of this study is to investigate the effect of diffraction, the possibility of diffraction removal and potential geoscientific applications for X-ray mapping. In this work the μ-EDXRF M4 Tornado from Bruker was operated with a Rh-tube and polychromatic beam with two SDD detectors mounted each at ± 90° to the tube. Due to the polychromatic beam the Bragg condition fits for several mineral lattice planes. Since diffraction depends on the angle, it is shown that a novel correction approach can be applied by measuring from two different angles and calculating the minimum spectrum of both detectors gaining a better limit of quantification for this method. Furthermore, it is possible to use the diffraction information for separation of differently oriented crystallites within a monomineralic aggregate and obtain parameters like particle size distribution for the sample, as it is done by thin section image analysis in cross-polarized light. Only with μ-EDXRF this can be made on larger samples without preparation of thin sections.

Microchemical Analysis Of Space Operation Debris

NASA Technical Reports Server (NTRS)

Cummings, Virginia J.; Kim, Hae Soo

1995-01-01

Report discusses techniques used in analyzing debris relative to space shuttle operations. Debris collected from space shuttle, expendable launch vehicles, payloads carried by space shuttle, and payloads carried by expendable launch vehicles. Optical microscopy, scanning electron microscopy with energy-dispersive spectrometry, analytical electron microscopy with wavelength-dispersive spectrometry, and X-ray diffraction chosen as techniques used in examining samples of debris.

Room Temperature Ferromagnetism of Fe Doped Indium Tin Oxide Based on Dispersed Fe3O4 Nanoparticles

NASA Astrophysics Data System (ADS)

Okada, Koichi; Kohiki, Shigemi; Nishi, Sachio; Shimooka, Hirokazu; Deguchi, Hiroyuki; Mitome, Masanori; Bando, Yoshio; Shishido, Toetsu

2007-09-01

Transmission electron microscopy revealed that Fe3O4 nanoparticles with diameter of ≈200 nm dispersed in Fe doped indium tin oxide (Fe@ITO) powders exhibiting co-occurrence of room temperature ferromagnetism and superparamagnetism. Although we observed no X-ray diffraction peak from Fe related compounds for Fe0.19@ITO (ITO: In1.9Sn0.1O3) powders, the powders showed both hysteresis loop in field dependent magnetization at 300 K and divergence of zero-field-cooled magnetization from field-cooled magnetization. Scanning transmission electron microscopy with energy dispersive X-ray spectroscopy demonstrated that the nanoparticle with diameter of ≈200 nm consists of Fe and oxygen. Transmission electron diffraction revealed that crystal structure of the nanoparticle is inverse spinel type Fe3O4. The Fe3O4 crystalline phase by electron diffraction is consistent with the saturation magnetization of 1.3 μB/Fe and magnetic anomaly at ≈110 K observed for the powders.

Dispersion fraction enhances cellular growth of carbon nanotube and aluminum oxide reinforced ultrahigh molecular weight polyethylene biocomposites.

PubMed

Patel, Anup Kumar; Balani, Kantesh

2015-01-01

Ultrahigh molecular weight polyethylene (UHMWPE) is widely used as bone-replacement material for articulating surfaces due to its excellent wear resistance and low coefficient of friction. But, the wear debris, generated during abrasion between mating surfaces, leads to aseptic loosening of implants. Thus, various reinforcing agents are generally utilized, which may alter the surface and biological properties of UHMWPE. In the current work, the cellular response of compression molded UHMWPE upon reinforcement of bioactive multiwalled carbon nanotubes (MWCNTs) and bioinert aluminum oxide (Al2O3) is investigated. The phase retention and stability were observed using X-ray diffraction, Raman spectroscopy and Fourier transform infrared (FTIR) spectroscopy. The reinforcement of MWCNTs and Al2O3 has shown to alter the wettability (from contact angle of ~88°±2° to ~118°±4°) and surface energy (from ~23.20 to ~17.75 mN/m) of composites with respect to UHMWPE, without eliciting any adverse effect on cytocompatibility for the L929 mouse fibroblast cell line. Interestingly, the cellular growth of the L929 mouse fibroblast cell line is observed to be dominated by the dispersion fraction of surface free energy (SFE). After 48 h of incubation period, a decrease in metabolic activity of MWCNT-Al2O3 reinforced composites is attributed to apatite formation that reduces the dispersion fraction of surface energy. The mineralized apatite during incubation was confirmed and quantified by energy dispersive spectroscopy and X-ray diffraction respectively. Thus, the dispersion fraction of surface free energy can be engineered to play an important role in achieving enhanced metabolic activity of the MWCNT-Al2O3 reinforced UHMWPE biopolymer composites. Copyright © 2014 Elsevier B.V. All rights reserved.

Misfit strain of oxygen precipitates in Czochralski silicon studied with energy-dispersive X-ray diffraction

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gröschel, A., E-mail: alexander.groeschel@fau.de; Will, J.; Bergmann, C.

Annealed Czochralski Silicon wafers containing SiO{sub x} precipitates have been studied by high energy X-ray diffraction in a defocused Laue setup using a laboratory tungsten tube. The energy dispersive evaluation of the diffracted Bragg intensity of the 220 reflection within the framework of the statistical dynamical theory yields the static Debye-Waller factor E of the crystal, which gives access to the strain induced by the SiO{sub x} precipitates. The results are correlated with precipitate densities and sizes determined from transmission electron microscopy measurements of equivalent wafers. This allows for the determination of the constrained linear misfit ε between precipitate andmore » crystal lattice. For samples with octahedral precipitates the values ranging from ε = 0.39 (+0.28/−0.12) to ε = 0.48 (+0.34/−0.16) indicate that self-interstitials emitted into the matrix during precipitate growth contribute to the lattice strain. In this case, the expected value calculated from literature values is ε = 0.26 ± 0.05. Further, the precise evaluation of Pendellösung oscillations in the diffracted Bragg intensity of as-grown wafers reveals a thermal Debye-Waller parameter for the 220 reflection B{sup 220}(293 K) of 0.5582 ± 0.0039 Å{sup 2} for a structure factor based on spherically symmetric scattering contributions.« less

Mercuric iodide detector systems for identifying substances by x-ray energy dispersive diffraction

DOE Office of Scientific and Technical Information (OSTI.GOV)

Iwanczyk, J.S.; Patt, B.E.; Wang, Y.J.

The use of mercuric iodide arrays for energy-dispersive x-ray diffraction (EDXRD) spectroscopy is now being investigated by the authors for inspection of specific crystalline powders in substances ranging from explosives to illicit drugs. Mercuric iodide has been identified as the leading candidate for replacing the Ge detectors previously employed in the development of this technique because HgI{sub 2} detectors: operate at or near room temperature; without the bulky apparatus associated with cryogenic cooling; and offer excellent spectroscopy performance with extremely high efficiency. Furthermore, they provide the practicality of constructing optimal array geometries necessary for these measurements. Proof of principle experimentsmore » have been performed using a single-HgI{sub 2} detector spectrometer. An energy resolution of 655 eV (FWHM) has been obtained for 60 keV gamma line from an {sup 241}Am source. The EDXRD signatures of various crystalline powdered compounds have been measured and the spectra obtained show the excellent potential of mercuric iodide for this application.« less

Analysis of energy dispersive x-ray diffraction profiles for material identification, imaging and system control

NASA Astrophysics Data System (ADS)

Cook, Emily Jane

2008-12-01

This thesis presents the analysis of low angle X-ray scatter measurements taken with an energy dispersive system for substance identification, imaging and system control. Diffraction measurements were made on illicit drugs, which have pseudo- crystalline structures and thus produce diffraction patterns comprising a se ries of sharp peaks. Though the diffraction profiles of each drug are visually characteristic, automated detection systems require a substance identification algorithm, and multivariate analysis was selected as suitable. The software was trained with measured diffraction data from 60 samples covering 7 illicit drugs and 5 common cutting agents, collected with a range of statistical qual ities and used to predict the content of 7 unknown samples. In all cases the constituents were identified correctly and the contents predicted to within 15%. Soft tissues exhibit broad peaks in their diffraction patterns. Diffraction data were collected from formalin fixed breast tissue samples and used to gen erate images. Maximum contrast between healthy and suspicious regions was achieved using momentum transfer windows 1.04-1.10 and 1.84-1.90 nm_1. The resulting images had an average contrast of 24.6% and 38.9% compared to the corresponding transmission X-ray images (18.3%). The data was used to simulate the feedback for an adaptive imaging system and the ratio of the aforementioned momentum transfer regions found to be an excellent pa rameter. Investigation into the effects of formalin fixation on human breast tissue and animal tissue equivalents indicated that fixation in standard 10% buffered formalin does not alter the diffraction profiles of tissue in the mo mentum transfer regions examined, though 100% unbuffered formalin affects the profile of porcine muscle tissue (a substitute for glandular and tumourous tissue), though fat is unaffected.

Optimised Combined Angular and Energy Dispersive Diffraction at the PSICHE Beam Line of the SOLEIL Synchrotron for Fast, High Q-range Structure Determination at High Pressure and Temperature.

NASA Astrophysics Data System (ADS)

King, A.; Guignot, N.; Boulard, E.; Deslandes, J. P.; Clark, A. N.; Morard, G.; Itié, J. P.

2017-12-01

Synchrotron diffraction is an ideal technique for investigating materials at high pressure and temperature, because the penetrating nature of high-energy X-rays allows measurements to be made inside pressure cells or sample environments. Wang et al. described the CAESAR acquisition strategy, in which energy and angular dispersive techniques are combined to produce an instrument particularly suitable for quantitative measurements from samples inside high-pressure apparati [1]. The PSICHE beam line of the SOLEIL Synchrotron is equipped with such a CAESAR system. Uniquely, this system allows energy dispersive diffraction spectra to be acquired at scattering angles between -5 and +30 degrees two theta, while maintaining a sphere of confusion at the measurement position in the order of 10 microns. The slits used to define the scattering angle act as Soller slits and select the diffracted volume, separating the sample from its environment. By developing an optimised acquisition strategy we are able to obtain data covering a very wide Q range (to 160nm-1 or more), while minimising the total acquisition time (one hour per complete acquisition). In addition, the 2D nature (angle and energy) of the acquired dataset enables the effective incident spectrum to be efficiently determined with no addition measurements, in order to normalise the acquired data. The resulting profile of scattered intensity as a function of Q is suitable for Fourier transform analysis of liquid or amorphous structures. PSICHE is a multi technique beam line, with a part of the beam time dedicated to parallel beam absorption and phase contrast radiography and tomography [2]. Examples will be given to show how these techniques can be combined with diffraction techniques to greatly enrich studies of materials at extreme conditions. [1] Wang, Y., Uchida, T., Von Dreele, R., Rivers, M. L., Nishiyama, N., Funakoshi, K., Nozawa, A., and Keneko, H., J. Appl. Crystallogr. 37, 947 (2004). [2] King, A., Guignot, N., Zerbino, P., Boulard, E., Desjardins, K., Bourdessoule, M., Leclerq, N., Le, S., Renaud, G., Cerato, M., Bornert, M., Lenoir, N., Delzon, S., Perrillat, J.-P., Legodec, Y., Itié, J.-P. Rev. Sci. Instrum. 87, 093704 (2016).

The relationship between coefficient of restitution and state of charge of zinc alkaline primary LR6 batteries [Bouncing alkaline batteries: A basic solution

DOE PAGES

Bhadra, S.; Hertzberg, B. J.; Croft, M.; ...

2015-03-13

The coefficient of restitution of alkaline batteries had been shown to increase as a function of depth of discharge. In this work, using non-destructive mechanical testing, the change in coefficient of restitution is compared to in situ energy-dispersive x-ray diffraction data to determine the cause of the macroscopic change in coefficient of restitution. The increase in coefficient of restitution correlates to the formation of a percolation pathway of ZnO within the anode of the cell, and that the coefficient of restitution saturates at a value of 0.63 ± .05 at 50% state if charge when the anode has densified intomore » porous ZnO solid. Of note is the sensitivity of coefficient of restitution to the amount of ZnO formation that rivals the sensitivity on in situ energy-dispersive x-ray diffraction spectroscopy.« less

Component analyses of urinary nanocrystallites of uric acid stone formers by combination of high-resolution transmission electron microscopy, fast Fourier transformation, energy dispersive X-ray spectroscopy, X-ray diffraction and Fourier transform infrared spectroscopy.

PubMed

Sun, Xin-Yuan; Xue, Jun-Fa; Xia, Zhi-Yue; Ouyang, Jian-Ming

2015-06-01

This study aimed to analyse the components of nanocrystallites in urines of patients with uric acid (UA) stones. X-ray diffraction (XRD), Fourier transform infrared spectroscopy, high-resolution transmission electron microscopy (HRTEM), fast Fourier transformation (FFT) of HRTEM, and energy dispersive X-ray spectroscopy (EDS) were performed to analyse the components of these nanocrystallites. XRD and FFT showed that the main component of urinary nanocrystallites was UA, which contains a small amount of calcium oxalate monohydrate and phosphates. EDS showed the characteristic absorption peaks of C, O, Ca and P. The formation of UA stones was closely related to a large number of UA nanocrystallites in urine. A combination of HRTEM, FFT, EDS and XRD analyses could be performed accurately to analyse the components of urinary nanocrystallites.

Structural analysis of aluminium substituted nickel ferrite nanoparticles

NASA Astrophysics Data System (ADS)

Singh, H. S.; Sangwa, Neha

2018-05-01

Aluminium substituted nickel ferrite nanoparticles were synthesized by High Energy Ball milling (HEBM) of the mixture of α-NiO, α-Al2O3 and α-Fe2O3 followed by annealing at 1000˚C. X-ray diffraction (XRD) and Energy dispersive spectroscopy analysis (EDS) characterization was done for Aluminium substituted nickel ferrite. The structural analysis reveals the formation of the single phase compound. The average grain size was estimated by X-ray diffraction technique ranges from 30 to 10 nm with the increasing concentration of Aluminium. EDS spectra conforms the homogeneous mixing and purity of ferrite.

Solid-solution CrCoCuFeNi high-entropy alloy thin films synthesized by sputter deposition

DOE PAGES

An, Zhinan; Jia, Haoling; Wu, Yueying; ...

2015-05-04

The concept of high configurational entropy requires that the high-entropy alloys (HEAs) yield single-phase solid solutions. However, phase separations are quite common in bulk HEAs. A five-element alloy, CrCoCuFeNi, was deposited via radio frequency magnetron sputtering and confirmed to be a single-phase solid solution through the high-energy synchrotron X-ray diffraction, energy-dispersive spectroscopy, wavelength-dispersive spectroscopy, and transmission electron microscopy. The formation of the solid-solution phase is presumed to be due to the high cooling rate of the sputter-deposition process.

Photometric study of single-shot energy-dispersive x-ray diffraction at a laser plasma facility

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hoidn, O. R.; Seidler, G. T., E-mail: seidler@uw.edu

The low repetition rates and possible shot-to-shot variations in laser-plasma studies place a high value on single-shot diagnostics. For example, white-beam scattering methods based on broadband backlighter x-ray sources are used to determine changes in the structure of laser-shocked crystalline materials by the evolution of coincidences of reciprocal lattice vectors and kinematically allowed momentum transfers. Here, we demonstrate that white-beam techniques can be extended to strongly disordered dense plasma and warm dense matter systems where reciprocal space is only weakly structured and spectroscopic detection is consequently needed to determine the static structure factor and thus, the ion-ion radial distribution function.more » Specifically, we report a photometric study of energy-dispersive x-ray diffraction (ED-XRD) for structural measurement of high energy density systems at large-scale laser facilities such as OMEGA and the National Ignition Facility. We find that structural information can be obtained in single-shot ED-XRD experiments using established backlighter and spectrometer technologies.« less

Enhanced thermoelectric figure-of-merit in Bi-Sb-Te nanocomposites with homogenously dispersed oxide ceramic ZrO2 nanoparticles

NASA Astrophysics Data System (ADS)

Madavali, B.; Kim, H. S.; Lee, K. H.; Hong, S. J.

2017-06-01

In this research, p-type BiSbTe/ZrO2 nanocomposite powders were fabricated by high-energy ball milling. Different weight percentages of ZrO2 (2, 4, and 6 wt. %) nanoparticles were incorporated into the bulk (BiSbTe) matrix by consolidation of as-synthesized nanocomposites (NCs) powder by spark plasma sintering at 673 K. The phase and existence of ZrO2 nano-inclusions was confirmed by X-ray diffraction and transmission electron microscopy-selected area electron diffraction analysis. The Seebeck coefficient of the BiSbTe/ZrO2 NCs was significantly improved (˜36% for 4 wt. % added NCs) by a decrease in the carrier concentration and energy filtering effect, whereas the thermal conductivity was much reduced via strong scattering of carriers/phonons. The peak thermoelectric figure-of-merit (1.34 ± 0.06) was obtained for BiSbTe into which 2 wt. % ZrO2 was dispersed, which was approximately 20% greater than that of the undispersed sample. The hardness of the nanocomposites was significantly improved (˜27%) due to grain-boundary hardening and a dispersion strengthening mechanism.

Illicit drug detection using energy dispersive x-ray diffraction

NASA Astrophysics Data System (ADS)

Cook, E. J.; Griffiths, J. A.; Koutalonis, M.; Gent, C.; Pani, S.; Horrocks, J. A.; George, L.; Hardwick, S.; Speller, R.

2009-05-01

Illicit drugs are imported into countries in myriad ways, including via the postal system and courier services. An automated system is required to detect drugs in parcels for which X-ray diffraction is a suitable technique as it is non-destructive, material specific and uses X-rays of sufficiently high energy to penetrate parcels containing a range of attenuating materials. A database has been constructed containing the measured powder diffraction profiles of several thousand materials likely to be found in parcels. These include drugs, cutting agents, packaging and other innocuous materials. A software model has been developed using these data to predict the diffraction profiles which would be obtained by X-ray diffraction systems with a range of suggested detector (high purity germanium, CZT and scintillation), source and collimation options. The aim of the model was to identify the most promising system geometries, which was done with the aid of multivariate analysis (MVA). The most promising systems were constructed and tested. The diffraction profiles of a range of materials have been measured and used to both validate the model and to identify the presence of drugs in sample packages.

Room temperature chemical synthesis of lead selenide thin films with preferred orientation

NASA Astrophysics Data System (ADS)

Kale, R. B.; Sartale, S. D.; Ganesan, V.; Lokhande, C. D.; Lin, Yi-Feng; Lu, Shih-Yuan

2006-11-01

Room temperature chemical synthesis of PbSe thin films was carried out from aqueous ammoniacal solution using Pb(CH3COO)2 as Pb2+ and Na2SeSO3 as Se2- ion sources. The films were characterized by a various techniques including, X-ray diffraction (XRD), energy dispersive X-ray analysis (EDAX), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high resolution transmission electron microscopy (HR-TEM), selected area electron diffraction (SAED), Fast Fourier transform (FFT) and UV-vis-NIR techniques. The study revealed that the PbSe thin film consists of preferentially oriented nanocubes with energy band gap of 0.5 eV.

Rapid crystallization of WS2 films assisted by a thin nickel layer: An in situ energy-dispersive X-ray diffraction study

NASA Astrophysics Data System (ADS)

Ellmer, K.; Seeger, S.; Mientus, R.

2006-08-01

By rapid thermal crystallization of an amorphous WS3+x film, deposited by reactive magnetron sputtering at temperatures below 150 °C, layer-type semiconducting tungsten disulfide films (WS2) were grown. The rapid crystallization was monitored in real-time by in situ energy-dispersive X-ray diffraction. The films crystallize very fast (>40 nm/s), provided that a thin nickel film acts as nucleation seeds. Experiments on different substrates and the onset of the crystallization only at a temperature between 600 and 700 °C points to the decisive role of seeds for the textured growth of WS2, most probably liquid NiSx drops. The rapidly crystallized WS2 films exhibit a pronounced (001) texture with the van der Waals planes oriented parallel to the surface, leading to photoactive layers with a high hole mobility of about 80 cm2/Vs making such films suitable as absorbers for thin film solar cells.

Reduction of aqueous Crvi using nanoscale zero-valent iron dispersed by high energy electron beam irradiation

NASA Astrophysics Data System (ADS)

Zhang, Jing; Zhang, Guilong; Wang, Min; Zheng, Kang; Cai, Dongqing; Wu, Zhengyan

2013-09-01

High energy electron beam (HEEB) irradiation was used to disperse nanoscale zero-valent iron (NZVI) for reduction of Crvi to Criii in aqueous solution. Pore size distribution, scanning electron microscopy and X-ray diffraction characterizations demonstrated that HEEB irradiation could effectively increase the dispersion of NZVI resulting in more active reduction sites of Crvi on NZVI. Batch reduction experiments indicated that the reductive capacity of HEEB irradiation-modified NZVI (IMNZVI) was significantly improved, as the reductive efficiency reached 99.79% under the optimal conditions (electron beam dose of 30 kGy at 10 MeV, pH 2.0 and 313 K) compared with that of raw NZVI (72.14%). Additionally, the NZVI was stable for at least two months after irradiation. The modification mechanism of NZVI by HEEB irradiation was investigated and the results indicated that charge and thermal effects might play key roles in dispersing the NZVI particles.

Dispersive effects from a comparison of electron and positron scattering from

DOE Office of Scientific and Technical Information (OSTI.GOV)

Paul Gueye; M. Bernheim; J. F. Danel

1998-05-01

Dispersive effects have been investigated by comparing elastic scattering of electrons and positrons from {sup 12}C at the Saclay Linear Accelerator. The results demonstrate that dispersive effects at energies of 262 MeV and 450 MeV are less than 2% below the first diffraction minimum [0.95 < q{sub eff} (fm{sup -1}) < 1.66] in agreement with the prediction of Friar and Rosen. At the position of this minimum (q{sub eff} = 1.84 fm{sup -1}), the deviation between the positron scattering cross section and the cross section derived from the electron results is -44% {+-} 30%.

Validation of molecular crystal structures from powder diffraction data with dispersion-corrected density functional theory (DFT-D).

PubMed

van de Streek, Jacco; Neumann, Marcus A

2014-12-01

In 2010 we energy-minimized 225 high-quality single-crystal (SX) structures with dispersion-corrected density functional theory (DFT-D) to establish a quantitative benchmark. For the current paper, 215 organic crystal structures determined from X-ray powder diffraction (XRPD) data and published in an IUCr journal were energy-minimized with DFT-D and compared to the SX benchmark. The on average slightly less accurate atomic coordinates of XRPD structures do lead to systematically higher root mean square Cartesian displacement (RMSCD) values upon energy minimization than for SX structures, but the RMSCD value is still a good indicator for the detection of structures that deserve a closer look. The upper RMSCD limit for a correct structure must be increased from 0.25 Å for SX structures to 0.35 Å for XRPD structures; the grey area must be extended from 0.30 to 0.40 Å. Based on the energy minimizations, three structures are re-refined to give more precise atomic coordinates. For six structures our calculations provide the missing positions for the H atoms, for five structures they provide corrected positions for some H atoms. Seven crystal structures showed a minor error for a non-H atom. For five structures the energy minimizations suggest a higher space-group symmetry. For the 225 SX structures, the only deviations observed upon energy minimization were three minor H-atom related issues. Preferred orientation is the most important cause of problems. A preferred-orientation correction is the only correction where the experimental data are modified to fit the model. We conclude that molecular crystal structures determined from powder diffraction data that are published in IUCr journals are of high quality, with less than 4% containing an error in a non-H atom.

Validation of molecular crystal structures from powder diffraction data with dispersion-corrected density functional theory (DFT-D)

PubMed Central

van de Streek, Jacco; Neumann, Marcus A.

2014-01-01

In 2010 we energy-minimized 225 high-quality single-crystal (SX) structures with dispersion-corrected density functional theory (DFT-D) to establish a quantitative benchmark. For the current paper, 215 organic crystal structures determined from X-ray powder diffraction (XRPD) data and published in an IUCr journal were energy-minimized with DFT-D and compared to the SX benchmark. The on average slightly less accurate atomic coordinates of XRPD structures do lead to systematically higher root mean square Cartesian displacement (RMSCD) values upon energy minimization than for SX structures, but the RMSCD value is still a good indicator for the detection of structures that deserve a closer look. The upper RMSCD limit for a correct structure must be increased from 0.25 Å for SX structures to 0.35 Å for XRPD structures; the grey area must be extended from 0.30 to 0.40 Å. Based on the energy minimizations, three structures are re-refined to give more precise atomic coordinates. For six structures our calculations provide the missing positions for the H atoms, for five structures they provide corrected positions for some H atoms. Seven crystal structures showed a minor error for a non-H atom. For five structures the energy minimizations suggest a higher space-group symmetry. For the 225 SX structures, the only deviations observed upon energy minimization were three minor H-atom related issues. Preferred orientation is the most important cause of problems. A preferred-orientation correction is the only correction where the experimental data are modified to fit the model. We conclude that molecular crystal structures determined from powder diffraction data that are published in IUCr journals are of high quality, with less than 4% containing an error in a non-H atom. PMID:25449625

Growth of single crystalline delafossite LaCuO2 by the travelling-solvent floating zone method

NASA Astrophysics Data System (ADS)

Mohan, A.; Büchner, B.; Wurmehl, S.; Hess, C.

2014-09-01

Single crystals of LaCuO2 have been grown for the first time using the travelling-solvent floating zone method. The crystal was grown in an Ar-atmosphere by reduction of La2Cu2O5, which was used as the feed rod composition for the growth. The grown crystal has been characterized with regard to phase purity and single crystallinity using powder X-ray diffraction, energy dispersive X-ray analysis, Laue diffraction and scanning electron microscopy.

Elucidating the Wavelength Dependence of Phonon Scattering in Nanoparticle-Matrix Composites using Phonon Spectroscopy

DTIC Science & Technology

2016-07-11

composites with x - ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), Rutherford backscattering spectroscopy...RBS), particle-induced x - ray emission (PIXE), and energy dispersive x - ray spectroscopy (EDX). This work complements earlier works on CdSe...sample shows only In2Se3 and CdIn2Se4 XRD peaks (Figure 1.4e), it is stoichiometrically   Figure 1.4. X - ray diffraction patterns of (a) γ-In2Se3

Synthesis and characterization of nanocrystalline graphite from coconut shell with heating process

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wachid, Frischa M., E-mail: frischamw@yahoo.com, E-mail: adhiyudhaperkasa@yahoo.com, E-mail: afandisar@yahoo.com, E-mail: nurulrosyidah92@gmail.com, E-mail: darminto@physics.its.ac.id; Perkasa, Adhi Y., E-mail: frischamw@yahoo.com, E-mail: adhiyudhaperkasa@yahoo.com, E-mail: afandisar@yahoo.com, E-mail: nurulrosyidah92@gmail.com, E-mail: darminto@physics.its.ac.id; Prasetya, Fandi A., E-mail: frischamw@yahoo.com, E-mail: adhiyudhaperkasa@yahoo.com, E-mail: afandisar@yahoo.com, E-mail: nurulrosyidah92@gmail.com, E-mail: darminto@physics.its.ac.id

Graphite were synthesized and characterized by heating process of coconut shell with varying temperature (400, 800 and 1000°C) and holding time (3 and 5 hours). After heating process, the samples were characterized by X-ray diffraction (XRD) and analyzed by X'pert HighScore Plus Software, Scanning Electron Microcope-Energy Dispersive X-Ray (SEM-EDX) and Transmission Electron Microscope-Energy Dispersive X-Ray (TEM-EDX). Graphite and londsdaelite phase were analyzed by XRD. According to EDX analysis, the sample was heated in 1000°C got the highest content of carbon. The amorphous carbon and nanocrystalline graphite were observed by SEM-EDX and TEM-EDX.

Ellipsometry study of optical parameters of AgIn5S8 crystals

NASA Astrophysics Data System (ADS)

Isik, Mehmet; Gasanly, Nizami

2015-12-01

AgIn5S8 crystals grown by Bridgman method were characterized for optical properties by ellipsometry measurements. Spectral dependence of optical parameters; real and imaginary parts of the pseudodielectric function, pseudorefractive index, pseudoextinction coefficient, reflectivity and absorption coefficient were obtained from ellipsometry experiments carried out in the 1.2-6.2 eV range. Direct band gap energy of 1.84 eV was found from the analysis of absorption coefficient vs. photon energy. The oscillator energy, dispersion energy and zero-frequency refractive index, high-frequency dielectric constant values were found from the analysis of the experimental data using Wemple-DiDomenico and Spitzer-Fan models. Crystal structure and atomic composition ratio of the constituent elements in the AgIn5S8 crystal were revealed from structural characterization techniques of X-ray diffraction and energy dispersive spectroscopy.

Abinitio powder x-ray diffraction and PIXEL energy calculations on thiophene derived 1,4 dihydropyridine

DOE Office of Scientific and Technical Information (OSTI.GOV)

Karthikeyan, N., E-mail: karthin10@gmail.com; Sivakumar, K.; Pachamuthu, M. P.

We focus on the application of powder diffraction data to get abinitio crystal structure determination of thiophene derived 1,4 DHP prepared by cyclocondensation method using solid catalyst. Crystal structure of the compound has been solved by direct-space approach on Monte Carlo search in parallel tempering mode using FOX program. Initial atomic coordinates were derived using Gaussian 09W quantum chemistry software in semi-empirical approach and Rietveld refinement was carried out using GSAS program. The crystal structure of the compound is stabilized by one N-H…O and three C-H…O hydrogen bonds. PIXEL lattice energy calculation was carried out to understand the physical naturemore » of intermolecular interactions in the crystal packing, on which the total lattice energy is contributed into Columbic, polarization, dispersion, and repulsion energies.« less

Infrastructure development for radioactive materials at the NSLS-II

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sprouster, D. J.; Weidner, R.; Ghose, S. K.

2018-02-01

The X-ray Powder Diffraction (XPD) Beamline at the National Synchrotron Light Source-II is a multipurpose instrument designed for high-resolution, high-energy X-ray scattering techniques. In this article, the capabilities, opportunities and recent developments in the characterization of radioactive materials at XPD are described. The overarching goal of this work is to provide researchers access to advanced synchrotron techniques suited to the structural characterization of materials for advanced nuclear energy systems. XPD is a new beamline providing high photon flux for X-ray Diffraction, Pair Distribution Function analysis and Small Angle X-ray Scattering. The infrastructure and software described here extend the existing capabilitiesmore » at XPD to accommodate radioactive materials. Such techniques will contribute crucial information to the characterization and quantification of advanced materials for nuclear energy applications. We describe the automated radioactive sample collection capabilities and recent X-ray Diffraction and Small Angle X-ray Scattering results from neutron irradiated reactor pressure vessel steels and oxide dispersion strengthened steels.« less

Infrastructure development for radioactive materials at the NSLS-II

DOE PAGES

Sprouster, David J.; Weidner, R.; Ghose, S. K.; ...

2017-11-04

The X-ray Powder Diffraction (XPD) Beamline at the National Synchrotron Light Source-II is a multipurpose instrument designed for high-resolution, high-energy X-ray scattering techniques. In this paper, the capabilities, opportunities and recent developments in the characterization of radioactive materials at XPD are described. The overarching goal of this work is to provide researchers access to advanced synchrotron techniques suited to the structural characterization of materials for advanced nuclear energy systems. XPD is a new beamline providing high photon flux for X-ray Diffraction, Pair Distribution Function analysis and Small Angle X-ray Scattering. The infrastructure and software described here extend the existing capabilitiesmore » at XPD to accommodate radioactive materials. Such techniques will contribute crucial information to the characterization and quantification of advanced materials for nuclear energy applications. Finally, we describe the automated radioactive sample collection capabilities and recent X-ray Diffraction and Small Angle X-ray Scattering results from neutron irradiated reactor pressure vessel steels and oxide dispersion strengthened steels.« less

Recent advance to 3 × 10(-5) rad near diffraction-limited beam divergence of dye laser with transverse-discharge flash-lamp pumping.

PubMed

Trusov, K K

1994-02-20

A new experimental setup of a Rhodamine 6G dye laser with a transverse-discharge flash-lamp-pumping system is presented. It differs from a previous setup [Sov. J. Quantum Electron. 16, 468-471 (1989)] in that it has a larger laser beam aperture (32 mm) and higher pumping energy (1 kJ), which made it possible to test the scalability and reach near diffraction-limited laser beam divergence of 3 × 10(-5) rad FWHM at beam energy 1.4 J. The effect of spectral dispersion in the active medium and of other optical elements on the beam divergence is also discussed.

Crystal Structure, Magnetic and Optical Properties of Mn-Doped BiFeO₃ by Hydrothermal Synthesis.

PubMed

Zhang, Ning; Wei, Qinhua; Qin, Laishun; Chen, Da; Chen, Zhi; Niu, Feng; Wang, Jiangying; Huanag, Yuexiang

2017-01-01

In this paper, Mn doped BiFeO₃ were firstly synthesized by hydrothermal process. The influence of Mn doping on structural, optical and magnetic properties of BiFeO₃ was studied. The different amounts of Mn doping in BiFeO₃ were characterized by X-ray diffraction, Scanning Electron Microscope, Energy Dispersive X-ray Spectroscope, UV-Vis diffuse reflectance spectroscopy and magnetic measurements. The X-ray diffraction (XRD) patterns confirmed the formation of pure phase rhombohedral structure in BiFe(1−x) Mn (x) O₃ (x = 0.01, 0.03, 0.05, 0.07) samples. The morphologies and chemical compositions of as-prepared samples could be observed by Scanning Electron Microscope (SEM) and Energy Dispersive X-ray Spectroscope (EDS). A relative large saturated magnetization (Ms) of 0.53 emu/g for x = 0.07 sample was obtained at room temperature, which is considered to be Mn ions doping. UV-Vis diffuse reflectance spectroscopy showed strong absorption of light in the range of 200–1000 nm, indicating the optical band gap in the visible region for these samples. This implied that BiFe(1−x) Mn(x)O₃ may be a potential photocatalyst for utilizing solar energy.

A furnace and environmental cell for the in situ investigation of molten salt electrolysis using high-energy X-ray diffraction.

PubMed

Styles, Mark J; Rowles, Matthew R; Madsen, Ian C; McGregor, Katherine; Urban, Andrew J; Snook, Graeme A; Scarlett, Nicola V Y; Riley, Daniel P

2012-01-01

This paper describes the design, construction and implementation of a relatively large controlled-atmosphere cell and furnace arrangement. The purpose of this equipment is to facilitate the in situ characterization of materials used in molten salt electrowinning cells, using high-energy X-ray scattering techniques such as synchrotron-based energy-dispersive X-ray diffraction. The applicability of this equipment is demonstrated by quantitative measurements of the phase composition of a model inert anode material, which were taken during an in situ study of an operational Fray-Farthing-Chen Cambridge electrowinning cell, featuring molten CaCl(2) as the electrolyte. The feasibility of adapting the cell design to investigate materials in other high-temperature environments is also discussed.

Hidden Gratings in Holographic Liquid Crystal Polymer-Dispersed Liquid Crystal Films.

PubMed

De Sio, Luciano; Lloyd, Pamela F; Tabiryan, Nelson V; Bunning, Timothy J

2018-04-18

Dynamic diffraction gratings that are hidden in the field-off state are fabricated utilizing a room-temperature photocurable liquid crystal (LC) monomer and nematic LC (NLC) using holographic photopolymerization techniques. These holographic LC polymer-dispersed LCs (HLCPDLCs) are hidden because of the refractive index matching between the LC polymer and the NLC regions in the as-formed state (no E-field applied). Application of a moderate E-field (5 V/μm) generates a refractive index mismatch because of the NLC reorientation (along the E-field) generating high-diffraction efficiency transmission gratings. These dynamic gratings are characterized by morphological, optical, and electrooptical techniques. They exhibit a morphology made of oriented LC polymer regions (containing residual NLC) alternating with a two-phase region of an NLC and LC polymer. Unlike classic holographic polymer-dispersed LC gratings formed with a nonmesogenic monomer, there is index matching between the as-formed alternating regions of the grating. These HLCPDLCs exhibit broad band and high diffraction efficiency (≈90%) at the Bragg angle, are transparent to white light across the visible range because of the refractive index matching, and exhibit fast response times (1 ms). The ability of HLCPDLCs not to consume electrical power in the off state opens new possibilities for the realization of energy-efficient switchable photonic devices.

Amorphous and liquid samples structure and density measurements at high pressure - high temperature using diffraction and imaging techniques

NASA Astrophysics Data System (ADS)

Guignot, N.; King, A.; Clark, A. N.; Perrillat, J. P.; Boulard, E.; Morard, G.; Deslandes, J. P.; Itié, J. P.; Ritter, X.; Sanchez-Valle, C.

2016-12-01

Determination of the density and structure of liquids such as iron alloys, silicates and carbonates is a key to understand deep Earth structure and dynamics. X-ray diffraction provided by large synchrotron facilities gives excellent results as long as the signal scattered from the sample can be isolated from its environment. Different techniques already exist; we present here the implementation and the first results given by the combined angle- and energy-dispersive structural analysis and refinement (CAESAR) technique introduced by Wang et al. in 2004, that has never been used in this context. It has several advantages in the study of liquids: 1/ the standard energy-dispersive technique (EDX), fast and compatible with large multi-anvil presses frames, is used for fast analysis free of signal pollution from the sample environment 2/ some limitations of the EDX technique (homogeneity of the sample, low resolution) are irrelevant in the case of liquid signals, others (wrong intensities, escape peaks artifacts, background subtraction) are solved by the CAESAR technique 3/ high Q data (up to 15 A-1 and more) can be obtained in a few hours (usually less than 2). We present here the facilities available on the PSICHE beamline (SOLEIL synchrotron, France) and a few results obtained using a Paris-Edinburgh (PE) press and a 1200 tons load capacity multi-anvil press with a (100) DIA compression module. X-ray microtomography, used in conjunction with a PE press featuring rotating anvils (RotoPEc, Philippe et al., 2013) is also very effective, by simply measuring the 3D volume of glass or liquid spheres at HPHT, thus providing density. This can be done in conjunction with the CAESAR technique and we illustrate this point. Finally, absorption profiles can be obtained via imaging techniques, providing another independent way to measure the density of these materials. References Y. Wang et al., A new technique for angle-dispersive powder diffraction using an energy-dispersive setup and synchrotron radiation (2004), J. Appl. Cryst. (2004). 37, 947-956 J. Philippe, Y. Le Godec, F. Bergame et M. Morand, Patent INPI 11 62335 (2013)

Zirconium and silver co-doped TiO2 nanoparticles as visible light catalyst for reduction of 4-nitrophenol, degradation of methyl orange and methylene blue

NASA Astrophysics Data System (ADS)

Naraginti, Saraschandra; Stephen, Finian Bernard; Radhakrishnan, Adhithya; Sivakumar, A.

2015-01-01

Catalytic activity of Zr and Ag co-doped TiO2 nanoparticles on the reduction of 4-nitrophenol, degradation of methylene blue and methyl orange was studied using sodium borohydride as reducing agent. The nanoparticles were characterized using X-ray diffraction, energy dispersive X-ray, high resolution transmission electron microscopy, selected area electron diffraction and UV-Vis spectroscopy. The rate of the reduction/degradation was found to increase with increasing amount of the photocatalyst which could be attributed to higher dispersity and small size of the nanoparticles. The catalytic activity of Zr and Ag co-doped TiO2 nanoparticles showed no significant difference even after recycling the catalyst four times indicating a promising potential for industrial application of the prepared photocatalyst.

Plasma in-liquid method for reduction of zinc oxide in zinc nanoparticle synthesis

NASA Astrophysics Data System (ADS)

Amaliyah, Novriany; Mukasa, Shinobu; Nomura, Shinfuku; Toyota, Hiromichi; Kitamae, Tomohide

2015-02-01

Metal air-batteries with high-energy density are expected to be increasingly applied in electric vehicles. This will require a method of recycling air batteries, and reduction of metal oxide by generating plasma in liquid has been proposed as a possible method. Microwave-induced plasma is generated in ethanol as a reducing agent in which zinc oxide is dispersed. Analysis by energy-dispersive x-ray spectrometry (EDS) and x-ray diffraction (XRD) reveals the reduction of zinc oxide. According to images by transmission electron microscopy (TEM), cubic and hexagonal metallic zinc particles are formed in sizes of 30 to 200 nm. Additionally, spherical fiber flocculates approximately 180 nm in diameter are present.

MgO-Al2O3-ZrO2 Amorphous Ternary Composite: A Dense and Stable Optical Coating

NASA Technical Reports Server (NTRS)

Shaoo, Naba K.; Shapiro, Alan P.

1998-01-01

The process-parameter-dependent optical and structural properties of MgO-Al2O3-ZrO2 ternary mixed-composite material were investigated. Optical properties were derived from spectrophotometric measurements. The surface morphology, grain size distributions, crystallographic phases, and process- dependent material composition of films were investigated through the use of atomic force microscopy, x-ray diffraction analysis, and energy-dispersive x-ray analysis. Energy-dispersive x-ray analysis made evident the correlation between the optical constants and the process-dependent compositions in the films. It is possible to achieve environmentally stable amorphous films with high packing density under certain optimized process conditions.

Reduction of aqueous CrVI using nanoscale zero-valent iron dispersed by high energy electron beam irradiation.

PubMed

Zhang, Jing; Zhang, Guilong; Wang, Min; Zheng, Kang; Cai, Dongqing; Wu, Zhengyan

2013-10-21

High energy electron beam (HEEB) irradiation was used to disperse nanoscale zero-valent iron (NZVI) for reduction of CrVI to CrIII in aqueous solution. Pore size distribution, scanning electron microscopy and X-ray diffraction characterizations demonstrated that HEEB irradiation could effectively increase the dispersion of NZVI resulting in more active reduction sites of Crvi on NZVI. Batch reduction experiments indicated that the reductive capacity of HEEB irradiation-modified NZVI (IMNZVI) was significantly improved, as the reductive efficiency reached 99.79% under the optimal conditions (electron beam dose of 30 kGy at 10 MeV, pH 2.0 and 313 K) compared with that of raw NZVI (72.14%). Additionally, the NZVI was stable for at least two months after irradiation. The modification mechanism of NZVI by HEEB irradiation was investigated and the results indicated that charge and thermal effects might play key roles in dispersing the NZVI particles.

HANFORD WASTE MINERALOGY REFERENCE REPORT

DOE Office of Scientific and Technical Information (OSTI.GOV)

DISSELKAMP RS

2010-06-29

This report lists the observed mineral phases present in the Hanford tanks. This task was accomplished by performing a review of numerous reports that used experimental techniques including, but not limited to: x-ray diffraction, polarized light microscopy, scanning electron microscopy, transmission electron microscopy, energy dispersive spectroscopy, electron energy loss spectroscopy, and particle size distribution analyses. This report contains tables that can be used as a quick reference to identify the crystal phases observed in Hanford waste.

HANFORD WASTE MINEROLOGY REFERENCE REPORT

DOE Office of Scientific and Technical Information (OSTI.GOV)

DISSELKAMP RS

2010-06-18

This report lists the observed mineral phase phases present in the Hanford tanks. This task was accomplished by performing a review of numerous reports using experimental techniques including, but not limited to: x-ray diffraction, polarized light microscopy, scanning electron microscopy, transmission electron microscopy, energy dispersive spectroscopy, electron energy loss spectroscopy, and particle size distribution analyses. This report contains tables that can be used as a quick reference to identify the crystal phases present observed in Hanford waste.

Crystal structure and density of helium to 232 kbar

NASA Technical Reports Server (NTRS)

Mao, H. K.; Wu, Y.; Jephcoat, A. P.; Hemley, R. J.; Bell, P. M.; Bassett, W. A.

1988-01-01

The properties of helium and hydrogen at high pressure are topics of great interest to the understanding of planetary interiors. These materials constitute 95 percent of the entire solar system. A technique was presented for the measurement of X-ray diffraction from single-crystals of low-Z condenses gases in a diamond-anvil cell at high pressure. The first such single-crystal X-ray diffraction measurements on solid hydrogen to 26.5 GPa were presented. The application of this technique to the problem of the crystal structure, equation of state, and phase diagram of solid helium is reported. Crucial for X-ray diffraction studies of these materials is the use of a synchrotron radiation source which provides high brillance, narrow collimation of the incident and diffracted X-ray beams to reduce the background noise, and energy-dispersive diffraction techniques with polychromatic (white) radiation, which provides high detection efficiency.

Single photon energy dispersive x-ray diffraction

DOE Office of Scientific and Technical Information (OSTI.GOV)

Higginbotham, Andrew; Patel, Shamim; Ciricosta, Orlando

2014-03-15

With the pressure range accessible to laser driven compression experiments on solid material rising rapidly, new challenges in the diagnosis of samples in harsh laser environments are emerging. When driving to TPa pressures (conditions highly relevant to planetary interiors), traditional x-ray diffraction techniques are plagued by increased sources of background and noise, as well as a potential reduction in signal. In this paper we present a new diffraction diagnostic designed to record x-ray diffraction in low signal-to-noise environments. By utilising single photon counting techniques we demonstrate the ability to record diffraction patterns on nanosecond timescales, and subsequently separate, photon-by-photon, signalmore » from background. In doing this, we mitigate many of the issues surrounding the use of high intensity lasers to drive samples to extremes of pressure, allowing for structural information to be obtained in a regime which is currently largely unexplored.« less

Hydrothermal synthesis of tungsten doped tin dioxide nanocrystals

NASA Astrophysics Data System (ADS)

Zhou, Cailong; Li, Yufeng; Chen, Yiwen; Lin, Jing

2018-01-01

Tungsten doped tin dioxide (WTO) nanocrystals were synthesized through a one-step hydrothermal method. The structure, composition and morphology of WTO nanocrystals were characterized by x-ray diffraction, x-ray photoelectron spectroscopy, energy dispersive x-ray spectroscopy, UV-vis diffuse reflectance spectra, zeta potential analysis and high-resolution transmission electron microscopy. Results show that the as-prepared WTO nanocrystals were rutile-type structure with the size near 13 nm. Compared with the undoped tin dioxide nanocrystals, the WTO nanocrystals possessed better dispersity in ethanol phase and formed transparent sol.

A von Hamos x-ray spectrometer based on a segmented-type diffraction crystal for single-shot x-ray emission spectroscopy and time-resolved resonant inelastic x-ray scattering studies

DOE Office of Scientific and Technical Information (OSTI.GOV)

Szlachetko, J.; Institute of Physics, Jan Kochanowski University, 25-406 Kielce; Nachtegaal, M.

2012-10-15

We report on the design and performance of a wavelength-dispersive type spectrometer based on the von Hamos geometry. The spectrometer is equipped with a segmented-type crystal for x-ray diffraction and provides an energy resolution in the order of 0.25 eV and 1 eV over an energy range of 8000 eV-9600 eV. The use of a segmented crystal results in a simple and straightforward crystal preparation that allows to preserve the spectrometer resolution and spectrometer efficiency. Application of the spectrometer for time-resolved resonant inelastic x-ray scattering and single-shot x-ray emission spectroscopy is demonstrated.

Phase transition studies of germanium to 1. 25 Mbar

DOE Office of Scientific and Technical Information (OSTI.GOV)

Vohra, Y.K.; Brister, K.E.; Desgreniers, S.

1986-05-05

New phase transitions in Ge were observed by energy-dispersive x-ray diffraction techniques for pressures up to 125 GPa (1.25 Mbar) as follows: the ..beta..-Sn structure to the simple hexagonal (sh) phase at 75 +- 3 GPa and to the double hexagonal close-packed structure (dhcp) at 102 +- 5 GPa. These are the highest pressures for which a crystalline structure change has been directly observed in any material by x-ray diffraction. Total-energy pseudopotential calculations predict 84 +- 10 GPa for the ..beta..-Sn to sh phase transition and 105 +- 21 GPa for sh to hcp (not dhcp) transition. The role ofmore » 3d core electrons in increasing the transformation pressures in Ge, as compared to Si, is emphasized.« less

Residual stress analysis of energy-dispersive diffraction data using a two-detector setup: Part I - Theoretical concept

NASA Astrophysics Data System (ADS)

Apel, Daniel; Meixner, Matthias; Liehr, Alexander; Klaus, Manuela; Degener, Sebastian; Wagener, Guido; Franz, Christian; Zinn, Wolfgang; Genzel, Christoph; Scholtes, Berthold

2018-01-01

A new goniometer setup for energy-dispersive X-ray diffraction is introduced which is based on simultaneous data acquisition with two detectors D1 and D2, both of them freely movable in a horizontal as well as in a vertical plane. From the multitude of measurement configurations that can be realised with this setup, we figured out three efficient concepts which aim at the fast analysis of residual stress depth profiles by combining the diffraction data gathered with the two detectors. The characteristic feature of the first two configurations consists in the vertical (horizontal) positioning of the first (second) detector, which results in a diffraction geometry where the two scattering vectors span a plane that coincides with the X-circle used for sample tilt. Because each detector does see the sample under another viewing angle, both the positive and the negative ψ-branch are covered by just one χ-tilt between 0°and 90°(configuration 1) and 0°and 60°(configuration 2), thus allowing for the simultaneous analysis of the in- and out-of-plane residual stress depth gradients σii(τ) and σi3(τ) (i = 1 , 2), respectively, from data sets dD1hkl(χ) and dD2hkl(χ). The third configuration introduced in this paper is based on a ϕ-rotation of the sample under a constant tilt angle χ and enables a fast and reliable tracing of shear stress fields σi3(τ) (i = 1, 2).

Characterization of the new neutron imaging and materials science facility IMAT

NASA Astrophysics Data System (ADS)

Minniti, Triestino; Watanabe, Kenichi; Burca, Genoveva; Pooley, Daniel E.; Kockelmann, Winfried

2018-04-01

IMAT is a new cold neutron imaging and diffraction instrument located at the second target station of the pulsed neutron spallation source ISIS, UK. A broad range of materials science and materials testing areas will be covered by IMAT. We present the characterization of the imaging part, including the energy-selective and energy-dispersive imaging options, and provide the basic parameters of the radiography and tomography instrument. In particular, detailed studies on mono and bi-dimensional neutron beam flux profiles, neutron flux as a function of the neutron wavelength, spatial and energy dependent neutron beam uniformities, guide artifacts, divergence and spatial resolution, and neutron pulse widths are provided. An accurate characterization of the neutron beam at the sample position, located 56 m from the source, is required to optimize collection of radiographic and tomographic data sets and for performing energy-dispersive neutron imaging via time-of-flight methods in particular.

Visible-light-assisted SLCs template synthesis of sea anemone-like Pd/PANI nanocomposites with high electrocatalytic activity for methane oxidation in acidic medium

NASA Astrophysics Data System (ADS)

Tan, De-Xin; Wang, Yan-Li

2018-03-01

Sea anemone-like palladium (Pd)/polyaniline (PANI) nanocomposites were synthesized via visible-light-assisted swollen liquid crystals (SLCs) template method. The resulting samples were characterized by transmission electron microscopy (TEM), selected area electron diffraction (SAED), energy dispersive spectrometer (EDS), x-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), ultraviolet-visible (UV–vis) absorption spectroscopy and Fourier transform infrared (FT-IR) spectroscopy, respectively. The electrocatalytic properties of Pd/PANI nanocomposites modified glass carbon electrode (GCE) for methane oxidation were investigated by cycle voltammetry (CV) and chronoamperometry. Those dispersed sea anemone-like Pd/PANI nanocomposites had an average diameter of 320 nm. The obtained Pd nanoparticles with an average diameter of about 45 nm were uniformly distributed in PANI matrix. Sea anemone-like Pd/PANI nanocomposites exhibited excellent electrocatalytic activity and stability for oxidation of methane (CH4).

Interfacial Reaction During High Energy Ball Milling Dispersion of Carbon Nanotubes into Ti6Al4V

NASA Astrophysics Data System (ADS)

Adegbenjo, A. O.; Olubambi, P. A.; Potgieter, J. H.; Nsiah-Baafi, E.; Shongwe, M. B.

2017-12-01

The unique thermal and mechanical properties of carbon nanotubes (CNTs) have made them choice reinforcements for metal matrix composites (MMCs). However, there still remains a critical challenge in achieving homogeneous dispersion of CNTs in metallic matrices. Although high energy ball milling (HEBM) has been reported as an effective method of dispersing CNTs into metal matrices, a careful selection of the milling parameters is important not to compromise the structural integrity of CNTs which may cause interfacial reactions with the matrix. In this study, multi-walled carbon nanotubes (MWCNTs) were purified by annealing in argon and vacuum atmospheres at 1000 and 1800 °C, respectively, for 5 h to remove possible metallic catalyst impurities. Subsequently, 1, 2 and 3 wt.% MWCNTs were dispersed by adapted HEBM into Ti6Al4V alloy metal matrix. Raman spectroscopy (RS), x-ray diffraction, scanning electron microscopy, energy-dispersive x-ray spectrometry and transmission electron microscopy techniques were used to characterize the as-received and annealed MWCNTs, as well as the admixed MWCNT/Ti6Al4V nanocomposite powders. The experimental results showed that vacuum annealing successfully eliminated retained nickel (Ni) catalysts from MWCNTs, while the adapted HEBM method achieved a relative homogeneous dispersion of MWCNTs into the Ti6Al4V matrix and helped to control interfacial reactions between defective MWCNTs and the metal matrix.

Crystallography and Morphology of Niobium Carbide in As-Cast HP-Niobium Reformer Tubes

NASA Astrophysics Data System (ADS)

Buchanan, Karl G.; Kral, Milo V.

2012-06-01

The microstructures of two as-cast heats of niobium-modified HP stainless steels were characterized. Particular attention was paid to the interdendritic niobium-rich carbides formed during solidification of these alloys. At low magnifications, these precipitates are grouped in colonies of similar lamellae. Higher magnifications revealed that the lamellae actually obtain two distinct morphologies. The type I morphology exhibits broad planar interfaces with a smooth platelike shape. Type II lamellae have undulating interfaces and an overall reticulated shape. To provide further insight into the origin of these two different morphologies, the microstructure and crystallography of each have been studied in detail using high resolution scanning electron microscopy, transmission electron microscopy, various electron diffraction methods (electron backscatter diffraction (EBSD), selected area diffraction (SAD), and convergent beam electron diffraction (CBED)), and energy dispersive X-ray spectroscopy.

Brominated carbon black: An EDXD study

DOE Office of Scientific and Technical Information (OSTI.GOV)

Carbone, Marilena; Gontrani, Lorenzo, E-mail: lorenzo.gontrani@uniroma1.it

2014-06-19

An energy dispersive X-Ray study of pure and brominated carbon black was carried out. The analysis of the diffraction patterns reveals that the low bromine load (ca.1% mol) is trapped into the structure, without significantly modifying it. This allows the application of the difference methods, widely tested for electrolyte solutions, inorganic matrices containing metals and isomorphic substitutions.

Naturally occurring vapor-liquid-solid (VLS) Whisker growth of germanium sulfide

USGS Publications Warehouse

Finkelman, R.B.; Larson, R.R.; Dwornik, E.J.

1974-01-01

The first naturally occurring terrestrial example of vapor-liquid-solid (VLS) growth has been observed in condensates from gases released by burning coal in culm banks. Scanning electron microscopy, X-ray diffraction, and energy dispersive analysis indicate that the crystals consist of elongated rods (??? 100 ??m) of germanium sulfide capped by bulbs depleted in germanium. ?? 1974.

Analysis of structural and optical properties of annealed fullerene thin films

NASA Astrophysics Data System (ADS)

El-Nahass, M. M.; Ali, H. A. M.; Gadallah, A.-S.; Atta Khedr, M.; Afify, H. A.

2015-08-01

Fullerene thin films were thermally deposited onto different substrates. The films annealed at 523 K for 10 h. X-ray diffraction technique was used to examine the structure of the films. The morphology of films was examined by field emission scanning electron microscopy. Fourier transform infrared spectra were recorded in wavenumber range 400-2000 cm-1. The optical characteristics were analyzed using UV- Vis-NIR spectrophotometric measurements in the spectral range 200-2500 nm. The refractive index and extinction coefficient were determined. Some dispersion parameters were calculated such as single oscillator energy, dispersion energy, dielectric constant at high frequency and lattice dielectric constant. As well as, the nonlinear optical susceptibility χ(3) and nonlinear refractive index n2 were determined.

Threat detection of liquid explosives and precursors from their x-ray scattering pattern using energy dispersive detector technology

NASA Astrophysics Data System (ADS)

Kehres, Jan; Lyksborg, Mark; Olsen, Ulrik L.

2017-09-01

Energy dispersive X-ray diffraction (EDXRD) can be applied for identification of liquid threats in luggage scanning in security applications. To define the instrumental design, the framework for data reduction and analysis and test the performance of the threat detection in various scenarios, a flexible laboratory EDXRD test setup was build. A data set of overall 570 EDXRD spectra has been acquired for training and testing of threat identification algorithms. The EDXRD data was acquired with limited count statistics and at multiple detector angles and merged after correction and normalization. Initial testing of the threat detection algorithms with this data set indicate the feasibility of detection levels of > 95 % true positive with < 6 % false positive alarms.

Nanometres-resolution Kikuchi patterns from materials science specimens with transmission electron forward scatter diffraction in the scanning electron microscope.

PubMed

Brodusch, N; Demers, H; Gauvin, R

2013-04-01

A charge-coupled device camera of an electron backscattered diffraction system in a scanning electron microscope was positioned below a thin specimen and transmission Kikuchi patterns were collected. Contrary to electron backscattered diffraction, transmission electron forward scatter diffraction provides phase identification and orientation mapping at the nanoscale. The minimum Pd particle size for which a Kikuchi diffraction pattern was detected and indexed reliably was 5.6 nm. An orientation mapping resolution of 5 nm was measured at 30 kV. The resolution obtained with transmission electron forward scatter diffraction was of the same order of magnitude than that reported in electron nanodiffraction in the transmission electron microscope. An energy dispersive spectrometer X-ray map and a transmission electron forward scatter diffraction orientation map were acquired simultaneously. The high-resolution chemical, phase and orientation maps provided at once information on the chemical form, orientation and coherency of precipitates in an aluminium-lithium 2099 alloy. © 2013 The Authors Journal of Microscopy © 2013 Royal Microscopical Society.

PSICHE: a new beamline dedicated to X-ray diffraction and tomography at high pressure at synchrotron SOLEIL

NASA Astrophysics Data System (ADS)

Guignot, N.; Itié, J.; Zerbino, P.; Delmotte, A.; Moreno, T.

2013-12-01

The PSICHE beamline (for 'Pressure, Structure and Imaging by Contrast at High Energy') is a new facility opened for high pressure experiments at synchrotron SOLEIL (St-Aubin, France). With its source, optics, detectors and 3 experimental stations, it can handle a large variety of experimental setups. High energy photons are produced with an in-vacuum wiggler. The white beam obtained, with photons energy ranging continuously from 15 to 80 keV (from a 2.75 GeV machine), is used on the first experimental station for energy dispersive X-ray diffraction (EDX) measurements using different pressure cells. The main setup is a 1200 tons load capacity multi-anvil press featuring a (100) DIA compression module with a 15° horizontal aperture, allowing measurements up to 30° in 2theta by rotating the press. Other setups are a Paris-Edinburgh (PE) large volume press and diamond anvil cells (DACs). On the detection side we have a rotating Ge detector, based on the CAESAR design described by Wang et al. (2004) (combination of EDX and angular dispersive X-ray diffraction, ADX). One of the difficulties when building such setups is the rotation mechanism which cannot be physically attached to the rotation axis, potentially leading to large circle of confusions on the horizontal position of this axis. Thanks to translation corrections done at each angle step, the circle of confusion is minimized to 3x6 μm2 along the 35° travel, making possible measurements on very small objects. Combining EDX and ADX has a lot of advantages and we will present our first results obtained using this setup. The PSICHE focusing optics and monochromator are also used to focus monochromatic beams (up to 52 keV) on 2 different experimental stations. The first focal point at 31 m gives a beam size of 100x50 μm2 (HxV) and is useful for low pressure experiments and experiments done with the PE press associated with Soller slits. A PerkinElmer flatpanel detector can be precisely scanned in 3 directions, making ADX measurements at the highest possible resolution on this beamline. This station will also be used for diffraction tomography experiments. The second focal point at 37.6 m is located behind KB mirrors on the third experimental station. 10x10 μm2 beam sizes (full width) are expected. This station will be used for DAC experiments, with or without our future laser heating setup. Finally, parallel beams can be produced with sizes up to 15x5 mm2 (HxV) for tomography experiments, in pink (filtered white) beam or monochromatic beam. We plan to use rotating anvils presses such as the rotoPEc (J. Philippe et al., 2013) to take full advantage of this beam mode, but it can be opened to other techniques. The PSICHE beamline is opened for users since July 2013. Some stations are not available yet, and will be opened through 2014 and 2015. References X. Dong et al., Ray tracing application in hard x-ray optical development: Soleil first wiggler beamline (PSICHÉ) case" (2011), Proc. SPIE 8141, 814113 Y. Wang et al., A new technique for angle-dispersive powder diffraction using an energy-dispersive setup and synchrotron radiation (2004), J. Appl. Cryst. 37, 947-956 J. Philippe, Y. Le Godec, F. Bergame et M. Morand, Patent INPI 11 62335 (2013)

Calibration of X-ray spectrometers for opacity experiments at the Orion laser facility (invited).

PubMed

Bentley, C; Allan, P; Brent, K; Bruce, N; Hoarty, D; Meadowcroft, A; Percival, J; Opie, C

2016-11-01

Accurately calibrated and characterised x-ray diagnostics are a key requirement in the fielding of experiments on the Orion laser where absolute measurements of x-ray emission are used to underpin the validity of models of emissivity and opacity. Diffraction crystals are used in spectrometers on Orion to record the dispersed spectral features emitted by the laser produced plasma to obtain a measurement of the plasma conditions. The ability to undertake diffraction crystal calibrations supports the successful outcome of these Orion experiments. This paper details the design and commissioning of a system to undertake these calibrations in the energy range 2.0 keV to approximately 8.5 keV. Improvements to the design are detailed which will extend the commissioned range of energies to below 1 keV.

Preparation of Al-Ti Master Alloys by Aluminothermic Reduction of TiO2 in Cryolite Melts at 960°C

NASA Astrophysics Data System (ADS)

Liu, Aimin; Xie, Kaiyu; Li, Liangxing; Shi, Zhongning; Hu, Xianwei; Xu, Junli; Gao, Bingliang; Wang, Zhaowen

Al-Ti master alloys were prepared by aluminothermic reduction between the dissolved titanium dioxide and aluminum in cryolite melts at 960°C. The kinetic analysis by differential scanning calorimetry indicated that the apparent activation energy of the reaction of reducing titanium dioxide by aluminium is 22.3 kJ/mol, and the reaction order is 0.5. The products were analyzed by means of X-ray diffraction, X-ray fluorescence, scanning electron microscopy and energy dispersive spectrometer. Results from X-ray diffraction showed that the phase compositions of produced alloys are Al and Al3Ti. In addition, Al-Ti master alloys containing 2-6 mass% Ti were formed at different reduction time of 2-5h in aluminothermic reduction experiment.

Nanouric acid or nanocalcium phosphate as central nidus to induce calcium oxalate stone formation: a high-resolution transmission electron microscopy study on urinary nanocrystallites

PubMed Central

Gao, Jie; Xue, Jun-Fa; Xu, Meng; Gui, Bao-Song; Wang, Feng-Xin; Ouyang, Jian-Ming

2014-01-01

Purpose This study aimed to accurately analyze the relationship between calcium oxalate (CaOx) stone formation and the components of urinary nanocrystallites. Method High-resolution transmission electron microscopy (HRTEM), selected area electron diffraction, fast Fourier transformation of HRTEM, and energy dispersive X-ray spectroscopy were performed to analyze the components of these nanocrystallites. Results The main components of CaOx stones are calcium oxalate monohydrate and a small amount of dehydrate, while those of urinary nanocrystallites are calcium oxalate monohydrate, uric acid, and calcium phosphate. The mechanism of formation of CaOx stones was discussed based on the components of urinary nanocrystallites. Conclusion The formation of CaOx stones is closely related both to the properties of urinary nanocrystallites and to the urinary components. The combination of HRTEM, fast Fourier transformation, selected area electron diffraction, and energy dispersive X-ray spectroscopy could be accurately performed to analyze the components of single urinary nanocrystallites. This result provides evidence for nanouric acid and/or nanocalcium phosphate crystallites as the central nidus to induce CaOx stone formation. PMID:25258530

Molybdenum cell for x-ray diffraction measurements of fluid alkali metals at high temperatures and high pressures

NASA Astrophysics Data System (ADS)

Matsuda, Kazuhiro; Tamura, Kozaburo; Katoh, Masahiro; Inui, Masanori

2004-03-01

We have developed a sample cell for x-ray diffraction measurements of fluid alkali metals at high temperatures and high pressures. All parts of the cell are made of molybdenum which is resistant to the chemical corrosion of alkali metals. Single crystalline molybdenum disks electrolytically thinned down to 40 μm were used as the walls of the cell through which x rays pass. The crystal orientation of the disks was controlled in order to reduce the background from the cell. All parts of the cell were assembled and brazed together using a high-temperature Ru-Mo alloy. Energy dispersive x-ray diffraction measurements have been successfully carried out for fluid rubidium up to 1973 K and 16.2 MPa. The obtained S(Q) demonstrates the applicability of the molybdenum cell to x-ray diffraction measurements of fluid alkali metals at high temperatures and high pressures.

Influence of gamma ray irradiation on stoichiometry of hydrothermally synthesized bismuth telluride nanoparticles

NASA Astrophysics Data System (ADS)

Abishek, N. S.; Naik, K. Gopalakrishna

2018-05-01

Bismuth telluride (Bi2Te3) nanoparticles were synthesized by the hydrothermal method at 200 °C for 24 h. The synthesized Bi2Te3 nanoparticles were irradiated with gamma rays at doses of 50 kGy and 100 kGy. The structural characterization of the pre-irradiated and post-irradiated samples was carried out by X-ray diffraction technique and was found to have rhombohedral phase having R3 ¯m (166) space group. The X-ray diffraction peaks were found to shift towards lower diffraction angle with gamma ray irradiation. The morphologies and compositions of the grown Bi2Te3 nanoparticles were studied using Field Emission Scanning Electron Microscope and X-ray energy dispersive analysis, respectively. The possible cause for the shift in the X-ray diffraction peaks with gamma ray irradiation has been discussed in the present work.

Production of oxygen from lunar ilmenite

NASA Technical Reports Server (NTRS)

Shadman, F.; Zhao, Y.

1991-01-01

The kinetics and the mechanism of reduction of synthetic ilmenite by hydrogen in the temperature range of 807 to 1014 C were investigated. At temperatures below 876 C, the temporal profiles of conversion have a sigmoidal shape and indicate the presence of three different stages (induction, acceleration, and deceleration) during the reduction reaction. The apparent activation energy for the reaction is 22.3 kcal/mole, whereas the intrinsic activation energy is 16.9 kcal/mole. Scanning electron microscopy and energy dispersive x-ray analyses show that the diffusion of Fe product away from the reaction front and through the TiO2 phase, followed by the nucleation and growth of a separate Fe phase is an important step affecting the process kinetics. X-ray diffraction and wavelength dispersive x-ray results indicate that the TiO2 can be reduced to lower oxides of titanium at temperatures higher than 876 C.

Vapor phase diamond growth technology

NASA Technical Reports Server (NTRS)

Angus, J. C.

1981-01-01

Ion beam deposition chambers used for carbon film generation were designed and constructed. Features of the developed equipment include: (1) carbon ion energies down to approx. 50 eV; (2) in suit surface monitoring with HEED; (3) provision for flooding the surface with ultraviolet radiation; (4) infrared laser heating of substrate; (5) residual gas monitoring; (6) provision for several source gases, including diborane for doping studies; and (7) growth from either hydrocarbon source gases or from carbon/argon arc sources. Various analytical techniques for characterization of from carbon/argon arc sources. Various analytical techniques for characterization of the ion deposited carbon films used to establish the nature of the chemical bonding and crystallographic structure of the films are discussed. These include: H2204/HN03 etch; resistance measurements; hardness tests; Fourier transform infrared spectroscopy; scanning auger microscopy; electron spectroscopy for chemical analysis; electron diffraction and energy dispersive X-ray analysis; electron energy loss spectroscopy; density measurements; secondary ion mass spectroscopy; high energy electron diffraction; and electron spin resonance. Results of the tests are summarized.

Hair treatment device for providing dispersed colors by light diffraction

DOEpatents

Lamartine, Bruce Carvell; Orler, Bruce E.; Sutton, Richard Matthew Charles; Song, Shuangqi

2016-01-26

Hair was coated with polymer-containing fluid and then hot pressed to form a composite of hair and a polymer film imprinted with a nanopattern. Polychromatic light incident on the nanopattern is diffracted into dispersed colored light.

Hair treatment process providing dispersed colors by light diffraction

DOEpatents

Lamartine, Bruce Carvell; Orler, E. Bruce; Sutton, Richard Matthew Charles; Song, Shuangqi

2014-11-11

Hair was coated with polymer-containing fluid and then hot pressed to form a composite of hair and a polymer film imprinted with a nanopattern. Polychromatic light incident on the nanopattern is diffracted into dispersed colored light.

Hair treatment process providing dispersed colors by light diffraction

DOEpatents

Lamartine, Bruce Carvell; Orler, E. Bruce; Sutton, Richard Matthew Charles; Song, Shuangqi

2013-12-17

Hair was coated with polymer-containing fluid and then hot pressed to form a composite of hair and a polymer film imprinted with a nanopattern. Polychromatic light incident on the nanopattern is diffracted into dispersed colored light.

Portable total reflection x-ray fluorescence analysis in the identification of unknown laboratory hazards

DOE Office of Scientific and Technical Information (OSTI.GOV)

Liu, Ying, E-mail: liu.ying.48r@st.kyoto-u.ac.jp; Imashuku, Susumu; Sasaki, Nobuharu

In this study, a portable total reflection x-ray fluorescence (TXRF) spectrometer was used to analyze unknown laboratory hazards that precipitated on exterior surfaces of cooling pipes and fume hood pipes in chemical laboratories. With the aim to examine the accuracy of TXRF analysis for the determination of elemental composition, analytical results were compared with those of wavelength-dispersive x-ray fluorescence spectrometry, scanning electron microscope and energy-dispersive x-ray spectrometry, energy-dispersive x-ray fluorescence spectrometry, inductively coupled plasma atomic emission spectrometry, x-ray diffraction spectrometry (XRD), and x-ray photoelectron spectroscopy (XPS). Detailed comparison of data confirmed that the TXRF method itself was not sufficient tomore » determine all the elements (Z > 11) contained in the samples. In addition, results suggest that XRD should be combined with XPS in order to accurately determine compound composition. This study demonstrates that at least two analytical methods should be used in order to analyze the composition of unknown real samples.« less

Synthesis and structural characterization of CZTS nanoparticles

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lydia, R.; Reddy, P. Sreedhara

2013-06-03

The CZTS nanoparticles were successfully synthesized by Chemical co-precipitation method with different pH values in the range of 6 to 8. The synthesized nanoparticles were characterized by X-ray diffraction, scanning electron microscopy and energy dispersive spectroscopy. XRD studies revealed that the CZTS nanoparticles exhibited Kesterite Structure with preferential orientation along the (112) direction. Sample at pH value of 7 reached the nearly stoichiometric ratio.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chen Shuguang, E-mail: hustcsg@sohu.com; Zeng Kai; Li Haibin

Dispersed rhombohedral NiS rods with high aspect ratios and rhombic dodecahedron-like cubic NiS{sub 2} crystals were prepared by solvothermal routes using NiCl{sub 2}.6H{sub 2}O and Na{sub 2}S{sub 2}O{sub 3}.5H{sub 2}O as reagents and ethylenediamine as a solvent, and 3D blossoming flower-like rhombohedral NiS microstructures were synthesized using different sulfur sources of thiourea. The products were characterized by X-ray diffraction, field emission scanning electron microscopy, transmission electron microscopy, energy dispersion spectrometry and selected area electronic diffraction. All the products were pure and had good single crystalline nature. The synthesis parameters were of great importance on the purity and morphology of themore » products. The possible growth mechanisms have been discussed based on the analyses of the effects of sulfur sources and solvent on the crystal structures and detailed configurations of the products. The present work is likely to help the phase-controlled synthesis of other metal chalcogenides. - Graphical abstract: Rhombohedral NiS dispersed rods and 3D flower-like microstructures are evolved from dispersed nucleus and aggregate of nucleus, respectively, and the cross-sections of such rods are in equilateral triangle-like shape. Highlights: > 3D blossoming flower-like r-NiS microstructures are obtained. > Equilateral triangle-like cross-sections of r-NiS rods are observed. > Approach based on XRD analysis to phase-controlled synthesis is presented.« less

In-situ and operando characterization of batteries with energy-dispersive synchrotron x-ray diffraction

NASA Astrophysics Data System (ADS)

Paxton, William Arthur

Batteries play a pivotal role in the low-carbon society that is required to thwart the effects of climate change. Alternative low-carbon energy sources, such as wind and solar, are often intermittent and unreliable. Batteries are able capture their energy and deliver it later when it is needed. The implementation of battery systems in grid-level and transportation sectors is essential for efficient use of alternative energy sources. Scientists and engineers need better tools to analyze and measure the performance characteristics of batteries. One of the main hindrances in the progress of battery research is that the constituent electrode materials are inaccessible once an electrochemical cell is constructed. This leaves the researcher with a limited number of available feedback mechanisms to assess the cell's performance, e.g., current, voltage, and impedance. These data are limited in their ability to reveal the more-localized smaller-scale structural mechanisms on which the batteries' performance is so dependent. Energy-dispersive x-ray diffraction (EDXRD) is one of the few techniques that can internally probe a sealed battery. By analyzing the structural behavior of battery electrodes, one is able to gain insight to the physical properties on which the battery's performance is dependent. In this dissertation, EDXRD with ultrahigh energy synchrotron radiation is used to probe the electrodes of manufactured primary and secondary lithium batteries under in-situ and operando conditions. The technique is then applied to solve specific challenges facing lithium ion batteries. Diffraction spectra are collected from within a battery at 40 micrometer resolution. Peak-fitting is used to quantitatively estimate the abundance of lithiated and non-lithiated phases. Through mapping the distribution of phases within, structural changes are linked to the battery's galvanic response. A three-dimensional spatial analysis of lithium iron phosphate batteries suggests that evolution of inhomogeneity is linked to the particle connectivity. Despite a non-linear local response, the average of the measured ensemble behaves linearly. The results suggest that inhomogeneity can be difficult to measure and highlights the power of the EDXRD technique. Additional applications of EDXRD are discussed.

Nanoscale interfacial mixing of Au/Bi layers using MeV ion beams

NASA Astrophysics Data System (ADS)

Prusty, Sudakshina; Siva, V.; Ojha, S.; Kabiraj, D.; Sahoo, P. K.

2017-05-01

We have studied nanoscale mixing of thermally deposited double bilayer films of Au/Bi after irradiating them by 1.5 MeV Au2+ ions. Post irradiation effects on the morphology and elemental identification in these films are studied by Scanning electron microscopy (SEM) and Energy dispersive X-ray spectroscopy (EDS). Glancing angle X-ray diffraction (GAXRD) of the samples indicate marginal changes in the irradiated samples due to combined effect of nuclear and electronic energy loss. The interfacial mixing is studied by Rutherford backscattering (RBS).

ITEP MEVVA ion beam for rhenium silicide production.

PubMed

Kulevoy, T; Gerasimenko, N; Seleznev, D; Kropachev, G; Kozlov, A; Kuibeda, R; Yakushin, P; Petrenko, S; Medetov, N; Zaporozhan, O

2010-02-01

The rhenium silicides are very attractive materials for semiconductor industry. In the Institute for Theoretical and Experimental Physics (ITEP) at the ion source test bench the research program of rhenium silicide production by ion beam implantation are going on. The investigation of silicon wafer after implantation of rhenium ion beam with different energy and with different total dose were carried out by secondary ions mass spectrometry, energy-dispersive x-ray microanalysis, and x-ray diffraction analysis. The first promising results of rhenium silicide film production by high intensity ion beam implantation are presented.

Development of ultrahigh-resolution inelastic x-ray scattering optics

NASA Astrophysics Data System (ADS)

Huang, Xian-Rong; Zhong, Zhong; Cai, Yong Q.; Coburn, S.

2008-08-01

One of the major goals of the National Synchrotron Light Source II project is to achieve ultrahigh energy resolution up to 0.1 meV for medium-energy inelastic X-ray scattering spectroscopy based on the angular dispersion optics employing extremely asymmetric backscattering geometry. In this papaer, we describe the complete monochromatization mechanisms underlying the new optics. We have also designed and tested a CDW-CDW prototype under ambient condition, with which we have successfully demonstrated the important angular dispersion effect, the Borrman enhanced transmission effect, and other optical principles involved in every step of the entire diffraction process, and found good agreement with the theoretical expectations. These studies indicate that the new optics are feasible in principle but face some technical challenges that need to be solved by our future systematic research and development activities before their practical applications.

Formation of Porous Germanium Layers by Silver-Ion Implantation

NASA Astrophysics Data System (ADS)

Stepanov, A. L.; Vorob'ev, V. V.; Nuzhdin, V. I.; Valeev, V. F.; Osin, Yu. N.

2018-04-01

We propose a method for the formation of porous germanium ( P-Ge) layers containing silver nanoparticles by means of high-dose implantation of low-energy Ag+ ions into single-crystalline germanium ( c-Ge). This is demonstrated by implantation of 30-keV Ag+ ions into a polished c-Ge plate to a dose of 1.5 × 1017 ion/cm2 at an ion beam-current density of 5 μA/cm2. Examination by high-resolution scanning electron microscopy (SEM), atomic-force microscopy (AFM), X-ray diffraction (XRD), energy-dispersive X-ray (EDX) microanalysis, and reflection high-energy electron diffraction (RHEED) showed that the implantation of silver ions into c-Ge surface led to the formation of a P-Ge layer with spongy structure comprising a network of interwoven nanofibers with an average diameter of ˜10-20 nm Ag nanoparticles on the ends of fibers. It is also established that the formation of pores during Ag+ ion implantation is accompanied by effective sputtering of the Ge surface.

CheMin Instrument Performance and Calibration on Mars

NASA Technical Reports Server (NTRS)

Vaniman, D. T.; Blake, D. F.; Morookian, J. M.; Yen, A. S.; Ming, D. W.; Morris, R. V.; Achilles, C. N.; Bish, D. L.; Chipera, S. J.; Morrison, S. M.;

DOE Office of Scientific and Technical Information (OSTI.GOV)

Dhanavel, S.; Nivethaa, E. A. K.; Esther, G.

Chitosan supported Palladium nanoparticles were synthesized by a simple cost effective chemical reduction method using NaBH{sub 4}. The prepared nanocomposite was characterized by X-Ray diffraction analysis, FESEM and Energy dispersive spectroscopy analysis of X-rays (EDAX). The catalytic performance of the nanocomposite was evaluated on the reduction of 2-Nitrophenol to the 2-Amino phenol with rate constant 1.08 × 10{sup −3} S{sup −1} by NaBH{sub 4} using Spectrophotometer.

Hybrid diffractive-refractive optical system design of head-mounted display for augmented reality

NASA Astrophysics Data System (ADS)

Zhang, Huijuan

2005-02-01

An optical see-through head-mounted display for augmented reality is designed in this paper. Considering the factors, such as the optical performance, the utilization ratios of energy of real world and virtual world, the feelings of users when he wears it and etc., a structure of the optical see-through is adopted. With the characteristics of the particular negative dispersive and the power of realizing random-phase modulation, the diffractive surface is helpful for optical system of reducing weight, simplifying structure and etc., and a diffractive surface is introduced in our optical system. The optical system with 25 mm eye relief, 12 mm exit pupil and 20° (H)x15.4° (V) field-of-view is designed. The utilization ratios of energy of real world and virtual world are 1/4 and 1/2, respectively. The angular resolution of display is 0.27 mrad and it less than that of the minimum of human eyes. The diameter of this system is less than 46mm, and it applies the binocular. This diffractive-refractive optical system of see-through head-mounted display not only satisfies the demands of user"s factors in structure, but also with high resolution, very small chromatic aberration and distortion, and satisfies the need of augmented reality. In the end, the parameters of the diffractive surface are discussed.

Study for the dispersion of double-diffraction spectrometers

NASA Astrophysics Data System (ADS)

Pang, Yajun; Zhang, Yinxin; Yang, Huaidong; Huang, Zhanhua; Xu, Mingming; Jin, Guofan

2018-01-01

Double-cascade spectrometers and double-pass spectrometers can be uniformly called double-diffraction spectrometers. In current double-diffraction spectrometers design theory, the differences of the incident angles in the second diffraction are ignored. There is a significant difference between the design in theory and the actual result. In this study, based on the geometries of the double-diffraction spectrometers, we strictly derived the theoretical formulas of their dispersion. By employing the ZEMAX simulation software, verification of our theoretical model is implemented, and the simulation results show big agreement with our theoretical formulas. Based on the conclusions, a double-pass spectrometer was set up and tested, and the experiment results agree with the theoretical model and the simulation.

Excitation of surface waves on one-dimensional solid–fluid phononic crystals and the beam displacement effect

DOE Office of Scientific and Technical Information (OSTI.GOV)

Moiseyenko, Rayisa P.; Georgia Institute of Technology, UMI Georgia Tech – CNRS, George W. Woodruff School of Mechanical Engineering, Georgia Tech Lorraine, 2 rue Marconi, 57070 Metz-Technopole; Liu, Jingfei

The possibility of surface wave generation by diffraction of pressure waves on deeply corrugated one-dimensional phononic crystal gratings is studied both theoretically and experimentally. Generation of leaky surface waves, indeed, is generally invoked in the explanation of the beam displacement effect that can be observed upon reflection on a shallow grating of an acoustic beam of finite width. True surface waves of the grating, however, have a dispersion that lies below the sound cone in water. They thus cannot satisfy the phase-matching condition for diffraction from plane waves of infinite extent incident from water. Diffraction measurements indicate that deeply corrugatedmore » one-dimensional phononic crystal gratings defined in a silicon wafer are very efficient diffraction gratings. They also confirm that all propagating waves detected in water follow the grating law. Numerical simulations however reveal that in the sub-diffraction regime, acoustic energy of a beam of finite extent can be transferred to elastic waves guided at the surface of the grating. Their leakage to the specular direction along the grating surface explains the apparent beam displacement effect.« less

Femtosecond fiber CPA system based on picosecond master oscillator and power amplifier with CCC fiber.

PubMed

Želudevičius, J; Danilevičius, R; Viskontas, K; Rusteika, N; Regelskis, K

2013-03-11

Results of numerical and experimental investigations of the simple fiber CPA system seeded by nearly bandwidth-limited pulses from the picosecond oscillator are presented. We utilized self-phase modulation in a stretcher fiber to broaden the pulse spectrum and dispersion of the fiber to stretch pulses in time. During amplification in the ytterbium-doped CCC fiber, gain-shaping and self-phase modulation effects were observed, which improved pulse compression with a bulk diffraction grating compressor. After compression with spectral filtering, pulses with the duration of 400 fs and energy as high as 50 µJ were achieved, and the output beam quality was nearly diffraction-limited.

Focusing Leaky Waves: A Class of Electromagnetic Localized Waves with Complex Spectra

NASA Astrophysics Data System (ADS)

Fuscaldo, Walter; Comite, Davide; Boesso, Alessandro; Baccarelli, Paolo; Burghignoli, Paolo; Galli, Alessandro

2018-05-01

Localized waves, i.e., the wide class of limited-diffraction, limited-dispersion solutions to the wave equation are generally characterized by real wave numbers. We consider the role played by localized waves with generally complex "leaky" wave numbers. First, the impact of the imaginary part of the wave number (i.e., the leakage constant) on the diffractive (spatial broadening) features of monochromatic localized solutions (i.e., beams) is rigorously evaluated. Then general conditions are derived to show that only a restricted class of spectra (either real or complex) allows for generating a causal localized wave. It turns out that backward leaky waves fall into this category. On this ground, several criteria for the systematic design of wideband radiators, namely, periodic radial waveguides based on backward leaky waves, are established in the framework of leaky-wave theory. An effective design method is proposed to minimize the frequency dispersion of the proposed class of devices and the impact of the "leakage" on the dispersive (temporal broadening) features of polychromatic localized solutions (i.e., pulses) is accounted for. Numerical results corroborate the concept, clearly highlighting the advantages and limitations of the leaky-wave approach for the generation of localized pulses at millimeter-wave frequencies, where energy focusing is in high demand in modern applications.

Multilayer manipulated diffraction in flower beetles Torynorrhina flammea: intraspecific structural colouration variation

NASA Astrophysics Data System (ADS)

Song, C. X.; Liu, F.; Hao, Y. H.; Hu, X. H.; Zhang, Y. F.; Liu, X. H.

2014-10-01

We report that the intraspecific structural colouration variation of the beetle Torynorrhina flammea is a result of diffraction shifting manipulated by a multilayer sub-structure contained in a three-dimensional (3D) photonic architecture. With a perpendicularly 2D quasiperiodic diffraction grating inserted into the multilayer, the 3D photonic structure gives rise to anticrossing bandgaps of diffraction from the coupling of grating and multilayer bands. The angular dispersion of diffraction induced by the multilayer band shift behaves normally, in contrast to the ‘ultranegative’ behaviour controlled by the quasiperiodic grating. In addition, the diffraction wavelength is more sensitive to the multilayer periodicity than the diffraction grating constant, which explains the ‘smart’ biological selection of T. flammea in its intraspecific colouration variation from red to green to blue. The elucidated mechanism could be advantageous for the potential exploration of novel dispersive optical elements.

New opportunities in the preparation of nanocomposites for biomedical applications: revised mechanosynthesis of magnetite-silica nanocomposites

NASA Astrophysics Data System (ADS)

Scano, Alessandra; Cabras, Valentina; Marongiu, Francesca; Peddis, Davide; Pilloni, Martina; Ennas, Guido

2017-02-01

Environmentally friendly preparation of functionalized magnetite-silica (Fe3O4/SiO2) nanocomposites (NCs) with different SiO2 content (6, 20 and 50 wt%) using revised mechanosynthesis is reported. High-energy ball milling of α-Fe2O3, Si and SiO2 mixtures was followed by hydrolysis and condensation of 3-aminopropyl-triethoxysilane. X-ray powder diffraction and transmission electron microscopy showed the formation of almost spherical Fe3O4 nanocrystals with a narrow size distribution (4-6 nm) uniformly dispersed in the amorphous 100-200 nm SiO2 agglomerates. Scanning electron microscopy and energy dispersive spectroscopy were used to study the elemental distribution in the sample. Fourier transform infrared spectroscopy confirmed the NC surface functionalization with amino groups. Magnetic properties were also explored, indicating a homogeneous distribution of magnetic nanoparticles in the silica matrix.

Hydroxyapatite-armored poly(ε-caprolactone) microspheres and hydroxyapatite microcapsules fabricated via a Pickering emulsion route.

PubMed

Fujii, Syuji; Okada, Masahiro; Nishimura, Taiki; Maeda, Hayata; Sugimoto, Tatsuya; Hamasaki, Hiroyuki; Furuzono, Tsutomu; Nakamura, Yoshinobu

2012-05-15

Hydroxyapatite (HAp) nanoparticle-armored poly(ε-caprolactone) (PCL) microspheres were fabricated via a "Pickering-type" emulsion solvent evaporation method in the absence of any molecular surfactants. It was clarified that the interaction between carbonyl/carboxylic acid groups of PCL and the HAp nanoparticles at an oil-water interface played a crucial role in the preparation of the stable Pickering-type emulsions and the HAp nanoparticle-armored microspheres. The HAp nanoparticle-armored PCL microspheres were characterized in terms of size, size distribution, morphology, and chemical compositions using scanning electron microscopy, laser diffraction, energy dispersive X-ray microanalysis, and thermogravimetric analysis. The presence of HAp nanoparticles at the surface of the microspheres was confirmed by scanning electron microscopy and energy dispersive X-ray microanalysis. Pyrolysis of the PCL cores led to the formation of the corresponding HAp hollow microcapsules. Copyright © 2012 Elsevier Inc. All rights reserved.

Investigation of ZrO/sub 2//mullite solid solution by energy dispersive X-ray spectroscopy and electron diffraction

DOE Office of Scientific and Technical Information (OSTI.GOV)

Dinger, T.R.; Krishnam, K.M.; Moya, J.S.

1984-10-01

A mullite/15 vol.%ZrO/sub 2/ composite was analyzed using the techniques of microdiffraction and energy dispersive X-ray spectroscopy (EDXS). The EDXS results indicate that there is a significantly high solid solubility of mullite in zirconia and zirconia in mullite; microdiffraction results suggest that ordering occurs in the ZrO/sub 2/(ss) phase based on the presence of forbidden reflections for the P 2/sub 1//c space group of monoclinic zirconia. The presence of a secondary phase at the grain boundaries, either amorphous or crystalline, has not been generally detected throughout the bulk. The results provide experimental evidence for the hypothesis of Moya and Osendimore » that the increased toughness and flexural strength of these composites are related to solid solution effects rather than to transformation or microcrack toughening mechanisms.« less

Effect of heat treatment on morphological, structural and optical properties of CoMTPP thin films

NASA Astrophysics Data System (ADS)

El-Nahass, M. M.; Ammar, A. H.; Farag, A. A. M.; Atta, A. A.; El-Zaidia, E. F. M.

2011-03-01

The morphologies and crystal structures of 5,10,15,20-tetrakis(4-methoxyphenyl)-21 H,23 H-porphine cobalt(II), CoMTPP, thin films were investigated by scanning electron microscopy (SEM) and X-ray diffraction (XRD), respectively. Optical constants namely the refractive index, n, and the absorption index, k, of CoMTPP were estimated by using spectrophotometric measurements of transmittance and reflectance in the spectral range from 200 to 2500 nm. The dispersion of the refractive index in terms of the single oscillator in the transparent region is discussed. The single oscillator energy ( E0), the dispersion energy ( E d), the high frequency dielectric constant ( ɛ∞) and the lattice dielectric constant ( ɛ L) were calculated. The analysis of the spectral behavior of the absorption coefficient in the intrinsic absorption region reveals two indirect allowed transitions for as-deposited and annealed films.

Effect of Cooling Rates on γ → α Transformation and Metastable States in Fe-Cu Alloys with Addition of Ni

NASA Astrophysics Data System (ADS)

Crozet, C.; Verdier, M.; Lay, S.; Antoni-Zdziobek, A.

2018-07-01

α/γ phase transformations occurring in Fe-10Cu-xNi alloys (0 ≤ x ≤ 15 in mass%) were studied using X-ray diffraction, scanning electron microscopy, electron back scattered diffraction, transmission electron microscopy and chemical analysis, combining X-ray microanalysis with energy dispersive spectrometry in the scanning electron microscope and electron microprobe analysis with wavelength dispersive spectrometry. The influence of cooling rate on the microstructure was investigated using ice-brine quenching and 2 °C/min slow cooling rate performed with dilatometry. Ni addition induces metastable transformations on cooling: massive and bainitic ferrite are formed depending on the alloy composition and cooling rate. Moreover, most of the Cu phase precipitates on cooling giving rise to a fine distribution of Cu particles in the ferrite grains. For both cooling conditions, the hardness increases with increasing Ni content and a higher hardness is obtained in the quenched alloy for each composition. The change in hardness is correlated to the effect of Ni solid solution, transformation structure and size of Cu particles.

Direct design of achromatic lens for Lambertian sources in collimating illumination

NASA Astrophysics Data System (ADS)

Yin, Peng; Xu, Xiping; Jiang, Zhaoguo; Wang, Hongshu

2017-10-01

Illumination design used to redistribute the spatial energy distribution of light source is a key technique in lighting applications. However, there is still no effective illumination design method for the removing of the chromatic dispersion. What we present here is an achromatic lens design to enhance the efficiency and uniform illumination of white light-emitting diode (LED) with diffractive optical element (DOE). We employ the chromatic aberration value (deg) to measure the degree of chromatic dispersion in illumination systems. Monte Carlo ray tracing simulation results indicate that the chromatic dispersion of the modified achromatic collimator significantly decreases from 0.5 to 0.1 with LED chip size of 1.0mm×1.0mm and simulation efficiency of 90.73%, compared with the traditional collimator. Moreover, with different corrected wavelengths we compared different chromatic aberration values that followed with the changing pupil percent. The achromatic collimator provided an effective way to achieve white LED with low chromatic dispersion at high efficiency and uniform illumination.

Facile and green fabrication of electrospun poly(vinyl alcohol) nanofibrous mats doped with narrowly dispersed silver nanoparticles.

PubMed

Lin, Song; Wang, Run-Ze; Yi, Ying; Wang, Zheng; Hao, Li-Mei; Wu, Jin-Hui; Hu, Guo-Han; He, Hua

2014-01-01

Submicrometer-scale poly(vinyl alcohol) (PVA) nanofibrous mats loaded with aligned and narrowly dispersed silver nanoparticles (AgNPs) are obtained via the electrospinning process from pure water. This facile and green procedure did not need any other chemicals or organic solvents. The doped AgNPs are narrowly distributed, 4.3±0.7 nm and their contents on the nanofabric mats can be easily tuned via in situ ultraviolet light irradiation or under preheating conditions, but with different particle sizes and size distributions. The morphology, loading concentrations, and dispersities of AgNPs embedded within PVA nanofiber mats are characterized by transmission electron microscopy, scanning electron microscopy, energy dispersive X-ray spectroscopy, ultraviolet-visible spectra, X-ray photoelectron spectroscopy, and X-ray diffraction, respectively. Moreover, the biocidal activities and cytotoxicity of the electrospun nanofiber mats are determined by zone of inhibition, dynamic shaking method, and cell counting kit (CCK)-8 assay tests.

Effect of rapid thermal annealing temperature on the dispersion of Si nanocrystals in SiO2 matrix

NASA Astrophysics Data System (ADS)

Saxena, Nupur; Kumar, Pragati; Gupta, Vinay

2015-05-01

Effect of rapid thermal annealing temperature on the dispersion of silicon nanocrystals (Si-NC's) embedded in SiO2 matrix grown by atom beam sputtering (ABS) method is reported. The dispersion of Si NCs in SiO2 is an important issue to fabricate high efficiency devices based on Si-NC's. The transmission electron microscopy studies reveal that the precipitation of excess silicon is almost uniform and the particles grow in almost uniform size upto 850 °C. The size distribution of the particles broadens and becomes bimodal as the temperature is increased to 950 °C. This suggests that by controlling the annealing temperature, the dispersion of Si-NC's can be controlled. The results are supported by selected area diffraction (SAED) studies and micro photoluminescence (PL) spectroscopy. The discussion of effect of particle size distribution on PL spectrum is presented based on tight binding approximation (TBA) method using Gaussian and log-normal distribution of particles. The study suggests that the dispersion and consequently emission energy varies as a function of particle size distribution and that can be controlled by annealing parameters.

Catharanthus roseus: a natural source for the synthesis of silver nanoparticles

PubMed Central

Mukunthan, KS; Elumalai, EK; Patel, Trupti N; Murty, V Ramachandra

2011-01-01

Objective To develop a simple rapid procedure for bioreduction of silver nanoparticles (AgNPs) using aqueous leaves extracts of Catharanthus roseus (C. roseus). Methods Characterization were determined by using UV-Vis spectrophotometry, scanning electron microscopy (SEM), energy dispersive X-ray and X-ray diffraction. Results SEM showed the formation of silver nanoparticles with an average size of 67 nm to 48 nm. X-ray diffraction analysis showed that the particles were crystalline in nature with face centered cubic geometry. Conclusions C. roseus demonstrates strong potential for synthesis of silver nanoparticles by rapid reduction of silver ions (Ag+ to Ag0). This study provides evidence for developing large scale commercial production of value-added products for biomedical/nanotechnology-based industries. PMID:23569773

An Assessment of Subsurface Residual Stress Analysis in SLM Ti-6Al-4V

PubMed Central

Mishurova, Tatiana; Cabeza, Sandra; Artzt, Katia; Haubrich, Jan; Klaus, Manuela; Genzel, Christoph; Requena, Guillermo; Bruno, Giovanni

2017-01-01

Ti-6Al-4V bridges were additively fabricated by selective laser melting (SLM) under different scanning speed conditions, to compare the effect of process energy density on the residual stress state. Subsurface lattice strain characterization was conducted by means of synchrotron diffraction in energy dispersive mode. High tensile strain gradients were found at the frontal surface for samples in an as-built condition. The geometry of the samples promotes increasing strains towards the pillar of the bridges. We observed that the higher the laser energy density during fabrication, the lower the lattice strains. A relief of lattice strains takes place after heat treatment. PMID:28772706

Growth of GaN@InGaN Core-Shell and Au-GaN Hybrid Nanostructures for Energy Applications

DOE PAGES

Kuykendall, Tevye; Aloni, Shaul; Jen-La Plante, Ilan; ...

2009-01-01

We demonstrated a method to control the bandgap energy of GaN nanowires by forming GaN@InGaN core-shell hybrid structures using metal organic chemical vapor deposition (MOCVD). Furthermore, we show the growth of Au nanoparticles on the surface of GaN nanowires in solution at room temperature. The work shown here is a first step toward engineering properties that are crucial for the rational design and synthesis of a new class of photocatalytic materials. The hybrid structures were characterized by various techniques, including photoluminescence (PL), energy dispersive x-ray spectroscopy (EDS), transmission and scanning electron microscopy (TEM and SEM), and x-ray diffraction (XRD).

Carbon Nanotube-Reinforced Aluminum Matrix Composites Produced by High-Energy Ball Milling

NASA Astrophysics Data System (ADS)

Travessa, Dilermando N.; da Rocha, Geovana V. B.; Cardoso, Kátia R.; Lieblich, Marcela

2017-05-01

Although multiwall carbon nanotubes (MWCNT) are promising materials to strengthen lightweight aluminum matrix composites, their dispersion into the metallic matrix is challenge. In the present work, MWCNT were dispersed into age-hardenable AA6061 aluminum alloy by high-energy ball milling and the blend was subsequently hot-extruded. The composite bars obtained were heat-treated by solution heat treatment at 520 °C and artificially aged at 177 °C for 8 h, in order to reach the T6 temper. Special attention was given to the integrity of the MWCNT along the entire composite production. The microstructure of the obtained bars was evaluated by optical and scanning electron microscopy, and the mechanical properties were evaluated by Vickers microhardness tests. Raman spectroscopy, x-ray diffraction and transmission electron microscopy were employed to evaluate the structural integrity of MWCNT. It was found that milling time is critical to reach a proper dispersion of the reinforcing phase. The composite hardness increased up to 67% with the dispersion of 2% in weight of MWCNT, when comparing with un-reinforced bars produced by similar route. However, age hardening was not observed in composite bars after heat treatment. It was also found that MWCNT continuously degraded along the process, being partially converted into Al4C3 in the final composite.

Poly(vinylpyrrolidone) coated iron nanoparticles in polar aprotic solvent.

PubMed

Ban, Zhihui; Cushing, Brian L; O'Connor, Charles J

2008-04-01

Poly(vinylpyrrolidone) (PVP) coated iron nanoparticles which show well-defined core-shell structures have been successfully synthesized in a polar aprotic solvent. In this approach, PVP was employed not as capping agent, but as coating polymer directly applied to the metallic (iron) core nanoparticles. The morphologies, structures, compositions and magnetic properties of the products were investigated by transmission electron microscopy (TEM), X-ray powder diffraction (XRD), energy dispersive X-ray spectroscopy (EDXS), SQUID magnetometry and FTIR spectroscopy.

Synthesis and characterization of polycrystalline CdSiP2

NASA Astrophysics Data System (ADS)

Bereznaya, S. A.; Korotchenko, Z. V.; Sarkisov, S. Yu; Korolkov, I. V.; Kuchumov, B. M.; Saprykin, A. I.; Atuchin, V. V.

2018-05-01

A modified method is proposed for the CdSiP2 compound synthesis from elemental starting components. The developed technique allows completing the synthesis process within 30 h. The phase and chemical composition of the synthesized material were confirmed by the x-ray diffraction analysis and scanning electron microscopy with energy-dispersive spectroscopy. The transparent crystal block sized 3 × 3 × 2 mm3 was cut from the polycrystalline ingot and characterized by optical methods.

Photosynthetic microorganism-mediated synthesis of akaganeite (beta-FeOOH) nanorods.

PubMed

Brayner, Roberta; Yéprémian, Claude; Djediat, Chakib; Coradin, Thibaud; Herbst, Fréderic; Livage, Jacques; Fiévet, Fernand; Couté, Alain

2009-09-01

Common Anabaena and Calothrix cyanobacteria and Klebsormidium green algae are shown to form intracellularly akaganeite beta-FeOOH nanorods of well-controlled size and unusual morphology at room temperature. X-ray diffraction (XRD), transmission electron microscopy (TEM), and scanning electron microscopy X-ray energy dispersive spectrometry (SEM-EDS) analyses are used to investigate particle structure, size, and morphology. A mechanism involving iron-siderophore complex formation is proposed and compared with iron biomineralization in magnetotactic bacteria.

Symposium U: Thermoelectric Power Generation. Held in Boston, Massachusetts on November 26-29, 2007

DTIC Science & Technology

2008-04-01

including X - ray /electron diffraction, TGA analysis, Raman / Fourier Transform Infrared Spectroscopy, electron microscopy, Rutherford back-scattering and...Energy dispersive X - ray analysis were performed on the treated sample. The results revealed that a surface layer (from 10 nm to up to micron in...nanoparticles into a matrix of bulk Bi2Te 3 material via a hot pressing process. These nanocomposites have been examined by SEM and X - ray powder

Electronic and structural characteristics of zinc-blende wurtzite biphasic homostructure GaN nanowires

DOE PAGES

Jacobs, Benjamin W.; Ayres, Virginia M.; Petkov, Mihail P.; ...

2007-04-07

Here, we report a new biphasic crystalline wurtzite/zinc-blende homostructure in gallium nitride nanowires. Cathodoluminescence was used to quantitatively measure the wurtzite and zinc-blende band gaps. High-resolution transmission electron microscopy was used to identify distinct wurtzite and zinc-blende crystalline phases within single nanowires through the use of selected area electron diffraction, electron dispersive spectroscopy, electron energy loss spectroscopy, and fast Fourier transform techniques. A mechanism for growth is identified.

Electronic and structural characteristics of zinc-blende wurtzite biphasic homostructure GaN nanowires.

PubMed

Jacobs, Benjamin W; Ayres, Virginia M; Petkov, Mihail P; Halpern, Joshua B; He, Maoqi; Baczewski, Andrew D; McElroy, Kaylee; Crimp, Martin A; Zhang, Jiaming; Shaw, Harry C

2007-05-01

We report a new biphasic crystalline wurtzite/zinc-blende homostructure in gallium nitride nanowires. Cathodoluminescence was used to quantitatively measure the wurtzite and zinc-blende band gaps. High-resolution transmission electron microscopy was used to identify distinct wurtzite and zinc-blende crystalline phases within single nanowires through the use of selected area electron diffraction, electron dispersive spectroscopy, electron energy loss spectroscopy, and fast Fourier transform techniques. A mechanism for growth is identified.

Synthesis of chitosan supported palladium nanoparticles and its catalytic activity towards 2-nitrophenol reduction

NASA Astrophysics Data System (ADS)

Dhanavel, S.; Nivethaa, E. A. K.; Esther, G.; Narayanan, V.; Stephen, A.

2016-05-01

Chitosan supported Palladium nanoparticles were synthesized by a simple cost effective chemical reduction method using NaBH4. The prepared nanocomposite was characterized by X-Ray diffraction analysis, FESEM and Energy dispersive spectroscopy analysis of X-rays (EDAX). The catalytic performance of the nanocomposite was evaluated on the reduction of 2-Nitrophenol to the 2-Amino phenol with rate constant 1.08 × 10-3 S-1 by NaBH4 using Spectrophotometer.

In situ strain profiling of elastoplastic bending in Ti-6Al-4V alloy by synchrotron energy dispersive x-ray diffraction

DOE Office of Scientific and Technical Information (OSTI.GOV)

Croft, M.; National Synchrotron Light Source, Brookhaven National Laboratory, Upton, New York 11973; Shukla, V.

Elastic and plastic strain evolution under four-point bending has been studied by synchrotron energy dispersive x-ray diffraction. Measured strain profiles across the specimen thickness showed an increasing linear elastic strain gradient under increasing four-point bending load up to approx2 kN. The bulk elastic modulus of Ti-6Al-4V was determined as 118 GPa. The onset of plastic deformation was found to set in at a total in-plane strain of approx0.008, both under tension and compression. Plastic deformation under bending is initiated in the vicinity of the surface and at a stress of 1100 MPa, and propagates inward, while a finite core regionmore » remains elastically deformed up to 3.67 kN loading. The onset of the plastic regime and the plastic regime itself has been verified by monitoring the line broadening of the (100) peak of alpha-Ti. The effective compression/tension stress-strain curve has been obtained from the scaling collapse of strain profile data taken at seven external load levels. A similar multiple load scaling collapse of the plastic strain variation has also been obtained. The level of precision in strain measurement reported herein was evaluated and found to be 1.5x10{sup -5} or better.« less

Hair treatment process providing dispersed colors by light diffraction

DOEpatents

Sutton, Richard Matthew Charles; Lamartine, Bruce Carvell; Orler, E. Bruce; Song, Shuangqi

2015-12-22

A hair treatment process for providing dispersed colors by light diffraction including (a) coating the hair with a material comprising a polymer, (b) pressing the hair with a pressing device including one or more surfaces, and (c) forming a secondary nanostructured surface pattern on the hair that is complementary to the primary nanostructured surface pattern on the one or more surfaces of the pressing device. The secondary nanostructured surface pattern diffracts light into dispersed colors that are visible on the hair. The section of the hair is pressed with the pressing device for from about 1 to 55 seconds. The polymer has a glass transition temperature from about 55.degree. C. to about 90.degree. C. The one or more surfaces include a primary nanostructured surface pattern.

I12: the Joint Engineering, Environment and Processing (JEEP) beamline at Diamond Light Source.

PubMed

Drakopoulos, Michael; Connolley, Thomas; Reinhard, Christina; Atwood, Robert; Magdysyuk, Oxana; Vo, Nghia; Hart, Michael; Connor, Leigh; Humphreys, Bob; Howell, George; Davies, Steve; Hill, Tim; Wilkin, Guy; Pedersen, Ulrik; Foster, Andrew; De Maio, Nicoletta; Basham, Mark; Yuan, Fajin; Wanelik, Kaz

2015-05-01

I12 is the Joint Engineering, Environmental and Processing (JEEP) beamline, constructed during Phase II of the Diamond Light Source. I12 is located on a short (5 m) straight section of the Diamond storage ring and uses a 4.2 T superconducting wiggler to provide polychromatic and monochromatic X-rays in the energy range 50-150 keV. The beam energy enables good penetration through large or dense samples, combined with a large beam size (1 mrad horizontally × 0.3 mrad vertically). The beam characteristics permit the study of materials and processes inside environmental chambers without unacceptable attenuation of the beam and without the need to use sample sizes which are atypically small for the process under study. X-ray techniques available to users are radiography, tomography, energy-dispersive diffraction, monochromatic and white-beam two-dimensional diffraction/scattering and small-angle X-ray scattering. Since commencing operations in November 2009, I12 has established a broad user community in materials science and processing, chemical processing, biomedical engineering, civil engineering, environmental science, palaeontology and physics.

I12: the Joint Engineering, Environment and Processing (JEEP) beamline at Diamond Light Source

PubMed Central

Drakopoulos, Michael; Connolley, Thomas; Reinhard, Christina; Atwood, Robert; Magdysyuk, Oxana; Vo, Nghia; Hart, Michael; Connor, Leigh; Humphreys, Bob; Howell, George; Davies, Steve; Hill, Tim; Wilkin, Guy; Pedersen, Ulrik; Foster, Andrew; De Maio, Nicoletta; Basham, Mark; Yuan, Fajin; Wanelik, Kaz

2015-01-01

I12 is the Joint Engineering, Environmental and Processing (JEEP) beamline, constructed during Phase II of the Diamond Light Source. I12 is located on a short (5 m) straight section of the Diamond storage ring and uses a 4.2 T superconducting wiggler to provide polychromatic and monochromatic X-rays in the energy range 50–150 keV. The beam energy enables good penetration through large or dense samples, combined with a large beam size (1 mrad horizontally × 0.3 mrad vertically). The beam characteristics permit the study of materials and processes inside environmental chambers without unacceptable attenuation of the beam and without the need to use sample sizes which are atypically small for the process under study. X-ray techniques available to users are radiography, tomography, energy-dispersive diffraction, monochromatic and white-beam two-dimensional diffraction/scattering and small-angle X-ray scattering. Since commencing operations in November 2009, I12 has established a broad user community in materials science and processing, chemical processing, biomedical engineering, civil engineering, environmental science, palaeontology and physics. PMID:25931103

Investigation of high-energy ion-irradiated MA957 using synchrotron radiation under in-situ tension

DOE PAGES

Mo, Kun; Yun, Di; Miao, Yinbin; ...

2016-01-02

In this paper, an MA957 oxide dispersion-strengthened (ODS) alloy was irradiated with high-energy ions in the Argonne Tandem Linac Accelerator System. Fe ions at an energy of 84 MeV bombarded MA957 tensile specimens, creating a damage region similar to 7.5 μm in depth; the peak damage (similar to 40 dpa) was estimated to be at similar to 7 μm from the surface. Following the irradiation, in-situ high-energy X-ray diffraction measurements were performed at the Advanced Photon Source in order to study the dynamic deformation behavior of the specimens after ion irradiation damage. In-situ X-ray measurements taken during tensile testing ofmore » the ion-irradiated MA957 revealed a difference in loading behavior between the irradiated and un-irradiated regions of the specimen. At equivalent applied stresses, lower lattice strains were found in the radiation-damaged region than those in the un-irradiated region. This might be associated with a higher level of Type II stresses as a result of radiation hardening. The study has demonstrated the feasibility of combining high-energy ion radiation and high-energy synchrotron X-ray diffraction to study materials' radiation damage in a dynamic manner.« less

Synthesis and dielectric properties of zinc oxide nanoparticles using a biotemplate

DOE Office of Scientific and Technical Information (OSTI.GOV)

P, Sharmila P, E-mail: sharmilavishram@gmail.com; Tharayil, Nisha J., E-mail: nishajohntharayil@gmail.com

Zinc Oxide nanoparticles are synthesized using DNA as capping agent. Zinc oxide nanoparticles are synthesized using DNA as a capping agent. Structural and morphological characterizations are done using SEM, FTIR and XRD. The particle size and lattice parameters are calculated from the diffraction data. The optical properties are studied using UV-Vis absorption spectroscopy and bandgap variation with temperature is determined. The dielectric property of nanoparticles is studied by varying temperature and frequency. The dielectric constant and dispersion parameters are found out. Method of Cole-Cole analysis is used to study the high temperature dispersion of relaxation time. The variation of bothmore » AC and DC conductivity are studied and activation energy calculated.« less

Biosynthesis and characterization of silver nanoparticles prepared from two novel natural precursors by facile thermal decomposition methods

NASA Astrophysics Data System (ADS)

Goudarzi, Mojgan; Mir, Noshin; Mousavi-Kamazani, Mehdi; Bagheri, Samira; Salavati-Niasari, Masoud

2016-09-01

In this work, two natural sources, including pomegranate peel extract and cochineal dye were employed for the synthesis of silver nanoparticles. The natural silver complex from pomegranate peel extract resulted in nano-sized structures through solution-phase method, but this method was not efficient for cochineal dye-silver precursor and the as-formed products were highly agglomerated. Therefore, an alternative facile solid-state approach was investigated as for both natural precursors and the results showed successful production of well-dispersed nanoparticles with narrow size distribution for cochineal dye-silver precursor. The products were characterized by X-ray diffraction (XRD), Scanning Electron Microscopy (SEM), Energy dispersive X-ray microanalysis (EDX), and Transmission Electron Microscopy (TEM).

Radiation attenuation by single-crystal diamond windows

DOE Office of Scientific and Technical Information (OSTI.GOV)

Guthrie, M.; Pruteanu, C. G.; Donnelly, M. -E.

As artificial diamond becomes more cost effective it is likely to see increasing use as a window for sample environment equipment used in diffraction experiments. Such windows are particularly useful as they exhibit exceptional mechanical properties in addition to being highly transparent to both X-ray and neutron radiation. A key application is in high-pressure studies, where diamond anvil cells (DACs) are used to access extreme sample conditions. However, despite their utility, an important consideration when using single-crystal diamond windows is their interaction with the incident beam. In particular, the Bragg condition will be satisfied for specific angles and wavelengths, leadingmore » to the appearance of diamond Bragg spots on the diffraction detectors but also, unavoidably, to loss of transmitted intensity of the beam that interacts with the sample. This effect can be particularly significant for energy-dispersive measurements, for example, in time-of-flight neutron diffraction work using DACs. This article presents a semi-empirical approach that can be used to correct for this effect, which is a prerequisite for the accurate determination of diffraction intensities.« less

Radiation attenuation by single-crystal diamond windows

DOE Office of Scientific and Technical Information (OSTI.GOV)

Guthrie, Malcolm; Pruteanu, Ciprian G.; Donnelly, Mary -Ellen

As artificial diamond becomes more cost effective it is likely to see increasing use as a window for sample environment equipment used in diffraction experiments. Such windows are particularly useful as they exhibit exceptional mechanical properties in addition to being highly transparent to both X-ray and neutron radiation. A key application is in high-pressure studies, where diamond anvil cells (DACs) are used to access extreme sample conditions. However, despite their utility, an important consideration when using single-crystal diamond windows is their interaction with the incident beam. In particular, the Bragg condition will be satisfied for specific angles and wavelengths, leadingmore » to the appearance of diamond Bragg spots on the diffraction detectors but also, unavoidably, to loss of transmitted intensity of the beam that interacts with the sample. This effect can be particularly significant for energy-dispersive measurements, for example, in time-of-flight neutron diffraction work using DACs. Furthermore, this article presents a semi-empirical approach that can be used to correct for this effect, which is a prerequisite for the accurate determination of diffraction intensities.« less

Radiation attenuation by single-crystal diamond windows

DOE PAGES

Guthrie, Malcolm; Pruteanu, Ciprian G.; Donnelly, Mary -Ellen; ...

2017-02-01

As artificial diamond becomes more cost effective it is likely to see increasing use as a window for sample environment equipment used in diffraction experiments. Such windows are particularly useful as they exhibit exceptional mechanical properties in addition to being highly transparent to both X-ray and neutron radiation. A key application is in high-pressure studies, where diamond anvil cells (DACs) are used to access extreme sample conditions. However, despite their utility, an important consideration when using single-crystal diamond windows is their interaction with the incident beam. In particular, the Bragg condition will be satisfied for specific angles and wavelengths, leadingmore » to the appearance of diamond Bragg spots on the diffraction detectors but also, unavoidably, to loss of transmitted intensity of the beam that interacts with the sample. This effect can be particularly significant for energy-dispersive measurements, for example, in time-of-flight neutron diffraction work using DACs. Furthermore, this article presents a semi-empirical approach that can be used to correct for this effect, which is a prerequisite for the accurate determination of diffraction intensities.« less

Linear Fresnel Spectrometer Chip with Gradient Line Grating

NASA Technical Reports Server (NTRS)

Choi, Sang Hyouk (Inventor); Park, Yeonjoon (Inventor)

2015-01-01

A spectrometer that includes a grating that disperses light via Fresnel diffraction according to wavelength onto a sensing area that coincides with an optical axis plane of the grating. The sensing area detects the dispersed light and measures the light intensity associated with each wavelength of the light. Because the spectrometer utilizes Fresnel diffraction, it can be miniaturized and packaged as an integrated circuit.

Fusion processing of itraconazole solid dispersions by kinetisol dispersing: a comparative study to hot melt extrusion.

PubMed

DiNunzio, James C; Brough, Chris; Miller, Dave A; Williams, Robert O; McGinity, James W

2010-03-01

KinetiSol Dispersing (KSD) is a novel high energy manufacturing process investigated here for the production of pharmaceutical solid dispersions. Solid dispersions of itraconazole (ITZ) and hypromellose were produced by KSD and compared to identical formulations produced by hot melt extrusion (HME). Materials were characterized for solid state properties by modulated differential scanning calorimetry and X-ray diffraction. Dissolution behavior was studied under supersaturated conditions. Oral bioavailability was determined using a Sprague-Dawley rat model. Results showed that KSD was able to produce amorphous solid dispersions in under 15 s while production by HME required over 300 s. Dispersions produced by KSD exhibited single phase solid state behavior indicated by a single glass transition temperature (T(g)) whereas compositions produced by HME exhibited two T(g)s. Increased dissolution rates for compositions manufactured by KSD were also observed compared to HME processed material. Near complete supersaturation was observed for solid dispersions produced by either manufacturing processes. Oral bioavailability from both processes showed enhanced AUC compared to crystalline ITZ. Based on the results presented from this study, KSD was shown to be a viable manufacturing process for the production of pharmaceutical solid dispersions, providing benefits over conventional techniques including: enhanced mixing for improved homogeneity and reduced processing times. 2009 Wiley-Liss, Inc. and the American Pharmacists Association

Novel diffraction gratings for next generation spectrographs with high spectral dispersion

NASA Astrophysics Data System (ADS)

Ebizuka, N.; Okamoto, T.; Hosobata, T.; Yamagata, Y.; Sasaki, M.; Uomoto, M.; Shimatsu, T.; Sato, S.; Hashimoto, N.; Tanaka, I.; Hattori, T.; Ozaki, S.; Aoki, W.

2016-07-01

As a transmission grating, a surface-relief (SR) grating with sawtooth shaped ridges and volume phase holographic (VPH) grating are widely used for instruments of astronomical observations. However the SR grating is difficult to achieve high diffraction efficiency at high angular dispersion, and the VPH grating has low diffraction efficiency in high diffraction orders. We propose novel gratings that solve these problems. We introduce the hybrid grism which combines a high refractive index prism with a replicated transmission grating, which has sawtooth shaped ridges of an acute apex angle. The birefringence VPH (B-VPH) grating which contains an anisotropic medium, such as a liquid crystal, achieves diffraction efficiency up to 100% at the first diffraction order for natural polarization and for circular polarization. The quasi-Bragg (QB) grating which consists of long rectangular mirrors aligned in parallel precisely, like a window blind, achieves diffraction efficiency of 60% or more in higher than the 4th diffraction order. The volume binary (VB) grating with narrow grooves also achieves diffraction efficiency of 60% or more in higher than the 6th diffraction order. The reflector facet transmission (RFT) grating which is a SR grating with sawtooth shaped ridges of an acute apex angle achieves diffraction efficiency up to 80% in higher than the 4th diffraction order.

A simple and low temperature process for super-hydrophilic rutile TiO 2 thin films growth

NASA Astrophysics Data System (ADS)

Mane, R. S.; Joo, Oh-Shim; Min, Sun-Ki; Lokhande, C. D.; Han, Sung-Hwan

2006-11-01

We investigate an environmentally friendly aqueous solution system for rutile TiO2 violet color nanocrystalline thin films growth on ITO substrate at room temperature. Film shows considerable absorption in visible region with excitonic maxima at 434 nm. X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), selected area electron diffraction (SAED), UV-vis, water surface contact angle and energy dispersive X-ray analysis (EDX) techniques in addition to actual photo-image that shows purely rutile phase of TiO2 with violet color, super-hydrophilic and densely packed nanometer-sized spherical grains of approximate diameter 3.15 ± 0.4 nm, characterize the films. Band gap energy of 4.61 eV for direct transition was obtained for the rutile TiO2 films. Film surface shows super-hydrophilic behavior, as exhibited water contact angle was 7°. Strong visible absorption (not due to chlorine) leaves future challenge to use these films in extremely thin absorber (ETA) solar cells.

Development of graphite/copper composites utilizing engineered interfaces. M.S. Thesis Final Report

NASA Technical Reports Server (NTRS)

Devincent, Sandra M.

1991-01-01

In situ measurements of graphite/copper alloy contact angles were made using the sessile drop method. The interfacial energy values obtained from these measurements were then applied to a model for the fiber matrix interfacial debonding phenomenon found in graphite/copper composites. The formation obtained from the sessile drop tests led to the development of a copper alloy that suitably wets graphite. Characterization of graphite/copper alloy interfaces subjected to elevated temperatures was conducted using Scanning Electron Microscopy, Energy Dispersive Spectroscopy, Auger Electron Spectroscopy, and X Ray Diffraction analyses. These analyses indicated that during sessile drop tests conducted at 1130 C for 1 hour, copper alloys containing greater than 0.98 at pct chromium form continuous reaction layers of approx. 10 microns in thickness. The reaction layers are adherent to the graphite surface. The copper wets the reaction layer to form a contact angle of 60 deg or less. X ray diffraction results indicate that the reaction layer is Cr3C2.

Synthesis and characterization of single-crystalline zinc tin oxide nanowires

NASA Astrophysics Data System (ADS)

Shi, Jen-Bin; Wu, Po-Feng; Lin, Hsien-Sheng; Lin, Ya-Ting; Lee, Hsuan-Wei; Kao, Chia-Tze; Liao, Wei-Hsiang; Young, San-Lin

2014-05-01

Crystalline zinc tin oxide (ZTO; zinc oxide with heavy tin doping of 33 at.%) nanowires were first synthesized using the electrodeposition and heat treatment method based on an anodic aluminum oxide (AAO) membrane, which has an average diameter of about 60 nm. According to the field emission scanning electron microscopy (FE-SEM) results, the synthesized ZTO nanowires are highly ordered and have high wire packing densities. The length of ZTO nanowires is about 4 μm, and the aspect ratio is around 67. ZTO nanowires with a Zn/(Zn + Sn) atomic ratio of 0.67 (approximately 2/3) were observed from an energy dispersive spectrometer (EDS). X-ray diffraction (XRD) and corresponding selected area electron diffraction (SAED) patterns demonstrated that the ZTO nanowire is hexagonal single-crystalline. The study of ultraviolet/visible/near-infrared (UV/Vis/NIR) absorption showed that the ZTO nanowire is a wide-band semiconductor with a band gap energy of 3.7 eV.

Synthesis and characterization of single-crystalline zinc tin oxide nanowires.

PubMed

Shi, Jen-Bin; Wu, Po-Feng; Lin, Hsien-Sheng; Lin, Ya-Ting; Lee, Hsuan-Wei; Kao, Chia-Tze; Liao, Wei-Hsiang; Young, San-Lin

2014-01-01

Crystalline zinc tin oxide (ZTO; zinc oxide with heavy tin doping of 33 at.%) nanowires were first synthesized using the electrodeposition and heat treatment method based on an anodic aluminum oxide (AAO) membrane, which has an average diameter of about 60 nm. According to the field emission scanning electron microscopy (FE-SEM) results, the synthesized ZTO nanowires are highly ordered and have high wire packing densities. The length of ZTO nanowires is about 4 μm, and the aspect ratio is around 67. ZTO nanowires with a Zn/(Zn + Sn) atomic ratio of 0.67 (approximately 2/3) were observed from an energy dispersive spectrometer (EDS). X-ray diffraction (XRD) and corresponding selected area electron diffraction (SAED) patterns demonstrated that the ZTO nanowire is hexagonal single-crystalline. The study of ultraviolet/visible/near-infrared (UV/Vis/NIR) absorption showed that the ZTO nanowire is a wide-band semiconductor with a band gap energy of 3.7 eV.

Melioration of Optical and Electrical Performance of Ga-N Codoped ZnO Thin Films

NASA Astrophysics Data System (ADS)

Narayanan, Nripasree; Deepak, N. K.

2018-06-01

Transparent and conducting p-type zinc oxide (ZnO) thin films doped with gallium (Ga) and nitrogen (N) simultaneously were deposited on glass substrates by spray pyrolysis technique. Phase composition analysis by X-ray diffraction confirmed the polycrystallinity of the films with pure ZnO phase. Energy dispersive X-ray analysis showed excellent incorporation of N in the ZnO matrix by means of codoping. The optical transmittance of N monodoped film was poor but got improved with Ga-N codoping and also resulted in the enhancement of optical energy gap. Hole concentration increased with codoping and consequently, lower resistivity and high stability were obtained.

Theoretical description and design of nanomaterial slab waveguides: application to compensation of optical diffraction.

PubMed

Kivijärvi, Ville; Nyman, Markus; Shevchenko, Andriy; Kaivola, Matti

2018-04-02

Planar optical waveguides made of designable spatially dispersive nanomaterials can offer new capabilities for nanophotonic components. As an example, a thin slab waveguide can be designed to compensate for optical diffraction and provide divergence-free propagation for strongly focused optical beams. Optical signals in such waveguides can be transferred in narrow channels formed by the light itself. We introduce here a theoretical method for characterization and design of nanostructured waveguides taking into account their inherent spatial dispersion and anisotropy. Using the method, we design a diffraction-compensating slab waveguide that contains only a single layer of silver nanorods. The waveguide shows low propagation loss and broadband diffraction compensation, potentially allowing transfer of optical information at a THz rate.

Hardness of pulsed electric current sintered and hot isostatically pressed Mo(Si,Al)2

NASA Astrophysics Data System (ADS)

Tanabe, Jun

2005-05-01

We improved the reactivity and mechanical characteristics of Mo(Si,Al)2 by pulsed electric current sintering (PECS) and hot isostatic pressing (HIP), and evaluated its reaction state and mechanical characteristics using energy dispersive spectroscopy (EDS), X-ray diffraction, and a hardness test. Mo(Si,Al)2 was generated by pretreatment using a furnace, and the application of the PECS and HIP treatments further densified the sintered body, resulting in an increase in the hardness.

Spray CVD for Making Solar-Cell Absorber Layers

NASA Technical Reports Server (NTRS)

Banger, Kulbinder K.; Harris, Jerry; Jin, Michael H.; Hepp, Aloysius

2007-01-01

Spray chemical vapor deposition (spray CVD) processes of a special type have been investigated for use in making CuInS2 absorber layers of thin-film solar photovoltaic cells from either of two subclasses of precursor compounds: [(PBu3) 2Cu(SEt)2In(SEt)2] or [(PPh3)2Cu(SEt)2 In(SEt)2]. The CuInS2 films produced in the experiments have been characterized by x-ray diffraction, scanning electron microscopy, energy-dispersive spectroscopy, and four-point-probe electrical tests.

Synthesis of samarium doped gadolinium oxide nanorods, its spectroscopic and physical properties

NASA Astrophysics Data System (ADS)

Boopathi, G.; Gokul Raj, S.; Ramesh Kumar, G.; Mohan, R.; Mohan, S.

2018-06-01

One-dimensional samarium doped gadolinium oxide [Sm:Gd2O3] nanorods have been synthesized successfully through co-precipitation technique in aqueous solution. The as-synthesized and calcined products were characterized by using powder X-ray diffraction pattern, Fourier transform Raman spectroscopy, thermogravimetric/differential thermal analysis, scanning electron microscopy with energy-dispersive X-ray analysis, transmission electron microscopy, Fourier transform infrared spectroscopy, Ultraviolet-Visible spectrometry, photoluminescence spectrophotometer and X-ray photoelectron spectroscopy techniques. The obtained results are discussed in detailed manner.

Synthesis of Polycrystalline CdSiP2 in a Gradient Temperature Field

NASA Astrophysics Data System (ADS)

Bereznaya, S. A.; Korotchenko, Z. V.; Kurasova, A. S.; Sarkisov, S. Yu.; Sarkisov, Yu. S.; Chernyshov, A. I.; Korolkov, I. V.; Kuchumov, B. M.; Saprykin, A. I.; Atuchin, V. V.

2018-05-01

A procedure for the synthesis of a CdSiP2 compound from the initial elementary components in a gradient thermal field has been developed. The phase and chemical composition of the synthesized and recrystallized material is confirmed by the data of X-ray diffraction analysis and scanning electron microscopy with an energy-dispersive system. The polycrystalline material obtained by the developed method will be used to grow bulk nonlinear optical CdSiP2 crystals.

Room-temperature synthesis and photoluminescence of hexagonal CePO4 nanorods

NASA Astrophysics Data System (ADS)

Zhu, J.; Zhang, K.; Zhao, H. Y.

2018-01-01

Hexagonal CePO4 nanorods were synthesized via a simple chemical precipitation route at room-temperature without the presence of surfactants and then characterized by powder X-ray diffraction (XRD), energy-dispersive X-ray (EDX) spectrometry, scanning electron microscopy (SEM), transmission electron microscopy (TEM), ultraviolet-visible (UV-vis) absorption and photoluminescence (PL) spectroscopy. Hexagonal CePO4 nanorods exhibit strong ultraviolet absorption and ultraviolet luminescence, which correspond to the electronic transitions between 4f and 5d state of Ce3+ ions.

Pressure-induced phase transition in GaN nanocrystals

NASA Astrophysics Data System (ADS)

Cui, Q.; Pan, Y.; Zhang, W.; Wang, X.; Zhang, J.; Cui, T.; Xie, Y.; Liu, J.; Zou, G.

2002-11-01

High-pressure in situ energy-dispersive x-ray diffraction experiments on GaN nanocrystals with 50 nm diameter have been carried out using a synchrotron x-ray source and a diamond-anvil cell up to about 79 GPa at room temperature. A pressure-induced first-order structural phase transition from the wurtzite-type structure to the rock-salt-type structure starts at about 48.8 GPa. The rock-salt-type phase persists to the highest pressure in our experimental range.

Mineralogy of chondritic interplanetary dust particle impact residues from LDEF

NASA Technical Reports Server (NTRS)

Barrett, R. A.; Zolensky, M. E.; Bernhard, R.

1993-01-01

A detailed structural and compositional analysis of several impactor residues was performed utilizing transmission electron microscopy, energy dispersive spectroscopy, and electron diffraction. Residues from the interior of several craters in gold surfaces were removed with a tungsten needle, mounted in EMBED-812 epoxy, and ultramicrotomed. The presence in these residues of equilibrated ferromagnesian minerals, recrystallization textures, glass, and melted metal and sulfide bodies decorating grain boundaries is indicative of varying degrees of shock metamorphism in all impact residues we have characterized.

Physicochemical characterization of tacrolimus-loaded solid dispersion with sodium carboxylmethyl cellulose and sodium lauryl sulfate.

PubMed

Park, Young-Joon; Ryu, Dong-Sung; Li, Dong Xun; Quan, Qi Zhe; Oh, Dong Hoon; Kim, Jong Oh; Seo, Youn Gee; Lee, Young-Im; Yong, Chul Soon; Woo, Jong Soo; Choi, Han-Gon

2009-06-01

To develop a novel tacrolimus-loaded solid dispersion with improved solubility, various solid dispersions were prepared with various ratios of water, sodium lauryl sulfate, citric acid and carboxylmethylcellulose-Na using spray drying technique. The physicochemical properties of solid dispersions were investigated using scanning electron microscopy, differential scanning calorimetery and powder X-ray diffraction. Furthermore, their solubility and dissolution were evaluated compared to drug powder. The solid dispersion at the tacrolimus/CMC-Na/sodium lauryl sulfate/citric acid ratio of 3/24/3/0.2 significantly improved the drug solubility and dissolution compared to powder. The scanning electron microscopy result suggested that carriers might be attached to the surface of drug in this solid dispersion. Unlike traditional solid dispersion systems, the crystal form of drug in this solid dispersion could not be converted to amorphous form, which was confirmed by the analysis of DSC and powder X-ray diffraction. Thus, the solid dispersion system with water, sodium lauryl sulfate, citric acid and CMC-Na should be a potential candidate for delivering a poorly water-soluble tacrolimus with enhanced solubility and no convertible crystalline.

One-Dimensional Photonic Crystal Superprisms

NASA Technical Reports Server (NTRS)

Ting, David

2005-01-01

Theoretical calculations indicate that it should be possible for one-dimensional (1D) photonic crystals (see figure) to exhibit giant dispersions known as the superprism effect. Previously, three-dimensional (3D) photonic crystal superprisms have demonstrated strong wavelength dispersion - about 500 times that of conventional prisms and diffraction gratings. Unlike diffraction gratings, superprisms do not exhibit zero-order transmission or higher-order diffraction, thereby eliminating cross-talk problems. However, the fabrication of these 3D photonic crystals requires complex electron-beam substrate patterning and multilayer thin-film sputtering processes. The proposed 1D superprism is much simpler in structural complexity and, therefore, easier to design and fabricate. Like their 3D counterparts, the 1D superprisms can exhibit giant dispersions over small spectral bands that can be tailored by judicious structure design and tuned by varying incident beam direction. Potential applications include miniature gas-sensing devices.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Prakash, Deo; Shaaban, E.R., E-mail: esam_ramadan2008@yahoo.com; Shapaan, M.

Highlights: • Combined experimental and theoretical researches on ZnSe Thin Films. • The film thickness and refractive index were determined using envelope method. • The absorption coefficient and the energy gap were calculated. • Dispersion parameters were determined using Wemple-DiDomenico relation. • The third order susceptibility and nonlinear refractive index were calculated. - Abstract: Zinc selenide (ZnSe) thin films with different thicknesses were evaporated onto glass substrates using the thermal evaporation technique. X-ray diffraction analysis confirmed that both the film and powder have cubic zinc-blende structure. The fundamental optical parameters like absorption coefficient, extinction coefficient and band gap were evaluatedmore » in transparent region of transmittance and reflectance spectrum. The optical transition of the films was found to be allowed, where the energy gap increased from 2.576 to 2.702 eV with increasing film thickness. Also, the refractive index value increase with increasing film thickness. The refractive indices evaluated through envelope method were extrapolated by Cauchy dispersion relationship over the whole spectra range. Additionally, the dispersion of refractive index was determined in terms of Wemple-DiDomenico single oscillator model. Third order susceptibility and nonlinear refractive index were determined for different thickness of ZnSe thin films.« less

Following the electroreduction of uranium dioxide to uranium in LiCl-KCl eutectic in situ using synchrotron radiation

NASA Astrophysics Data System (ADS)

Brown, L. D.; Abdulaziz, R.; Jervis, R.; Bharath, V. J.; Atwood, R. C.; Reinhard, C.; Connor, L. D.; Simons, S. J. R.; Inman, D.; Brett, D. J. L.; Shearing, P. R.

2015-09-01

The electrochemical reduction of uranium dioxide to metallic uranium has been investigated in lithium chloride-potassium chloride eutectic molten salt. Laboratory based electrochemical studies have been coupled with in situ energy dispersive X-ray diffraction, for the first time, to deduce the reduction pathway. No intermediate phases were identified using the X-ray diffraction before, during or after electroreduction to form α-uranium. This suggests that the electrochemical reduction occurs via a single, 4-electron-step, process. The rate of formation of α-uranium is seen to decrease during electrolysis and could be a result of a build-up of oxygen anions in the molten salt. Slow transport of O2- ions away from the UO2 working electrode could impede the electrochemical reduction.

Nanobelt formation of magnesium hydroxide sulfate hydrate via a soft chemistry process.

PubMed

Zhou, Zhengzhi; Sun, Qunhui; Hu, Zeshan; Deng, Yulin

2006-07-13

The nanobelt formation of magnesium hydroxide sulfate hydrate (MHSH) via a soft chemistry approach using carbonate salt and magnesium sulfate as reactants was successfully demonstrated. X-ray diffraction (XRD), energy dispersion X-ray spectra (EDS), selected area electron diffraction (SAED), scanning electron microscopy (SEM), and transmission electron microscopy (TEM) analysis revealed that the MHSH nanobelts possessed a thin belt structure (approximately 50 nm in thickness) and a rectangular cross profile (approximately 200 nm in width). The MHSH nanobelts suffered decomposition under electron beam irradiation during TEM observation and formed MgO with the pristine nanobelt morphology preserved. The formation process of the MHSH nanobelts was studied by tracking the morphology of the MHSH nanobelts during the reaction. A possible chemical reaction mechanism is proposed.

Phase transformations and equation of state of praseodymium metal to 103 GPa

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chesnut, Gary N.; Vohra, Yogesh K.

2000-08-01

Pressure-induced structural phase transformations in a trivalent rare-earth metal praseodymium (Pr) were studied at room temperature in a diamond anvil cell to 103 GPa by energy dispersive x-ray diffraction using a synchrotron source. Our x-ray diffraction studies document the following crystal structure sequence: dhcp{yields}fcc{yields}distorted fcc(hR24 type){yields}monoclinic(C2/m){yields}{alpha}-uranium with increasing pressure. We measure a 16.7% volume collapse at the transition to the {alpha}-uranium phase at 20 GPa. The high-pressure {alpha}-uranium phase in Pr was found to be stable to the highest pressure of 103 GPa, which corresponds to a volume compression V/V{sub 0}=0.407. (c) 2000 The American Physical Society.

A fiber-compatible spectrally encoded imaging system using a 45° tilted fiber grating

NASA Astrophysics Data System (ADS)

Wang, Guoqing; Wang, Chao; Yan, Zhijun; Zhang, Lin

2016-04-01

We propose and demonstrate, for the first time to our best knowledge, the use of a 45° tilted fiber grating (TFG) as an infiber lateral diffraction element in an efficient and fiber-compatible spectrally encoded imaging (SEI) system. Under proper polarization control, the TFG has significantly enhanced diffraction efficiency (93.5%) due to strong tilted reflection. Our conceptually new fiber-topics-based design eliminates the need for bulky and lossy free-space diffraction gratings, significantly reduces the volume and cost of the imaging system, improves energy efficiency, and increases system stability. As a proof-of-principle experiment, we use the proposed system to perform an one dimensional (1D) line scan imaging of a customer-designed three-slot sample and the results show that the constructed image matches well with the actual sample. The angular dispersion of the 45° TFG is measured to be 0.054°/nm and the lateral resolution of the SEI system is measured to be 28 μm in our experiment.

Microstructural evolution and grain growth kinetics of GZ31 magnesium alloy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Roostaei, M., E-mail: miladroustaei68@ut.ac.ir

2016-08-15

Grain growth behavior of Mg–3Gd–1Zn (GZ31) magnesium alloy was studied in a wide range of annealing time and temperature to clarify the kinetics of grain growth, microstructural evolution and related metallurgical phenomena. This material exhibited typical normal grain growth mode under annealing conditions with annealing temperature of lower than 300 °C and soaking time of lower than 240 min. However, the abnormality in grain growth was also evident at annealing temperature of 400 °C and 500 °C. The dependence of abnormal grain growth (AGG) at mentioned annealing temperatures upon microstructural features such as dispersed precipitates, which were rich in Znmore » and Gd, was investigated by optical micrographs, X-ray diffraction patterns, scanning electron microscopy images, and energy dispersive X-ray analysis spectra. The bimodality in grain-size distribution histograms also signified the occurrence of AGG. Based on the experimental data on grain growth obtained by annealing treatments, the grain growth exponent and the activation energy were also figured out.« less

Ellipsometric analysis and optical absorption characterization of gallium phosphide nanoparticulate thin film

NASA Astrophysics Data System (ADS)

Zhang, Qi-Xian; Wei, Wen-Sheng; Ruan, Fang-Ping

2011-04-01

Gallium phosphide (GaP) nanoparticulate thin films were easily fabricated by colloidal suspension deposition via GaP nanoparticles dispersed in N,N-dimethylformamide. The microstructure of the film was performed by x-ray diffraction, high resolution transmission electron microscopy and field emission scanning electron microscopy. The film was further investigated by spectroscopic ellipsometry. After the model GaP+void|SiO2 was built and an effective medium approximation was adopted, the values of the refractive index n and the extinction coefficient k were calculated for the energy range of 0.75 eV-4.0 eV using the dispersion formula in DeltaPsi2 software. The absorption coefficient of the film was calculated from its k and its energy gaps were further estimated according to the Tauc equation, which were further verified by its fluorescence spectrum measurement. The structure and optical absorption properties of the nanoparticulate films are promising for their potential applications in hybrid solar cells.

Nanostructured Boron Nitride With High Water Dispersibility For Boron Neutron Capture Therapy

PubMed Central

Singh, Bikramjeet; Kaur, Gurpreet; Singh, Paviter; Singh, Kulwinder; Kumar, Baban; Vij, Ankush; Kumar, Manjeet; Bala, Rajni; Meena, Ramovatar; Singh, Ajay; Thakur, Anup; Kumar, Akshay

2016-01-01

Highly water dispersible boron based compounds are innovative and advanced materials which can be used in Boron Neutron Capture Therapy for cancer treatment (BNCT). Present study deals with the synthesis of highly water dispersible nanostructured Boron Nitride (BN). Unique and relatively low temperature synthesis route is the soul of present study. The morphological examinations (Scanning/transmission electron microscopy) of synthesized nanostructures showed that they are in transient phase from two dimensional hexagonal sheets to nanotubes. It is also supported by dual energy band gap of these materials calculated from UV- visible spectrum of the material. The theoretically calculated band gap also supports the same (calculated by virtual nano lab Software). X-ray diffraction (XRD) analysis shows that the synthesized material has deformed structure which is further supported by Raman spectroscopy. The structural aspect of high water disperse ability of BN is also studied. The ultra-high disperse ability which is a result of structural deformation make these nanostructures very useful in BNCT. Cytotoxicity studies on various cell lines (Hela(cervical cancer), human embryonic kidney (HEK-293) and human breast adenocarcinoma (MCF-7)) show that the synthesized nanostructures can be used for BNCT. PMID:27759052

Development of solid dispersions of artemisinin for transdermal delivery.

PubMed

Shahzad, Yasser; Sohail, Sadia; Arshad, Muhammad Sohail; Hussain, Talib; Shah, Syed Nisar Hussain

2013-11-30

Solid dispersions of the poorly soluble drug artemisinin were developed using polymer blends of polyvinylpyrrolidone (PVP) and polyethylene glycol (PEG) with the aim of enhancing solubility and in vitro permeation of artemisinin through skin. Formulations were characterised using a combination of molecular dynamics (MD) simulations, differential scanning calorimetry (DSC), X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FT-IR). Solubility of artemisinin was determined in two solvents: de-ionised water and phosphate buffered saline (PBS; pH 7.4), while in vitro drug permeation studies were carried out using rabbit skin as a model membrane. MD simulations revealed miscibility between the drug and polymers. DSC confirmed the molecular dispersion of the drug in the polymer blend. Decrease in crystallinity of artemisinin with respect to polymer content and the absence of specific drug-polymer interactions were confirmed using XRD and FT-IR, respectively. The solubility of artemisinin was dramatically enhanced for the solid dispersions, as was the permeation of artemisinin from saturated solid-dispersion vehicles relative to that from saturated solutions of the pure drug. The study suggests that high energy solid forms of artemisinin could possibly enable transdermal delivery of artemisinin. Copyright © 2013 Elsevier B.V. All rights reserved.

Nanostructured Boron Nitride With High Water Dispersibility For Boron Neutron Capture Therapy

NASA Astrophysics Data System (ADS)

Singh, Bikramjeet; Kaur, Gurpreet; Singh, Paviter; Singh, Kulwinder; Kumar, Baban; Vij, Ankush; Kumar, Manjeet; Bala, Rajni; Meena, Ramovatar; Singh, Ajay; Thakur, Anup; Kumar, Akshay

2016-10-01

Highly water dispersible boron based compounds are innovative and advanced materials which can be used in Boron Neutron Capture Therapy for cancer treatment (BNCT). Present study deals with the synthesis of highly water dispersible nanostructured Boron Nitride (BN). Unique and relatively low temperature synthesis route is the soul of present study. The morphological examinations (Scanning/transmission electron microscopy) of synthesized nanostructures showed that they are in transient phase from two dimensional hexagonal sheets to nanotubes. It is also supported by dual energy band gap of these materials calculated from UV- visible spectrum of the material. The theoretically calculated band gap also supports the same (calculated by virtual nano lab Software). X-ray diffraction (XRD) analysis shows that the synthesized material has deformed structure which is further supported by Raman spectroscopy. The structural aspect of high water disperse ability of BN is also studied. The ultra-high disperse ability which is a result of structural deformation make these nanostructures very useful in BNCT. Cytotoxicity studies on various cell lines (Hela(cervical cancer), human embryonic kidney (HEK-293) and human breast adenocarcinoma (MCF-7)) show that the synthesized nanostructures can be used for BNCT.

Preparation and characterization of new photoluminescent nano-powder based on Eu3+:La2Ti2O7 and dispersed into silica matrix for latent fingerprint detection

NASA Astrophysics Data System (ADS)

Saif, M.; Alsayed, N.; Mbarek, A.; El-Kemary, M.; Abdel-Mottaleb, M. S. A.

2016-12-01

Pure lanthanum titanate doped with europium metal ions (La2Ti2O7:Eu3+) and dispersed in silica matrix phosphor powder was prepared by sol-gel process followed by thermal treatment. The prepared nanophosphors were characterized by powder X-ray Diffraction (XRD), Fourier Transform Infrared (FT-IR), Transmission Electron Microscope (TEM), Energy Dispersive Spectroscopy (EDX), and Photoluminescence Spectroscopy (PL). The effects of silica, thermal treatment, Eu3+ ion, and surfactant (CTAB) concentrations on the crystal, morphology, and photoluminescence properties were investigated. The present work found that dispersion of La2Ti2O7:Eu3+ into silica matrix significantly altered the morphology of La2Ti2O7:Eu3+ from high crystalline micro-plate like shape into amorphous aggregated Nano-spherical shape. The high separated spherical shape with intense red PL emission and long lifetime was obtained from 10 mol% Eu3+:La2Ti2O7:Eu3+, dispersed into silica matrix, and prepared in the presence of CTAB. The high PL Nano-phosphor has been successfully used in developing latent fingerprint from various forensic relevant materials.

TiO2-V2O5 nanocomposites as alternative energy storage substances for photocatalysts.

PubMed

Ngaotrakanwiwat, Pailin; Meeyoo, Vissanu

2012-01-01

TiO2-V2O5 was prepared and evaluated as an energy storage material for photocatalysts with high capacity and initial charging rate. The compound was successfully obtained by sol-gel technique and effects of compound composition and calcination temperature on the energy storage ability were investigated. The synthesized compounds were characterized by means of X-ray powder diffraction (XRD), scanning electron microscopy equipped with energy-dispersive X-ray analysis (SEM-EDX) and transmission electron microscopy (TEM). The results reveals that the compound of Ti:V molar ratio equal to 1:0.11 calcined at 550 degrees C exhibited superior energy storage ability than parent substances and 1.7-times higher capacity and 2.3-times higher initial charging rate compared to WO3, indicating that the compound is a remarkable alternative to conventional energy storage substances.

Rate Dependent Multi-Mechanism Discharge of Ag 0.50VOP 4·1.8H 2O: Insights from In Situ Energy Dispersive X-ray Diffraction

DOE Office of Scientific and Technical Information (OSTI.GOV)

Huie, Matthew M.; Bock, David C.; Zhong, Zhong

Ag 0.50VOPO 4·1.8H 2O (silver vanadium phosphate, SVOP) demonstrates a counterintuitive higher initial loaded voltage under higher discharge current. Energy dispersive X-ray diffraction (EDXRD) from synchrotron radiation was used to create tomographic profiles of cathodes at various depths of discharge for two discharge rates. SVOP displays two reduction mechanisms, reduction of a vanadium center accompanied by lithiation of the structure, or reduction-displacement of a silver cation to form silver metal. In-situ EDXRD provides the opportunity to observe spatially resolved changes to the parent SVOP crystal and formation of Ag 0 during reduction. At a C/170 discharge rate V 5+ reductionmore » is the preferred initial reaction resulting in higher initial loaded voltage. At a discharge rate of C/400 reduction of Ag + with formation of conductive Ag 0 occurs earlier during discharge. Discharge rate also affects the spatial location of reduction products. The faster discharge rate initiates reduction close to the current collector with non-uniform distribution of silver metal resulting in isolated cathode areas. The slower rate develops a more homogenous distribution of reduced SVOP and silver metal. This study illuminates the roles of electronic and ionic conductivity limitations within a cathode at the mesoscale and how they impact the course of reduction processes and loaded voltage.« less

Rate Dependent Multi-Mechanism Discharge of Ag 0.50VOP 4·1.8H 2O: Insights from In Situ Energy Dispersive X-ray Diffraction

DOE PAGES

Huie, Matthew M.; Bock, David C.; Zhong, Zhong; ...

2016-09-01

Ag 0.50VOPO 4·1.8H 2O (silver vanadium phosphate, SVOP) demonstrates a counterintuitive higher initial loaded voltage under higher discharge current. Energy dispersive X-ray diffraction (EDXRD) from synchrotron radiation was used to create tomographic profiles of cathodes at various depths of discharge for two discharge rates. SVOP displays two reduction mechanisms, reduction of a vanadium center accompanied by lithiation of the structure, or reduction-displacement of a silver cation to form silver metal. In-situ EDXRD provides the opportunity to observe spatially resolved changes to the parent SVOP crystal and formation of Ag 0 during reduction. At a C/170 discharge rate V 5+ reductionmore » is the preferred initial reaction resulting in higher initial loaded voltage. At a discharge rate of C/400 reduction of Ag + with formation of conductive Ag 0 occurs earlier during discharge. Discharge rate also affects the spatial location of reduction products. The faster discharge rate initiates reduction close to the current collector with non-uniform distribution of silver metal resulting in isolated cathode areas. The slower rate develops a more homogenous distribution of reduced SVOP and silver metal. This study illuminates the roles of electronic and ionic conductivity limitations within a cathode at the mesoscale and how they impact the course of reduction processes and loaded voltage.« less

Quantitative Imaging of Single Unstained Magnetotactic Bacteria by Coherent X-ray Diffraction Microscopy.

PubMed

Fan, Jiadong; Sun, Zhibin; Zhang, Jian; Huang, Qingjie; Yao, Shengkun; Zong, Yunbing; Kohmura, Yoshiki; Ishikawa, Tetsuya; Liu, Hong; Jiang, Huaidong

2015-06-16

Novel coherent diffraction microscopy provides a powerful lensless imaging method to obtain a better understanding of the microorganism at the nanoscale. Here we demonstrated quantitative imaging of intact unstained magnetotactic bacteria using coherent X-ray diffraction microscopy combined with an iterative phase retrieval algorithm. Although the signal-to-noise ratio of the X-ray diffraction pattern from single magnetotactic bacterium is weak due to low-scattering ability of biomaterials, an 18.6 nm half-period resolution of reconstructed image was achieved by using a hybrid input-output phase retrieval algorithm. On the basis of the quantitative reconstructed images, the morphology and some intracellular structures, such as nucleoid, polyβ-hydroxybutyrate granules, and magnetosomes, were identified, which were also confirmed by scanning electron microscopy and energy dispersive spectroscopy. With the benefit from the quantifiability of coherent diffraction imaging, for the first time to our knowledge, an average density of magnetotactic bacteria was calculated to be ∼1.19 g/cm(3). This technique has a wide range of applications, especially in quantitative imaging of low-scattering biomaterials and multicomponent materials at nanoscale resolution. Combined with the cryogenic technique or X-ray free electron lasers, the method could image cells in a hydrated condition, which helps to maintain their natural structure.

Crystalline Colloidal Arrays in Polymer Matrices

NASA Technical Reports Server (NTRS)

Sunkara, Hari B.; Penn, B. G.; Frazier, D. O.; Ramachandran, N.

1997-01-01

Crystalline Colloidal Arrays (CCA, also known as colloidal crystals), composed of aqueous or nonaqueous dispersions of self-assembled nanosized polymer colloidal spheres, are emerging toward the development of advanced optical devices for technological applications. The spontaneous self assembly of polymer spheres in a dielectric medium results from the electrostatic repulsive interaction between particles of uniform size and charge distribution. In a way similar to atomic crystals that diffract X-rays, CCA dispersions in thin quartz cells selectively and efficiently Bragg diffract the incident visible light. The reason for this diffraction is because the lattice (body or face centered cubic) spacing is on the order of the wavelength of visible light. Unlike the atomic crystals that diffract a fixed wavelength, colloidal crystals in principle, depending on the particle size, particle number and charge density, can diffract W, Vis or IR light. Therefore, the CCA dispersions can be used as laser filters. Besides, the diffraction intensity depends on the refractive index mismatch between polymer spheres and dielectric medium; therefore, it is possible to modulate incident light intensities by manipulating the index of either the spheres or the medium. Our interest in CCA is in the fabrication of all-optical devices such as optical switches, limiters, and spatial light modulators for optical signal processing. The two major requirements from a materials standpoint are the incorporation of suitable nonlinear optical materials (NLO) into polymer spheres which will allow us to alter the refractive index of the spheres by intense laser radiation, and preparation of solid CCA filters which can resist laser damage. The fabrication of solid composite filters not only has the advantage that the films are easier to handle, but also the arrays in solid films are more robust than in liquid media. In this paper, we report the photopolymerization process used to trap CCA in polymer matrices, the factors which affect the optical diffraction qualities of resulting polymer films, and methods to improve the efficiencies of solid optical filters. Before this, we also present the experimental demonstration, of controlling the optical diffraction intensities from aqueous CCA dispersions by varying the temperature, which establishes the feasibility of fabricating all-optical switching devices with nonlinear periodic array structures.

Upconversion luminescence of Er3+/Yb3+ doped Sr5(PO4)3OH phosphor powders

NASA Astrophysics Data System (ADS)

Mokoena, P. P.; Swart, H. C.; Ntwaeaborwa, O. M.

2018-04-01

Sr5(PO4)3OH co-doped with Er3+and Yb3+ powder phosphors were synthesized by urea combustion method. The crystal structure was analyzed using X-ray diffraction (XRD). Particle morphology was analyzed using a Jeol JSM 7800F thermal field emission scanning electron microscope (FE-SEM) and the chemical composition analysis was carried out using an Oxford Instruments AzTEC energy dispersive spectrometer (EDS) attached to the FE-SEM. Upconversion emission was measured by using a FLS980 Spectrometer equipped with a 980 nm NIR laser as the excitation source, and a photomultiplier (PMT) detector. The XRD data of the Sr5(PO4)3OH powder exhibited characteristic diffraction patterns of the hexagonal structure referenced in the standard JCPDS card number 00-033-1348. The sharp peaks revealed the formation of crystalline Sr5(PO4)3OH. The powders were made up of hexagonal nanospheres. The enhanced red emission due to the 4F9/2 → 4I15/2 transitions of Er3+ was observed and was attributed to up conversion (UC) energy transfer from Yb3+. The upconversion energy transfer mechanism from Yb3+ to Er3+ is discussed.

Homogeneous synthesis of Ag nanoparticles-doped water-soluble cellulose acetate for versatile applications.

PubMed

Cao, Jie; Sun, Xunwen; Zhang, Xinxing; Lu, Canhui

2016-11-01

We report a facile and efficient approach for synthesis of well-dispersed and stable silver nanoparticles (Ag NPs) using water-soluble cellulose acetate (CA) as both reductant and stabilizer. Partially substituted CA with highly active hydroxyl groups and excellent water-solubility is able to reduce silver ions in homogeneous aqueous medium effectively. The synthesized Ag NPs were characterized by UV-vis spectroscopy, X-ray diffraction, X-ray photoelectron spectroscopy, transmission electron microscopy and energy dispersive X-ray spectroscope analysis. The as-prepared Ag NPs were well-dispersed, showing a surface plasmon resonance peak at 426nm. The resulted Ag NPs@CA nanohybrids exhibit high catalytic activity for the reduction of 4-nitrophenol to 4-aminophenol in the presence of NaBH 4 . Meanwhile, the nanohybrids are also effective in inhibiting the growth of bacterial. This environmentally friendly method promotes the use of renewable natural resources to prepare a variety of inorganic-organic materials for catalysis, antibacterial, sensors and other applications. Copyright © 2016 Elsevier B.V. All rights reserved.

Thermoelectric properties of Co4Sb12 with Bi2Te3 nanoinclusions

NASA Astrophysics Data System (ADS)

Ghosh, Sanyukta; Bisht, Anuj; Karati, Anirudha; Rogl, Gerda; Rogl, Peter; Murty, B. S.; Suwas, Satyam; Mallik, Ramesh Chandra

2018-03-01

The figure of merit (zT) of a thermoelectric material can be enhanced by incorporation of nanoinclusions into bulk material. The presence of bismuth telluride (Bi2Te3) nanoinclusions in Co4Sb12 leads to lower phonon thermal conductivity by introducing interfaces and defects; it enhances the average zT between 300-700 K. In the current study, Bi2Te3 nanoparticles were dispersed into bulk Co4Sb12 by ball-milling. The bulk was fabricated by spark plasma sintering. The presence of Bi2Te3 dispersion in Co4Sb12 was confirmed by x-ray diffraction, scanning electron microscopy, transmission electron microscopy and electron back scattered diffraction technique. Energy dispersive spectroscopy showed antimony (Sb) as an impurity phase for higher contents of Bi2Te3 in the sample. The Seebeck coefficient (S) and electrical conductivity (σ) were measured in the temperature range of 350-673 K. The negative value of S indicates that most of the charge carriers were electrons. A decrease in S and increase in σ with Bi2Te3 content are due to the increased carrier concentration, as confirmed by Hall measurement. The thermal conductivity, measured between 423-673 K, decreased due to the increased phonon scattering at interfaces. A maximum zT of 0.17 was achieved at 523 K and it did not vary much throughout the temperature range. The experimental results of composites were compared by using effective medium theories.

Thermoelectric properties of Co4Sb12 with Bi2Te3 nanoinclusions.

PubMed

Ghosh, Sanyukta; Bisht, Anuj; Karati, Anirudha; Rogl, Gerda; Rogl, Peter; Murty, B S; Suwas, Satyam; Mallik, Ramesh Chandra

2018-02-12

The figure of merit (zT) of a thermoelectric material can be enhanced by incorporation of nanoinclusions into bulk material. The presence of bismuth telluride (Bi 2 Te 3 ) nanoinclusions in Co 4 Sb 12 leads to lower phonon thermal conductivity by introducing interfaces and defects; it enhances the average zT between 300-700 K. In the current study, Bi 2 Te 3 nanoparticles were dispersed into bulk Co 4 Sb 12 by ball-milling. The bulk was fabricated by spark plasma sintering. The presence of Bi 2 Te 3 dispersion in Co 4 Sb 12 was confirmed by x-ray diffraction, scanning electron microscopy, transmission electron microscopy and electron back scattered diffraction technique. Energy dispersive spectroscopy showed antimony (Sb) as an impurity phase for higher contents of Bi 2 Te 3 in the sample. The Seebeck coefficient (S) and electrical conductivity (σ) were measured in the temperature range of 350-673 K. The negative value of S indicates that most of the charge carriers were electrons. A decrease in S and increase in σ with Bi 2 Te 3 content are due to the increased carrier concentration, as confirmed by Hall measurement. The thermal conductivity, measured between 423-673 K, decreased due to the increased phonon scattering at interfaces. A maximum zT of 0.17 was achieved at 523 K and it did not vary much throughout the temperature range. The experimental results of composites were compared by using effective medium theories.

Studies on design of 351  nm focal plane diagnostic system prototype and focusing characteristic of SGII-upgraded facility at half achievable energy performance.

PubMed

Liu, Chong; Ji, Lailin; Yang, Lin; Zhao, Dongfeng; Zhang, Yanfeng; Liu, Dong; Zhu, Baoqiang; Lin, Zunqi

2016-04-01

In order to obtain the intensity distribution of a 351 nm focal spot and smoothing by spectral dispersion (SSD) focal plane profile of a SGII-upgraded facility, a type of off-axis imaging system with three spherical mirrors, suitable for a finite distance source point to be imaged near the diffraction limit has been designed. The quality factor of the image system is 1.6 times of the diffraction limit tested by a 1053 nm point source. Because of the absence of a 351 nm point source, we can use a Collins diffraction imaging integral with respect to λ=351  nm, corresponding to a quality factor that is 3.8 times the diffraction limit at 351 nm. The calibration results show that at least the range of ±10  mrad of view field angle and ±50  mm along the axial direction around the optimum object distance can be satisfied with near diffraction limited image that is consistent with the design value. Using this image system, the No. 2 beam of the SGII-upgraded facility has been tested. The test result of the focal spot of final optics assembly (FOA) at 351 nm indicates that about 80% of energy is encompassed in 14.1 times the diffraction limit, while the output energy of the No. 2 beam is 908 J at 1053 nm. According to convolution theorem, the true value of a 351 nm focal spot of FOA is about 12 times the diffraction limit because of the influence of the quality factor. Further experimental studies indicate that the RMS value along the smoothing direction is less than 15.98% in the SSD spot test experiment. Computer simulations show that the quality factor of the image system used in the experiment has almost no effect on the SSD focal spot test. The image system can remarkably distort the SSD focal spot distribution under the circumstance of the quality factor 15 times worse than the diffraction limit. The distorted image shows a steep slope in the contour of the SSD focal spot along the smoothing direction that otherwise has a relatively flat top region around the focal spot center.

Synthesis of parallel and antiparallel core-shell triangular nanoparticles

NASA Astrophysics Data System (ADS)

Bhattacharjee, Gourab; Satpati, Biswarup

2018-04-01

Core-shell triangular nanoparticles were synthesized by seed mediated growth. Using triangular gold (Au) nanoparticle as template, we have grown silver (Ag) shellto get core-shell nanoparticle. Here by changing the chemistry we have grown two types of core-shell structures where core and shell is having same symmetry and also having opposite symmetry. Both core and core-shell nanoparticles were characterized using transmission electron microscopy (TEM) and energy dispersive X-ray spectroscopy (EDX) to know the crystal structure and composition of these synthesized core-shell nanoparticles. From diffraction pattern analysis and energy filtered TEM (EFTEM) we have confirmed the crystal facet in core is responsible for such two dimensional growth of core-shell nanostructures.

A Holistic Multi Evidence Approach to Study the Fragmentation Behaviour of Crystalline Mannitol

PubMed Central

Koner, Jasdip S.; Rajabi-Siahboomi, Ali; Bowen, James; Perrie, Yvonne; Kirby, Daniel; Mohammed, Afzal R.

2015-01-01

Mannitol is an essential excipient employed in orally disintegrating tablets due to its high palatability. However its fundamental disadvantage is its fragmentation during direct compression, producing mechanically weak tablets. The primary aim of this study was to assess the fracture behaviour of crystalline mannitol in relation to the energy input during direct compression, utilising ball milling as the method of energy input, whilst assessing tablet characteristics of post-milled powders. Results indicated that crystalline mannitol fractured at the hydrophilic (011) plane, as observed through SEM, alongside a reduction in dispersive surface energy. Disintegration times of post-milled tablets were reduced due to the exposure of the hydrophilic plane, whilst more robust tablets were produced. This was shown through higher tablet hardness and increased plastic deformation profiles of the post-milled powders, as observed with a lower yield pressure through an out-of-die Heckel analysis. Evaluation of crystal state using x-ray diffraction/differential scanning calorimetry showed that mannitol predominantly retained the β-polymorph; however x-ray diffraction provided a novel method to calculate energy input into the powders during ball milling. It can be concluded that particle size reduction is a pragmatic strategy to overcome the current limitation of mannitol fragmentation and provide improvements in tablet properties. PMID:26553127

A Holistic Multi Evidence Approach to Study the Fragmentation Behaviour of Crystalline Mannitol

NASA Astrophysics Data System (ADS)

Koner, Jasdip S.; Rajabi-Siahboomi, Ali; Bowen, James; Perrie, Yvonne; Kirby, Daniel; Mohammed, Afzal R.

2015-11-01

Mannitol is an essential excipient employed in orally disintegrating tablets due to its high palatability. However its fundamental disadvantage is its fragmentation during direct compression, producing mechanically weak tablets. The primary aim of this study was to assess the fracture behaviour of crystalline mannitol in relation to the energy input during direct compression, utilising ball milling as the method of energy input, whilst assessing tablet characteristics of post-milled powders. Results indicated that crystalline mannitol fractured at the hydrophilic (011) plane, as observed through SEM, alongside a reduction in dispersive surface energy. Disintegration times of post-milled tablets were reduced due to the exposure of the hydrophilic plane, whilst more robust tablets were produced. This was shown through higher tablet hardness and increased plastic deformation profiles of the post-milled powders, as observed with a lower yield pressure through an out-of-die Heckel analysis. Evaluation of crystal state using x-ray diffraction/differential scanning calorimetry showed that mannitol predominantly retained the β-polymorph however x-ray diffraction provided a novel method to calculate energy input into the powders during ball milling. It can be concluded that particle size reduction is a pragmatic strategy to overcome the current limitation of mannitol fragmentation and provide improvements in tablet properties.

Mechanosynthesis of A Ferritic ODS (Oxide Dispersion Strengthened) Steel Containing 14% Chromium and Its Characterization

NASA Astrophysics Data System (ADS)

Rivai, A. K.; Dimyati, A.; Adi, W. A.

2017-05-01

One of the advanced materials for application at high temperatures which is aggressively developed in the world is ODS (Oxide Dispersion strengthened) steel. ODS ferritic steels are one of the candidate materials for future nuclear reactors in the world (Generation IV reactors) because it is able to be used in the reactor above 600 °C. ODS ferritic steels have also been developed for the interconnect material of SOFC (Solid Oxide Fuel Cell) which will be exposed to about 800 °C of temperature. The steel is strengthened by dispersing homogeneously of oxide particles (ceramic) in nano-meter sized in the matrix of the steel. Synthesis of a ferritic ODS steel by dispersion of nano-particles of yttrium oxide (yttria: Y2O3) as the dispersion particles, and containing high-chromium i.e. 14% has been conducted. Synthesis of the ODS steels was done mechanically (mechanosynthesis) using HEM (High Energy ball Milling) technique for 40 and 100 hours. The resulted samples were characterized using SEM-EDS (Scanning Electron Microscope-Energy Dispersive Spectroscope), and XRD (X-ray diffraction) to analyze the microstructure characteristics. The results showed that the crystal grains of the sample with 100 hours milling time was much smaller than the sample with 40 hours milling time, and some amount of alloy was formed during the milling process even for 40 hours milling time. Furthermore, the structure analysis revealed that some amount of iron atom substituted by a slight amount of chromium atom as a solid solution. The quantitative analysis showed that the phase mostly consisted of FeCr solid-solution with the structure was BCC (body-centered cubic).

Powder diffraction and crystal structure prediction identify four new coumarin polymorphs

DOE Office of Scientific and Technical Information (OSTI.GOV)

Shtukenberg, Alexander G.; Zhu, Qiang; Carter, Damien J.

Coumarin, a simple, commodity chemical isolated from beans in 1820, has, to date, only yielded one solid state structure. Here, we report a rich polymorphism of coumarin grown from the melt. Four new metastable forms were identified and their crystal structures were solved using a combination of computational crystal structure prediction algorithms and X-ray powder diffraction. With five crystal structures, coumarin has become one of the few rigid molecules showing extensive polymorphism at ambient conditions. We demonstrate the crucial role of advanced electronic structure calculations including many-body dispersion effects for accurate ranking of the stability of coumarin polymorphs and themore » need to account for anharmonic vibrational contributions to their free energy. As such, coumarin is a model system for studying weak intermolecular interactions, crystallization mechanisms, and kinetic effects.« less

X-ray diffraction of solid tin to 1.2 TPa

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lazicki, A.; Rygg, J. R.; Coppari, F.

2015-08-12

In this study, we report direct in situ measurements of the crystal structure of tin between 0.12 and 1.2 TPa, the highest stress at which a crystal structure has ever been observed. Using angle-dispersive powder x-ray diffraction, we find that dynamically compressed Sn transforms to the body-centered-cubic (bcc) structure previously identified by ambient-temperature quasistatic-compression studies and by zero-kelvin density-functional theory predictions between 0.06 and 0.16 TPa. However, we observe no evidence for the hexagonal close-packed (hcp) phase found by those studies to be stable above 0.16 TPa. Instead, our results are consistent with bcc up to 1.2 TPa. We conjecturemore » that at high temperature bcc is stabilized relative to hcp due to differences in vibrational free energy.« less

Synthesis of zirconia (ZrO2) nanowires via chemical vapor deposition

NASA Astrophysics Data System (ADS)

Baek, M. K.; Park, S. J.; Choi, D. J.

2017-02-01

Monoclinic zirconia nanowires were synthesized by chemical vapor deposition using ZrCl4 powder as a starting material at 1200 °C and 760 Torr. Graphite was employed as a substrate, and an Au thin film was pre-deposited on the graphite as a catalyst. The zirconia nanostructure morphology was observed through scanning electron microscopy and transmission electron microscopy. Based on X-ray diffraction, selected area electron diffraction, and Raman spectroscopy data, the resulting crystal structure was found to be single crystalline monoclinic zirconia. The homogeneous distributions of Zr, O and Au were studied by scanning transmission electron microscopy with energy dispersive X-ray spectroscopy mapping, and there was no metal droplet at the nanowire tips despite the use of an Au metal catalyst. This result is apart from that of conventional metal catalyzed nanowires.

Magneto-structural studies of sol-gel synthesized nanocrystalline manganese substituted nickel ferrites

NASA Astrophysics Data System (ADS)

Pandav, R. S.; Patil, R. P.; Chavan, S. S.; Mulla, I. S.; Hankare, P. P.

2016-11-01

Nanocrystalline NiFe2-xMnxO4 (2≥x≥0) ferrites were prepared by sol-gel method. X-ray diffraction patterns reveal that synthesized compounds are in single phase cubic spinel lattice for all the composition. The surface morphology of all the samples were studied by scanning electron microscopy. The particle size measured from transmission electron microscopy and X-ray diffraction patterns confirms the nanosized dimension of the as-prepared powder. The elemental analysis was carried out by energy dispersive X-ray analysis technique. Magnetic properties such as saturation magnetization, coercivity and remanence are studied as a function of increasing Mn concentration at room temperature. The saturation magnetization shows a decreasing trend with increase in Mn content. The substitution of manganese in the nickel ferrite affects the structural and magnetic properties of cubic spinels.

Determination of the absolute chirality of tellurium using resonant diffraction with circularly polarized x-rays.

PubMed

Tanaka, Y; Collins, S P; Lovesey, S W; Matsumami, M; Moriwaki, T; Shin, S

2010-03-31

Many proteins, sugars and pharmaceuticals crystallize into two forms that are mirror images of each other (enantiomers) like our right and left hands. Tellurium is one enantiomer having a space group pair, P3(1)21 (right-handed screw) and P3(2)21 (left-handed screw). X-ray diffraction with dispersion correction terms has been playing an important role in determining the handedness of enantiomers for a long time. However, this approach is not applicable for an elemental crystal such as tellurium or selenium. We have demonstrated that positive and negative circularly polarized x-rays at the resonant energy of tellurium can be used to absolutely distinguish right from left tellurium. This method is applicable to chiral motifs that occur in biomolecules, liquid crystals, ferroelectrics and antiferroelectrics, multiferroics, etc.

A chemical reduction approach to the synthesis of copper nanoparticles

NASA Astrophysics Data System (ADS)

Khan, Ayesha; Rashid, Audil; Younas, Rafia; Chong, Ren

2016-11-01

Development of improved methods for the synthesis of copper nanoparticles is of high priority for the advancement of material science and technology. Herein, starch-protected zero-valent copper (Cu) nanoparticles have been successfully synthesized by a novel facile route. The method is based on the chemical reduction in aqueous copper salt using ascorbic acid as reducing agent at low temperature (80 °C). X-ray diffraction, scanning electron microscopy and energy-dispersive X-ray spectroscopy measurements were taken to investigate the size, structure and composition of synthesized Cu nanocrystals, respectively. Average crystallite size of Cu nanocrystals calculated from the major diffraction peaks using the Scherrer formula is about 28.73 nm. It is expected that the outcomes of the study take us a step closer toward designing rational strategies for the synthesis of nascent Cu nanoparticles without inert gas protection.

Synthesis and characterization of hollow spherical copper phosphide (Cu 3P) nanopowders

NASA Astrophysics Data System (ADS)

Liu, Shuling; Qian, Yitai; Xu, Liqiang

2009-03-01

In this paper, hollow spherical Cu 3P nanopowders were synthesized by using copper sulfate pentahydrate (CuSO 4ṡ5H 2O) and yellow phosphorus in a mixed solvent of glycol, ethanol and water at 140-180 ∘C for 12 h. X-ray powder diffraction (XRD), energy dispersive X-ray spectroscopy (EDX), electron diffraction pattern (ED) and transmission electronic microscopy (TEM) studies show that the as-synthesized nanocrystal is pure hexagonal phase Cu 3P with a hollow spherical morphology. Based on the TEM observations, a possible aggregation growth mechanism was proposed for the formation of Cu 3P hollow structures. Meanwhile, the effects of some key factors such as solvents, reaction temperature and reaction time on the final formation of the Cu 3P hollow structure were also discussed.

Powder diffraction and crystal structure prediction identify four new coumarin polymorphs

DOE PAGES

Shtukenberg, Alexander G.; Zhu, Qiang; Carter, Damien J.; ...

2017-05-15

Coumarin, a simple, commodity chemical isolated from beans in 1820, has, to date, only yielded one solid state structure. Here, we report a rich polymorphism of coumarin grown from the melt. Four new metastable forms were identified and their crystal structures were solved using a combination of computational crystal structure prediction algorithms and X-ray powder diffraction. With five crystal structures, coumarin has become one of the few rigid molecules showing extensive polymorphism at ambient conditions. We demonstrate the crucial role of advanced electronic structure calculations including many-body dispersion effects for accurate ranking of the stability of coumarin polymorphs and themore » need to account for anharmonic vibrational contributions to their free energy. As such, coumarin is a model system for studying weak intermolecular interactions, crystallization mechanisms, and kinetic effects.« less

Structural and optical properties of WTe2 single crystals synthesized by DVT technique

NASA Astrophysics Data System (ADS)

Dixit, Vijay; Vyas, Chirag; Pathak, V. M.; Soalanki, G. K.; Patel, K. D.

2018-05-01

Layered transition metal di-chalcogenide (LTMDCs) crystals have attracted much attention due to their potential in optoelectronic device applications recently due to realization of their monolayer based structures. In the present investigation we report growth of WTe2 single crystals by direct vapor transport (DVT) technique. These crystals are then characterized by energy dispersive analysis of x-rays (EDAX) to study stoichiometric composition after growth. The structural properties are studied by x-ray diffraction (XRD) and selected area electron diffraction (SAED) is used to confirm orthorhombic structure of grown WTe2 crystal. Surface morphological properties of the crystals are also studied by scanning electron microscope (SEM). The optical properties of the grown crystals are studied by UV-Visible spectroscopy which gives direct band gap of 1.44 eV for grown WTe2 single crystals.

Solvothermal synthesis of Au@Fe3O4 nanoparticles for antibacterial applications

NASA Astrophysics Data System (ADS)

Kelgenbaeva, Zhazgul; Abdullaeva, Zhypargul; Murzubraimov, Bektemir

2018-04-01

We present Au@Fe3O4 nanoparticles obtained from Fe nanoparticles and HAuCl4 using a simple solvothermal method. Trisodium citrate (C6H5Na3O7*2H2O) served as a reducing agent for Au. X-ray diffraction analysis, electronic microscopes and energy-dispersive X-ray spectroscopy revealed cubic structure, elemental composition (Au, Fe and O) and spherical shape of nanoparticles. Antibacterial activity of the sample was tested against E. coli bacteria and obtained results were discussed.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Malik, Hitendra K., E-mail: hkmalik@physics.iitd.ac.in; Singh, Omveer; Dahiya, Raj P.

We have established a hot cathode arc discharge plasma system, where different stainless steel samples can be treated by monitoring the plasma parameters and nitriding parameters independently. In the present work, a mixture of 70% N{sub 2} and 30% H{sub 2} gases was fed into the plasma chamber and the treatment time and substrate temperature were optimized for treating 304L Stainless Steel samples. Various physical techniques such as x-ray diffraction, energy dispersive x-ray spectroscopy and micro-vickers hardness tester were employed to determine the structural, surface composition and surface hardness of the treated samples.

Growth and microtopographic study of CuInSe{sub 2} single crystals

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chauhan, Sanjaysinh M.; Chaki, Sunil, E-mail: sunilchaki@yahoo.co.in; Deshpande, M. P.

2016-05-23

The CuInSe{sub 2} single crystals were grown by chemical vapour transport (CVT) technique using iodine as transporting agent. The elemental composition of the as-grown CuInSe{sub 2} single crystals was determined by energy dispersive analysis of X-ray (EDAX). The unit cell crystal structure and lattice parameters were determined by X-ray diffraction (XRD) technique. The surface microtopographic study of the as-grown CuInSe{sub 2} single crystals surfaces were done to study the defects, growth mechanism, etc. of the CVT grown crystals.

Preparation of carbon nanotubes/BiOBr composites with higher visible light photocatalytic activity

NASA Astrophysics Data System (ADS)

You, Y. J.; Zhang, Y. X.; Li, R. R.; Li, C. H.

2014-12-01

A novel flower-like photocatalyst CNTs/BiOBr was successfully prepared by a facile hydrothermal method. The morphology and the physicochemical properties of the prepared samples were investigated using scanning electron microscopy (SEM), X-ray diffraction (XRD), energy dispersive X-ray spectrometry (EDX), and UV-visible diffuse reflectance spectroscopy (UV-vis DRS). The photocatalytic activity was evaluated by degradation of Rhodamin B (RhB) dye. It was demonstrated that CNTs/BiOBr photocatalyst could effectively photodegrade RhB under visible light (VL) irradiation.

One-pot nucleation, growth, morphogenesis, and passivation of 1.4 nm Au nanoparticles on self-assembled rosette nanotubes.

PubMed

Chhabra, Rahul; Moralez, Jesus G; Raez, Jose; Yamazaki, Takeshi; Cho, Jae-Young; Myles, Andrew J; Kovalenko, Andriy; Fenniri, Hicham

2010-01-13

A one-pot strategy for the nucleation, growth, morphogenesis, and passivation of 1.4 nm Au nanoparticles (NPs) on self-assembled rosette nanotubes (RNTs) is described. Tapping-mode atomic force microscopy, transmission electron microscopy, energy-dispersive X-ray analysis, and selected-area electron diffraction were used to establish the structure and organization of this hybrid material. Notably, we found that the Au NPs formed were nearly monodisperse clusters of Au(55) (1.4-1.5 nm) nestled in pockets on the RNT surface.

Tailoring oxidation of aluminum nanoparticles reinforced with carbon nanotubes

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sharma, Manjula; Sharma, Vimal, E-mail: manjula.physics@gmail.com

2016-05-23

In this report, the oxidation temperature and reaction enthalpy of Aluminum (Al) nanoparticles has been controlled by reinforcing with carbon nanotubes. The physical mixing method with ultrasonication was employed to synthesize CNT/Al nanocomposite powders. The micro-morphology of nanoconmposite powders has been analysed by scanning electron microscopy, energy dispersive spectroscopy, Raman spectroscopy and X-ray diffraction techniques. The oxidation behavior of nanocomposite powders analyzed by thermogravimetry/differential scanning calorimertry showed improvement in the exothermic enthalpy. Largest exothermic enthalpy of-1251J/g was observed for CNT (4 wt%)/Al nanocomposite.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Srivastava, Himanshu; Ganguli, Tapas; Deb, S. K.

Growth of CuO nanowires by annealing method has been studied in-situ by grazing incidence Energy Dispersive X-ray Diffraction (EDXRD) technique on Indus-2. It was observed that Cu slowly oxidized to Cu{sub 2}O and finally to CuO. The data was taken as a function of time at two annealing temperatures 500 Degree-Sign C where nanowires form and 300 Degree-Sign C where nanowires don't form. We found that the strain in the CuO layer may be a principal factor for the spontaneous growth of nanowires in annealing method.

Synthesis and Raman scattering of GaN nanorings, nanoribbons and nanowires

NASA Astrophysics Data System (ADS)

Li, Z. J.; Chen, X. L.; Li, H. J.; Tu, Q. Y.; Yang, Z.; Xu, Y. P.; Hu, B. Q.

Low-dimensional GaN materials, including nanorings, nanoribbons and smooth nanowires have been synthesized by reacting gallium and ammonia using Ag particles as a catalyst on the substrate of MgO single crystals. They were characterized by field emission scanning electron microscopy (FE-SEM), energy dispersive X-ray spectroscopy (EDX) and X-ray diffraction (XRD). EDX, XRD indicated that the low-dimensional nanomaterials were wurtzite GaN. New features are found in Raman scatterings for these low-dimensional GaN materials, which are different from the previous observations of GaN materials.

Determination of dispersive optical constants of nanocrystalline CdSe (nc-CdSe) thin films

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sharma, Kriti; Al-Kabbi, Alaa S.; Saini, G.S.S.

2012-06-15

Highlights: ► nc-CdSe thin films are prepared by thermal vacuum evaporation technique. ► TEM analysis shows NCs are spherical in shape. ► XRD reveals the hexagonal (wurtzite) crystal structure of nc-CdSe thin films. ► The direct optical bandgap of nc-CdSe is 2.25 eV in contrast to bulk (1.7 eV). ► Dispersion of refractive index is discussed in terms of Wemple–DiDomenico single oscillator model. -- Abstract: The nanocrystalline thin films of CdSe are prepared by thermal evaporation technique at room temperature. These thin films are characterized by transmission electron microscopy (TEM), scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDX), X-raymore » diffraction (XRD) and photoluminescence spectroscopy (PL). The transmission spectra are recorded in the transmission range 400–3300 nm for nc-CdSe thin films. Transmittance measurements are used to calculate the refractive index (n) and absorption coefficient (α) using Swanepoel's method. The optical band gap (E{sub g}{sup opt}) has been determined from the absorption coefficient values using Tauc's procedure. The optical constants such as extinction coefficient (k), real (ε{sub 1}) and imaginary (ε{sub 2}) dielectric constants, dielectric loss (tan δ), optical conductivity (σ{sub opt}), Urbach energy (E{sub u}) and steepness parameter (σ) are also calculated for nc-CdSe thin films. The normal dispersion of refractive index is described using Wemple–DiDomenico single-oscillator model. Refractive index dispersion is further analysed to calculate lattice dielectric constant (ε{sub L}).« less

Scanning transmission electron microscopy and its application to the study of nanoparticles and nanoparticle systems.

PubMed

Liu, Jingyue

2005-06-01

Scanning transmission electron microscopy (STEM) techniques can provide imaging, diffraction and spectroscopic information, either simultaneously or in a serial manner, of the specimen with an atomic or a sub-nanometer spatial resolution. High-resolution STEM imaging, when combined with nanodiffraction, atomic resolution electron energy-loss spectroscopy and nanometer resolution X-ray energy dispersive spectroscopy techniques, is critical to the fundamental studies of importance to nanoscience and nanotechnology. The availability of sub-nanometer or sub-angstrom electron probes in a STEM instrument, due to the use of a field emission gun and aberration correctors, ensures the greatest capabilities for studies of sizes, shapes, defects, crystal and surface structures, and compositions and electronic states of nanometer-size regions of thin films, nanoparticles and nanoparticle systems. The various imaging, diffraction and spectroscopy modes available in a dedicated STEM or a field emission TEM/STEM instrument are reviewed and the application of these techniques to the study of nanoparticles and nanostructured catalysts is used as an example to illustrate the critical role of the various STEM techniques in nanotechnology and nanoscience research.

Na0.44MnO2 nanorods as a cathode material for Na-ion batteries

NASA Astrophysics Data System (ADS)

Avci, Sevda; Oz, Erdinc; Demirel, Serkan; Altin, Emine; Altin, Serdar; Bayri, Ali; Yakinci, Eyyuphan

2014-03-01

Lithium-ion batteries have dominated the rechargeable battery market because of their high energy and power capability. On the other hand, sodium is one of the more abundant elements on Earth unlike Li. Moreover, Na has similar chemical properties to Li, indicating that Na-ion batteries can be an alternative to Li counterparts. With that respect, we have synthesized Na0.44MnO2 nanorods as cathode materials for Na-ion batteries. We have investigated the effects of structural, electrical, and magnetic properties on battery performance. We report the synthesis conditions and growth mechanism of the nanorods. The structure and the morphology of the materials were investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive X-ray (EDX), and atomic force microscopy (AFM) techniques. Temperature dependent structural changes were determined via in situ X-ray diffraction and TG-DTA measurements showing structural changes above room temperature. This work is funded by The Scientific and Technological Research Council of Turkey with Grant No:112M487.

Green synthesis and spectral characterization of silver nanoparticles from Lakshmi tulasi (Ocimum sanctum) leaf extract

NASA Astrophysics Data System (ADS)

Subba Rao, Y.; Kotakadi, Venkata S.; Prasad, T. N. V. K. V.; Reddy, A. V.; Sai Gopal, D. V. R.

2013-02-01

A simple method for the green synthesis of silver nanoparticles (AgNPs) using aqueous extract of Lakshmi tulasi (Ocimum sanctum) leaf as a reducing and stabilizing agent. AgNPs were rapidly synthesized using aqueous extract of tulasi leaf with AgNO3 solution within 15 min. The green synthesized AgNPs were characterized using physic-chemical techniques viz., UV-Vis, X-ray diffraction (XRD), scanning electron microscope (SEM) coupled with X-ray energy dispersive spectroscopy (EDX) and Fourier transform-infrared spectroscopy (FT-IR). Characterization data reveals that the particles were crystalline in nature and triangle shaped with an average size of 42 nm. The zeta potential of AgNPs were found to be -55.0 mV. This large negative zeta potential value indicates repulsion among AgNPs and their dispersion stability.

Size-dependent antimicrobial properties of the cobalt ferrite nanoparticles

NASA Astrophysics Data System (ADS)

Žalnėravičius, Rokas; Paškevičius, Algimantas; Kurtinaitiene, Marija; Jagminas, Arūnas

2016-10-01

The growing resistance of bacteria to conventional antibiotics elicited considerable interest to non-typical drugs. In this study, antimicrobial investigations were performed on low-size dispersion cobalt ferrite nanoparticles (Nps) fabricated by co-precipitation approach in several average sizes, in particular, 15.0, 5.0, and 1.65 nm. A variety of experimental tests demonstrated that the size of these Nps is determinant for antimicrobial efficiency against S. cerevisiae and several Candida species, in particular, C. parapsilosis, C. krusei, and C. albicans. The small and ultra-small fractions of CoFe2O4 Nps possess especially strong antimicrobial activity against all tested microorganisms. The possible reasons are discussed. Nps were characterized by means of transmission and high-resolution transmission electron microscopy, X-ray diffraction, energy dispersive X-ray spectroscopy and atomic force microscopy, chemical analysis and magnetic measurements.

Cu Nanoparticles Improved Thermal Property of Form-Stable Phase Change Materials Made with Carbon Nanofibers and LA-MA-SA Eutectic Mixture.

PubMed

Song, Xiaofei; Cai, Yibing; Huang, Cong; Gu, Ying; Zhang, Junhao; Qiao, Hui; Wei, Qufu

2018-04-01

A novel form-stable phase change materials (FSPCMs) was fabricated by incorporating fatty acid eutectics with electrospun carbon nanofibers (CNFs) surface-attached with copper (Cu) nanoparticles. Three different Cu/CNFs mats were made through combining the technique and principle of electrospinning, pre-oxidation/carbonization and in-situ reduction, while lauric-myristic-stearic acid (LA-MA-SA) ternary eutectic mixture was prepared as the model PCM. The morphology and crystal structure of Cu/CNFs were characterized by Fourier transfer infrared (FT-IR) spectra, Scanning electron microscopy (SEM), X-ray diffraction (XRD) and X-ray energy dispersive spectroscopy (EDS), respectively. The results showed that Cu nanoparticles dispersed uniformly on the surface of CNFs mats without agglomeration, and Cu/CNFs mats could provide the mechanical support for FSPCMs and effectively prevent the flow/leakage of molten fatty acid. Morphological structures, as well as the properties of thermal energy storage and thermal energy storage/retrieval rates, of the resulting FSPCMs were investigated by SEM, Differential scanning calorimetry (DSC), and measurement of melting/freezing times, respectively. The results indicated that the fabricated FSPCMs exhibited desired structural morphology, and LA-MA-SA well dispersed in three-dimensional porous structure of Cu/CNFs mats. The melting and crystallization enthalpies of the fabricated FSPCMs were in the range of 117.1-140.7 kJ/kg and 117.2-142.4 kJ/kg, respectively. In comparison with melting/freezing times of LA-MA-SA ternary eutectic mixture, the melting/freezing times of fabricated FSPCMs were respectively decreased ~27.0-49.2% and ~44.1-63.0%. The fabricated FSPCMs possessed good thermal energy storage/retrieval property, and might have great potential for renewable energy storage applications.

Diffractive Optical Elements for Spectral Imaging

NASA Technical Reports Server (NTRS)

Wilson, D.; Maker, P.; Muller, R.; Mourolis, P.; Descour, M.; Volin, C.; Dereniak, E.

2000-01-01

Diffractive optical elements fabricated on flat and non-flat substrates frequently act as dispersive elements in imaging spectrometers. We describe the design and electron-beam fabrication of blazed and computer-generated-hologram gratings for slit and tomographic imaging spectrometer.

Diffractive Optical Elements for Spectral Imaging

NASA Technical Reports Server (NTRS)

Wilson, D.; Maker, P.; Muller, R.; Maker, P.; Mouroulis, P.; Descour, M.; Volin, C.; Dereniak, E.

2000-01-01

Diffractive optical elements fabricated on flat and non-flat substrates frequently act as dispersive elements in imaging spectrometers. We describe the design and electron-beam fabrication of blazed and computer-generated-hologram gratings for slit and tomographic imaging spectrometers.

Refractive index of colloidal dispersions of spheroidal particles

DOE Office of Scientific and Technical Information (OSTI.GOV)

Meeten, G.H.

1980-09-01

The effect of particle shape on the refractive index of a colloidal dispersion of spheroidal particles is investigated theoretically, using the Rayleigh, Rayleigh- Gans-Debye, and the anomalous diffraction light-scattering approximations. It is shown that departure from particle sphericity modify the dispersion refractive index, both size and shape being of importance.

Evaluate the ability of PVP to inhibit crystallization of amorphous solid dispersions by density functional theory and experimental verify.

PubMed

Wang, Bing; Wang, Dandan; Zhao, Shan; Huang, Xiaobin; Zhang, Jianbin; Lv, Yan; Liu, Xiaocen; Lv, Guojun; Ma, Xiaojun

2017-01-01

In this study, we used density functional theory (DFT) to predict polymer-drug interactions, and then evaluated the ability of poly (vinyl pyrrolidone) (PVP) to inhibit crystallization of amorphous solid dispersions by experimental-verification. Solid dispersions of PVP/resveratrol (Res) and PVP/griseofulvin (Gri) were adopted for evaluating the ability of PVP to inhibit crystallization. The density functional theory (DFT) with the B3LYP was used to calculate polymer-drug and drug-drug interactions. Fourier transform infrared spectroscopy (FTIR) was used to confirm hydrogen bonding interactions. Polymer-drug miscibility and drug crystallinity were characterized by the modulated differential scanning calorimetry (MDSC) and X-ray powder diffraction (XRD). The release profiles were studied to investigate the dissolution advantage. DFT results indicated that E PVP-Res >E Res-Res (E: represents hydrogen bonding energy). A strong interaction was formed between PVP and Res. In addition, Fourier transform infrared spectroscopy (FTIR) analysis showed hydrogen bonding formed between PVP and Res, but not between PVP and Gri. MDSC and XRD results suggested that 70-90wt% PVP/Res and PVP/Gri solid dispersions formed amorphous solid dispersions (ASDs). Under the accelerated testing condition, PVP/Res dispersions with higher miscibility quantified as 90/10wt% were more stable than PVP/Gri dispersions. The cumulative dissolution rate of 90wt% PVP/Res dispersions still kept high after 90days storage due to the strong interaction. However, the cumulative dissolution rate of PVP/Gri solid dispersions significantly dropped because of the recrystallization of Gri. Copyright © 2016 Elsevier B.V. All rights reserved.

Flat ion milling: a powerful tool for preparation of cross-sections of lead-silver alloys.

PubMed

Brodusch, Nicolas; Boisvert, Sophie; Gauvin, Raynald

2013-06-01

While conventional mechanical and chemical polishing results in stress, deformation and polishing particles embedded on the surface, flat milling with Ar+ ions erodes the material with no mechanical artefacts. This flat milling process is presented as an alternative method to prepare a Pb-Ag alloy cross-section for scanning electron microscopy. The resulting surface is free of scratches with very little to no stress induced, so that electron diffraction and channelling contrast are possible. The results have shown that energy dispersive spectrometer (EDS) mapping, electron channelling contrast imaging and electron backscatter diffraction can be conducted with only one sample preparation step. Electron diffraction patterns acquired at 5 keV possessed very good pattern quality, highlighting an excellent surface condition. An orientation map was acquired at 20 keV with an indexing rate of 90.1%. An EDS map was performed at 5 keV, and Pb-Ag precipitates of sizes lower than 100 nm were observed. However, the drawback of the method is the generation of a noticeable surface topography resulting from the interaction of the ion beam with a polycrystalline and biphasic sample.

Examining the ground layer of St. Anthony from Padua 19th century oil painting by Raman spectroscopy, scanning electron microscopy and X-ray diffraction

NASA Astrophysics Data System (ADS)

Vančo, Ľubomír; Kadlečíková, Magdaléna; Breza, Juraj; Čaplovič, Ľubomír; Gregor, Miloš

2013-01-01

In this paper we studied the material composition of the ground layer of a neoclassical painting. We used Raman spectroscopy (RS) as a prime method. Thereafter scanning electron microscopy combined with energy dispersive spectroscopy (SEM-EDS) and X-ray powder diffraction (XRD) were employed as complementary techniques. The painting inspected was of the side altar in King St. Stephen's Church in Galanta (Slovakia), signed and dated by Jos. Chr. Mayer 1870. Analysis was carried out on both covered and uncovered ground layers. Four principal compounds (barite, lead white, calcite, dolomite) and two minor compounds (sphalerite, quartz) were identified. This ground composition is consistent with the 19th century painting technique used in Central Europe consisting of white pigments and white fillers. Transformation of lead white occurred under laser irradiation. Subdominant Raman peaks of the components were measured. The observed results elucidate useful partnership of RS and SEM-EDS measurements supported by X-ray powder diffraction as well as possibilities and limitations of non-destructive analysis of covered lower layers by RS.

Direct laser interference patterning of ophthalmic polydimethylsiloxane (PDMS) polymers

NASA Astrophysics Data System (ADS)

Sola, D.; Lavieja, C.; Orera, A.; Clemente, M. J.

2018-07-01

The inscription of diffractive elements in ophthalmic polymers and ocular tissues to induce refractive index changes is of great interest in the fields of Optics and Ophthalmology. In this work fabrication of linear periodic patterns in polydimethylsiloxane (PDMS) intraocular lenses by means of the direct laser interference patterning (DLIP) technique was studied. A Q-Switch Nd:YAG laser coupled to second and third harmonic modules emitting linearly polarized 4 ns pulses at 355 nm with 20 Hz repetition rate was used as the laser source. Laser processing parameters were modified to produce the linear patterns. Processed samples were characterized by means of optical confocal microscopy, Scanning Electron Microscopy SEM, Energy Dispersive X-ray Spectroscopy EDX, Attenuated Total Reflectance-Infrared Spectroscopy ATR-FTIR, and Raman Spectroscopy. Depending on the laser parameters both photo-thermal and photo-chemical damage were observed in the DLIP irradiated areas. Finally, diffractive techniques were used to characterize the diffraction gratings inscribed in the samples resulting in a refractive index change of 1.9 × 10-2 under illumination of a 632.8 nm He-Ne laser.

Rapid fabrication of superhydrophobic Al/Fe2O3 nanothermite film with excellent energy-release characteristics and long-term storage stability

NASA Astrophysics Data System (ADS)

Ke, Xiang; Zhou, Xiang; Hao, Gaozi; Xiao, Lei; Liu, Jie; Jiang, Wei

2017-06-01

One of the challenges for the application of energetic materials is their energy-retaining capabilities after long-term storage. In this study, we report a facile method to fabricate superhydrophobic Al/Fe2O3 nanothermite film by combining electrophoretic deposition and surface modification technologies. Different concentrations of dispersion solvents and additives are investigated to optimize the deposition parameters. Meanwhile, the dependence of deposition rates on nanoparticle concentrations is also studied. The surface morphology and chemical composition are characterized by field-emission scanning electron microscopy, X-ray diffraction, X-ray energy-dispersive spectroscopy, and X-ray photoelectron spectroscopy. A static contact angles as high as 156° shows the superhydrophobicity of the nanothermite film. Natural and accelerated aging tests are performed and the thermal behavior is analyzed. Thermal analysis shows that the surface modification contributes to significantly improved energy-release characteristics for both fresh and aged samples, which is supposed to be attributed to the preignition reaction between Al2O3 shell and FAS-17. Superhydrophobic Al/Fe2O3 nanothermite film exhibits excellent long-time storage stability with 83.4% of energy left in natural aging test and 60.5% in accelerated aging test. This study is instructive to the practical applications of nanothermites, especially in highly humid environment.

Anisotropic Thermal Expansion of Zirconium Diboride: An Energy-Dispersive X-Ray Diffraction Study

DOE Office of Scientific and Technical Information (OSTI.GOV)

Paxton, William A.; Özdemir, Tevfik E.; Şavklıyıldız, İlyas

Zirconiumore » m diboride (ZrB 2) is an attractive material due to its thermal and electrical properties. In recent years, ZrB 2has been investigated as a superior replacement for sapphire when used as a substrate for gallium nitride devices. Like sapphire, ZrB 2has an anisotropic hexagonal structure which defines its directionally dependent properties. However, the anisotropic behavior of ZrB 2is not well understood. In this paper, we use energy-dispersive synchrotron X-ray diffraction to measure the thermal expansion of polycrystalline ZrB 2powder from 300 to 1150 K. Nine Bragg reflections are fit using Pseudo-Voigt peak profiles and used to compute the a and c lattice parameters using a nonlinear least-squares approximation. The temperature-dependent instantaneous thermal expansion coefficients are determined for each a -axis and c -axis direction and are described by the following equations: α a = ( 4.1507 × 10 - 6 + 5.1086 × 10 - 9 ( T - 293.15 ) )/( 1 + 4.1507 × 10 - 6 ( T - 293.15 ) + 2.5543 × 10 - 9 ( T - 293.15 ) 2 ) and α c = ( 4.5374 × 10 - 6 + 4.3004 × 10 - 9 ( T - 293.15 ) )/( 1 + 4.5374 × 10 - 6 ( T - 293.15 ) + 2.1502 × 10 - 9 ( T - 293.15 ) 2 ). Our results are within range of previously reported values but describe the temperature anisotropy in more detail. We show that anisotropic expansion coefficients converge to the same value at about 780 K and diverge at higher temperatures. Results are compared with other reported values.« less

Diffractive-refractive optics: (+,-,-,+) X-ray crystal monochromator with harmonics separation.

PubMed

Hrdý, Jaromír; Mikulík, Petr; Oberta, Peter

2011-03-01

A new kind of two channel-cut crystals X-ray monochromator in dispersive (+,-,-,+) position which spatially separates harmonics is proposed. The diffracting surfaces are oriented so that the diffraction is inclined. Owing to refraction the diffracted beam is sagittally deviated. The deviation depends on wavelength and is much higher for the first harmonics than for higher harmonics. This leads to spatial harmonics separation. The idea is supported by ray-tracing simulation.

Inhibition effects of protein-conjugated amorphous zinc sulfide nanoparticles on tumor cells growth

NASA Astrophysics Data System (ADS)

Cao, Ying; Wang, Hua-Jie; Cao, Cui; Sun, Yuan-Yuan; Yang, Lin; Wang, Bao-Qing; Zhou, Jian-Guo

2011-07-01

In this article, a facile and environmentally friendly method was applied to fabricate BSA-conjugated amorphous zinc sulfide (ZnS) nanoparticles using bovine serum albumin (BSA) as the matrix. Transmission electron microscopy analysis indicated that the stable and well-dispersed nanoparticles with the diameter of 15.9 ± 2.1 nm were successfully prepared. The energy dispersive X-ray, X-ray powder diffraction, Fourier transform infrared spectrograph, high resolution transmission electron microscope, and selected area electron diffraction measurements showed that the obtained nanoparticles had the amorphous structure and the coordination occurred between zinc sulfide surfaces and BSA in the nanoparticles. In addition, the inhibition effects of BSA-conjugated amorphous zinc sulfide nanoparticles on tumor cells growth were described in detail by cell viability analysis, optical and electron microscopy methods. The results showed that BSA-conjugated amorphous zinc sulfide nanoparticles could inhibit the metabolism and proliferation of human hepatocellular carcinoma cells, and the inhibition was dose dependent. The half maximal inhibitory concentration (IC50) was 0.36 mg/mL. Overall, this study suggested that BSA-conjugated amorphous zinc sulfide nanoparticles had the application potential as cytostatic agents and BSA in the nanoparticles could provide the modifiable site for the nanoparticles to improve their bioactivity or to endow them with the target function.

Uncover the mantle: rediscovering Gregório Lopes palette and technique with a study on the painting "Mater Misericordiae"

NASA Astrophysics Data System (ADS)

Antunes, Vanessa; Candeias, António; Oliveira, Maria J.; Carvalho, Maria L.; Dias, Cristina Barrocas; Manhita, Ana; Francisco, Maria J.; Costa, Sónia; Lauw, Alexandra; Manso, Marta

2016-11-01

Gregório Lopes (c. 1490-1550) was one of the most prominent painters of the renaissance and Mannerism in Portugal. The painting "Mater Misericordiae" made for the Sesimbra Holy House of Mercy, circa 1535-1538, is one of the most significant works of the artist, and his only painting on this theme, being also one of the most significant Portuguese paintings of sixteenth century. The recent restoration provided the possibility to study materially the painting for the first time, with a multianalytical methodology incorporating portable energy-dispersive X-ray fluorescence spectroscopy, scanning electron microscopy-energy-dispersive spectroscopy, micro-X-ray diffraction, micro-Raman spectroscopy and high-performance liquid chromatography coupled to diode array and mass spectrometry detectors. The analytical study was complemented by infrared reflectography, allowing the study of the underdrawing technique and also by dendrochronology to confirm the date of the wooden panels (1535-1538). The results of this study were compared with previous ones on the painter's workshop, and significant differences and similitudes were found in the materials and techniques used.

High-yield production of graphene by liquid-phase exfoliation of graphite.

PubMed

Hernandez, Yenny; Nicolosi, Valeria; Lotya, Mustafa; Blighe, Fiona M; Sun, Zhenyu; De, Sukanta; McGovern, I T; Holland, Brendan; Byrne, Michele; Gun'Ko, Yurii K; Boland, John J; Niraj, Peter; Duesberg, Georg; Krishnamurthy, Satheesh; Goodhue, Robbie; Hutchison, John; Scardaci, Vittorio; Ferrari, Andrea C; Coleman, Jonathan N

2008-09-01

Fully exploiting the properties of graphene will require a method for the mass production of this remarkable material. Two main routes are possible: large-scale growth or large-scale exfoliation. Here, we demonstrate graphene dispersions with concentrations up to approximately 0.01 mg ml(-1), produced by dispersion and exfoliation of graphite in organic solvents such as N-methyl-pyrrolidone. This is possible because the energy required to exfoliate graphene is balanced by the solvent-graphene interaction for solvents whose surface energies match that of graphene. We confirm the presence of individual graphene sheets by Raman spectroscopy, transmission electron microscopy and electron diffraction. Our method results in a monolayer yield of approximately 1 wt%, which could potentially be improved to 7-12 wt% with further processing. The absence of defects or oxides is confirmed by X-ray photoelectron, infrared and Raman spectroscopies. We are able to produce semi-transparent conducting films and conducting composites. Solution processing of graphene opens up a range of potential large-area applications, from device and sensor fabrication to liquid-phase chemistry.

Synthesis and characterization of immobilized Ni-Co bimetallic using Tapanuli clay for catalyst application

DOE Office of Scientific and Technical Information (OSTI.GOV)

Nuryanti,; Juwono, Ariadne L., E-mail: ariadne@sci.ui.ac.id; Krisnandi, Yuni K.

2016-04-19

Heterogeneous catalysts hold various advantages, namely, easy to separate from their products, reusable and regarded as environmental friendly materials. The synthesis of immobilized Ni monometallic, Co monometallic and Ni-Co bimetallic by Tapanuli clay were carried out using intercalation method. Firstly, the synthesis of Na-Bentonite was conducted to provide sufficient area to immobilize bimetal in the clay interlayer. Secondly, Ni, Co and Ni-Co were immobilized in the Tapanuli clay interlayer. Several techniques, such as X-Ray Diffraction, Fourier Transform Infra Red and Energy Dispersive X-Ray Analysis were applied to characterize and compare the properties of the synthesized materials. The results showed thatmore » the insertion of Ni, Co and Ni-Co in the clay interlayer occurred through a cation exchange reaction. The Energy Dispersive X-Ray analysis for Ni-Co bimetallic showed that the immobilized Ni and Co in the clay is in the ratio of 1:1. Catalytic test with Gas Chromatography showed that Ni-Co bimetallic generates a higher yield percentage compared to Ni and Co monometallic.« less

Contribution of Microchemical Surface Analysis of Archaeological Artefacts

NASA Astrophysics Data System (ADS)

Mousser, H.; Madani, A.; Amri, R.; Mousser, A.; Darchen, A.

2009-11-01

Museum CIRTA of the town of Constantine has a collection of more than 35000 coins and statuettes going back to Numide, Roman, Republican, Vandal and Byzantine times and is struck in the name of the cities, of the kingdoms and the empires. Surface analysis of these coins gives information about the chemical composition and leads to recommendations for restoration and preservations. This work is a contribution of microchemical surface study of coin with the effigy of the Numide King Massinissa (Constantine between 3rd and 2nd century before Jesus Christ). The photographic and scanning electron microscopy coupled with energy dispersive spectrometry (SEM + EDS) and diffraction of X-ray (DRX) was used. The optic microscopy (OMP) and SEM pictures of coins showed heterogeneous surface. Scanning electron microscopy coupled with energy dispersive spectrometry identified three basic metals copper (46.06%), antimony (17.74%) and lead (12.06%), (Weight Percentage). The DRX identifies stages (copper and lead) and their crystalline oxides Bindheimite (Pb2Sb2O7) and Bystromite (MgSb2O6) on the coin's surface.

Structural and optical properties of the ZnS/GaSe heterojunctions

NASA Astrophysics Data System (ADS)

Alharbi, S. R.; Abdallaha, Maisam M. A.; Qasrawi, A. F.

2017-11-01

In the current work, the ZnS/GaSe thin film heterojunction interfaces are experimentally designed and characterized by means of x-ray diffraction, scanning electron microscopy, energy dispersion spectroscopy and optical spectroscopy techniques. The heterojunction is observed to exhibit physical nature of formation with an induced crystallization of GaSe by the ZnS substrate. For this heterojunction, the hot probe technique suggested the formation of a p-ZnS/n-GaSe interface. In addition, the designed energy band diagram of the heterojunction which was actualized with the help of the optical spectrophotometric data analysis revealed a respective conduction and valence band offsets of 0.67 and 0.73 eV. On the other hand, the dielectric dispersion analysis and modeling which was studied in the frequency range of 270-1000 THz, have shown that the interfacing of the ZnS with GaSe strongly affects the properties of ZnS as it reduces the number of free carriers, shifts down the plasmon frequency, increases the charge carrier scattering time and results in higher values of drift mobility at Terahertz frequencies.

Exploring Divisibility and Summability of 'Photon' Wave Packets in Nonlinear Optical Phenomena

NASA Technical Reports Server (NTRS)

Prasad, Narasimha; Roychoudhuri, Chandrasekhar

2009-01-01

Formulations for second and higher harmonic frequency up and down conversions, as well as multi photon processes directly assume summability and divisibility of photons. Quantum mechanical (QM) interpretations are completely congruent with these assumptions. However, for linear optical phenomena (interference, diffraction, refraction, material dispersion, spectral dispersion, etc.), we have a profound dichotomy. Most optical engineers innovate and analyze all optical instruments by propagating pure classical electromagnetic (EM) fields using Maxwell s equations and gives only lip-service to the concept "indivisible light quanta". Further, irrespective of linearity or nonlinearity of the phenomena, the final results are always registered through some photo-electric or photo-chemical effects. This is mathematically well modeled by a quadratic action (energy absorption) relation. Since QM does not preclude divisibility or summability of photons in nonlinear & multi-photon effects, it cannot have any foundational reason against these same possibilities in linear optical phenomena. It implies that we must carefully revisit the fundamental roots behind all light-matter interaction processes and understand the common origin of "graininess" and "discreteness" of light energy.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Häusler, I., E-mail: ines.haeusler@bam.de; Dörfel, I., E-mail: Ilona.doerfel@bam.de; Peplinski, B., E-mail: Burkhard.peplinski@bam.de

A model system was used to simulate the properties of tribofilms which form during automotive braking. The model system was prepared by ball milling of a blend of 70 vol.% iron oxides, 15 vol.% molybdenum disulfide and 15 vol.% graphite. The resulting mixture was characterized by X-ray powder diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and various transmission electron microscopic (TEM) methods, including energy dispersive X-ray spectroscopy (EDXS), high resolution investigations (HRTEM) with corresponding simulation of the HRTEM images, diffraction methods such as scanning nano-beam electron diffraction (SNBED) and selected area electron diffraction (SAED). It could be shown that the ballmore » milling caused a reduction of the grain size of the initial components to the nanometer range. Sometimes even amorphization or partial break-down of the crystal structure was observed for MoS{sub 2} and graphite. Moreover, chemical reactions lead to a formation of surface coverings of the nanoparticles by amorphous material, molybdenum oxides, and iron sulfates as derived from XPS. - Highlights: • Ball milling of iron oxides, MoS{sub 2}, and graphite to simulate a tribofilm • Increasing coefficient of friction after ball milling of the model blend • Drastically change of the diffraction pattern of the powder mixture • TEM & XPS showed the components of the milled mixture and the process during milling. • MoS{sub 2} and graphite suffered a loss in translation symmetry or became amorphous.« less

Crystallization and preliminary crystallographic characterization of the origin-binding domain of the bacteriophage λ O replication initiator

DOE Office of Scientific and Technical Information (OSTI.GOV)

Struble, E. B., E-mail: evi.struble@nist.gov; Department of Biochemistry and Molecular Biology, Johns Hopkins Bloomberg School of Public Health, Baltimore, MD 21205; Center for Advanced Research in Biotechnology/NIST, 9600 Gudelsky Drive, Rockville, MD 20850

2007-06-01

Crystallization and preliminary diffraction data of the N-terminal 19–139 fragment of the origin-binding domain of bacteriophage λ O replication initiator are reported. The bacteriophage λ O protein binds to the λ replication origin (oriλ) and serves as the primary replication initiator for the viral genome. The binding energy derived from the binding of O to oriλ is thought to help drive DNA opening to facilitate initiation of DNA replication. Detailed understanding of this process is severely limited by the lack of high-resolution structures of O protein or of any lambdoid phage-encoded paralogs either with or without DNA. The production ofmore » crystals of the origin-binding domain of λ O that diffract to 2.5 Å is reported. Anomalous dispersion methods will be used to solve this structure.« less

Room temperature synthesis of Cu₂O nanospheres: optical properties and thermal behavior.

PubMed

Nunes, Daniela; Santos, Lídia; Duarte, Paulo; Pimentel, Ana; Pinto, Joana V; Barquinha, Pedro; Carvalho, Patrícia A; Fortunato, Elvira; Martins, Rodrigo

2015-02-01

The present work reports a simple and easy wet chemistry synthesis of cuprous oxide (Cu2O) nanospheres at room temperature without surfactants and using different precursors. Structural characterization was carried out by X-ray diffraction, transmission electron microscopy, and scanning electron microscopy coupled with focused ion beam and energy-dispersive X-ray spectroscopy. The optical band gaps were determined from diffuse reflectance spectroscopy. The photoluminescence behavior of the as-synthesized nanospheres showed significant differences depending on the precursors used. The Cu2O nanospheres were constituted by aggregates of nanocrystals, in which an on/off emission behavior of each individual nanocrystal was identified during transmission electron microscopy observations. The thermal behavior of the Cu2O nanospheres was investigated with in situ X-ray diffraction and differential scanning calorimetry experiments. Remarkable structural differences were observed for the nanospheres annealed in air, which turned into hollow spherical structures surrounded by outsized nanocrystals.

Reaction layer formation at the graphite/copper-chromium alloy interface

NASA Technical Reports Server (NTRS)

Devincent, Sandra M.; Michal, Gary M.

1992-01-01

Sessile drop tests were used to obtain information about copper chromium alloys that suitably wet graphite. Characterization of graphite/copper-chromium alloy interfaces subjected to elevated temperatures were conducted using scanning electron micrography, energy dispersive spectroscopy, auger electron spectroscopy, and x ray diffraction analyses. These analyses indicate that during sessile drop tests conducted at 1130 C for one hour, copper alloys containing greater than 0.98 percent chromium form continuous reaction layers of approximately 10 micron thickness. The reaction layers adhere to the graphite surface. The copper wets the reaction layer to form a contact angle of 60 degrees or less. X ray diffraction results indicate that the reaction layer is chromium carbide. The kinetics of reaction layer formation were modelled in terms of bulk diffusion mechanisms. Reaction layer thickness is controlled initially by the diffusion of Cr out of Cu alloy and later by the diffusion of C through chromium carbide.

Enhancement of bioactivity of titanium carbonitride nanocomposite thin films on steels with biosynthesized hydroxyapatite

PubMed Central

Thampi, VV Anusha; Dhandapani, P; Manivasagam, Geetha; Subramanian, B

2015-01-01

Thin films of titanium carbonitride (TiCN) were fabricated by DC magnetron sputtering on medical grade steel. The biocompatibility of the coating was further enhanced by growing hydroxyapatite crystals over the TiCN-coated substrates using biologically activated ammonia from synthetic urine. The coatings were characterized using X-ray diffraction, X-ray photoelectron spectroscopy, scanning electron microscopy (SEM)-energy dispersive spectroscopy, and Raman spectroscopy. The electrochemical behavior of the coatings was determined in simulated body fluid. In addition, hemocompatibility was assessed by monitoring the attachment of platelets on the coating using SEM. The wettability of the coatings was measured in order to correlate with biocompatibility results. Formation of a coating with granular morphology and the preferred orientation was confirmed by SEM and X-ray diffraction results. The hydroxyapatite coating led to a decrease in thrombogenicity, resulting in controlled blood clot formation, hence demonstrating the hemocompatibility of the coating. PMID:26491312

Enhancement of bioactivity of titanium carbonitride nanocomposite thin films on steels with biosynthesized hydroxyapatite.

PubMed

Thampi, V V Anusha; Dhandapani, P; Manivasagam, Geetha; Subramanian, B

2015-01-01

Thin films of titanium carbonitride (TiCN) were fabricated by DC magnetron sputtering on medical grade steel. The biocompatibility of the coating was further enhanced by growing hydroxyapatite crystals over the TiCN-coated substrates using biologically activated ammonia from synthetic urine. The coatings were characterized using X-ray diffraction, X-ray photoelectron spectroscopy, scanning electron microscopy (SEM)-energy dispersive spectroscopy, and Raman spectroscopy. The electrochemical behavior of the coatings was determined in simulated body fluid. In addition, hemocompatibility was assessed by monitoring the attachment of platelets on the coating using SEM. The wettability of the coatings was measured in order to correlate with biocompatibility results. Formation of a coating with granular morphology and the preferred orientation was confirmed by SEM and X-ray diffraction results. The hydroxyapatite coating led to a decrease in thrombogenicity, resulting in controlled blood clot formation, hence demonstrating the hemocompatibility of the coating.

Controlled vapor crystal growth of N a4I r3O8 : A three-dimensional quantum spin liquid candidate

NASA Astrophysics Data System (ADS)

Zheng, Hong; Zhang, Junjie; Stoumpos, Constantinos C.; Ren, Yang; Chen, Yu-Sheng; Dally, Rebecca; Wilson, Stephen D.; Islam, Zahirul; Mitchell, J. F.

2018-04-01

We report the successful bulk single-crystal growth of the hyperkagome lattice iridate N a4I r3O8 (Na438) by vapor transport using a sealed aluminum oxide tube as a container. Crystals were characterized by magnetization, x-ray diffraction, and energy-dispersive x-ray measurements, confirming their identity and properties. Single-crystal x-ray diffraction experiments revealed superlattice peaks indexed on a propagation vector q =(1 /3 ,1 /3 ,1 /3 ) based on the cubic substructure with cell parameter a =8.986 (1 )Å . This superlattice is three-dimensional and fully coherent. Polarization analysis rules out spin and/or orbital order as the underlying origin of the modulation and points to long-range ordering of Na ions at the notionally disordered Na sites as a plausible origin for the observed superlattice.

Thin single-crystalline Bi2(Te1-xSex)3 ternary nanosheets synthesized by a solvothermal technique

NASA Astrophysics Data System (ADS)

Guo, Jing; Jian, Jikang; Zhang, Zhihua; Wu, Rong; Li, Jin; Sun, Yanfei

2016-01-01

Bi2(Te1-xSex)3 ternary nanosheets have been successfully synthesized through a facile solvothermal technique using diethylenetriamine as solvent, where x can vary from 0 to 1. X-ray diffraction (XRD) and Scanning electron microscopy (SEM) indicate that the as-synthesized Bi2(Te1-xSex)3 samples are nanosheets with rhombohedral structure, and the thickness of the nanosheets can be as thin as several nanometers. High resolution transmission electron microscopy (HRTEM) and selected area electron diffraction (SAED) reveal that the nanosheets are single crystalline with a rhombohedral structure. Energy disperse spectroscopy (EDS) and XRD analysis by Vegard's law confirm that the ternary Bi2(Te1-xSex)3 nanosheets have been obtained here. The growth of the nanosheets is discussed based on an amine-based molecular template mechanism that has been employed to synthesize some other metal chalcogenides.

Reaction layer formation at the graphite/copper-chromium alloy interface

NASA Technical Reports Server (NTRS)

Devincent, Sandra M.; Michal, Gary M.

1993-01-01

Sessile drop tests were used to obtain information about copper chromium alloys that suitably wet graphite. Characterization of graphite/copper-chromium alloy interfaces subjected to elevated temperatures were conducted using scanning electron micrography, energy dispersive spectroscopy, Auger electron spectroscopy, and X-ray diffraction analyses. These analyses indicate that during sessile drop tests conducted at 1130 C for one hour, copper alloys containing greater than 0.98 percent chromium form continuous reaction layers of approximately 10 micron thickness. The reaction layers adhere to the graphite surface. The copper wets the reaction layer to form a contact angle of 60 degrees or less. X-ray diffraction results indicate that the reaction layer is chromium carbide. The kinetics of reaction layer formation were modelled in terms of bulk diffusion mechanisms. Reaction layer thickness is controlled initially by the diffusion of Cr out of Cu alloy and later by the diffusion of C through chromium carbide.

Coaxial carbon plasma gun deposition of amorphous carbon films

NASA Technical Reports Server (NTRS)

Sater, D. M.; Gulino, D. A.; Rutledge, S. K.

1984-01-01

A unique plasma gun employing coaxial carbon electrodes was used in an attempt to deposit thin films of amorphous diamond-like carbon. A number of different structural, compositional, and electrical characterization techniques were used to characterize these films. These included scanning electron microscopy, scanning transmission electron microscopy, X ray diffraction and absorption, spectrographic analysis, energy dispersive spectroscopy, and selected area electron diffraction. Optical absorption and electrical resistivity measurements were also performed. The films were determined to be primarily amorphous, with poor adhesion to fused silica substrates. Many inclusions of particulates were found to be present as well. Analysis of these particulates revealed the presence of trace impurities, such as Fe and Cu, which were also found in the graphite electrode material. The electrodes were the source of these impurities. No evidence of diamond-like crystallite structure was found in any of the film samples. Details of the apparatus, experimental procedure, and film characteristics are presented.

Controlled vapor crystal growth of N a 4 I r 3 O 8 : A three-dimensional quantum spin liquid candidate

DOE PAGES

Zheng, Hong; Zhang, Junjie; Stoumpos, Constantinos C.; ...

2018-04-24

In this work, we report the successful bulk single-crystal growth of the hyperkagome lattice iridate Na 4Ir 3O 8 (Na438) by vapor transport using a sealed aluminum oxide tube as a container. Crystals were characterized by magnetization, x-ray diffraction, and energy-dispersive x-ray measurements, confirming their identity and properties. Single-crystal x-ray diffraction experiments revealed superlattice peaks indexed on a propagation vector q=(1/3,1/3,1/3) based on the cubic substructure with cell parameter a=8.986(1)Å. This superlattice is three-dimensional and fully coherent. Polarization analysis rules out spin and/or orbital order as the underlying origin of the modulation and points to long-range ordering of Na ionsmore » at the notionally disordered Na sites as a plausible origin for the observed superlattice.« less

The microstructural characterization of an in situ grown Si{sub 3}N{sub 4} whisker-reinforced BAS glass-ceramic matrix composite

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yu, Feng; Ortiz-Longo, C.R.; White, K.W.

The microstructure of barium aluminum silicate (BAS)/silicon nitride in situ whisker reinforced ceramic matrix composite was examined by X-ray diffraction, transmission electron microscopy, electron diffraction and energy-dispersive X-ray microanalysis. Although the authors can not conclusively exclude the presence of orthorhombic BAS, hexagonal BAS and both {alpha}-Si{sub 3}N{sub 4} and {beta}-Si{sub 3}N{sub 4} were identified in this material. The {beta}-Si{sub 3}N{sub 4} whiskers nucleate and grow in random directions in the nearly continuous matrix of metastable hexacelsian. The crystallization process of the glass phase can be taken almost to completion but a small proportion of residual glass phase is present atmore » the interface and grains-junction. Both whisker-like and equiaxed {beta}-Si{sub 3}N{sub 4} exist in this material.« less

Observation of indium ion migration-induced resistive switching in Al/Mg{sub 0.5}Ca{sub 0.5}TiO{sub 3}/ITO

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lin, Zong-Han; Wang, Yeong-Her, E-mail: yhw@ee.ncku.edu.tw

2016-08-01

Understanding switching mechanisms is very important for resistive random access memory (RRAM) applications. This letter reports an investigation of Al/Mg{sub 0.5}Ca{sub 0.5}TiO{sub 3} (MCTO)/ITO RRAM, which exhibits bipolar resistive switching behavior. The filaments that connect Al electrodes with indium tin oxide electrodes across the MCTO layer at a low-resistance state are identified. The filaments composed of In{sub 2}O{sub 3} crystals are observed through energy-dispersive X-ray spectroscopy, high-resolution transmission electron microscopy, nanobeam diffraction, and comparisons of Joint Committee on Powder Diffraction Standards (JCPDS) cards. Finally, a switching mechanism resulting from an electrical field induced by In{sup 3+} ion migration is proposed.more » In{sup 3+} ion migration forms/ruptures the conductive filaments and sets/resets the RRAM device.« less

Controlled vapor crystal growth of N a 4 I r 3 O 8 : A three-dimensional quantum spin liquid candidate

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zheng, Hong; Zhang, Junjie; Stoumpos, Constantinos C.

In this work, we report the successful bulk single-crystal growth of the hyperkagome lattice iridate Na 4Ir 3O 8 (Na438) by vapor transport using a sealed aluminum oxide tube as a container. Crystals were characterized by magnetization, x-ray diffraction, and energy-dispersive x-ray measurements, confirming their identity and properties. Single-crystal x-ray diffraction experiments revealed superlattice peaks indexed on a propagation vector q=(1/3,1/3,1/3) based on the cubic substructure with cell parameter a=8.986(1)Å. This superlattice is three-dimensional and fully coherent. Polarization analysis rules out spin and/or orbital order as the underlying origin of the modulation and points to long-range ordering of Na ionsmore » at the notionally disordered Na sites as a plausible origin for the observed superlattice.« less

Compact focusing spectrometer: visible (1 eV) to hard x-rays (200 keV).

PubMed

Baronova, E O; Stepanenko, A M; Pereira, N R

2014-11-01

A low-cost spectrometer that covers a wide range of photon energies can be useful to teach spectroscopy, and for simple, rapid measurements of the photon spectrum produced by small plasma devices. The spectrometer here achieves its wide range, nominally from 1 eV to 200 keV, with a series of spherically and cylindrically bent gratings or crystals that all have the same shape and the same radius of curvature; they are complemented by matching apertures and diagnostics on the Rowland circle that serves as the circular part of the spectrometer's vacuum vessel. Spectral lines are easily identified with software that finds their positions from the dispersion of each diffractive element and the known energies of the lines.

Effect of PbO on optical properties of tellurite glass

NASA Astrophysics Data System (ADS)

Elazoumi, S. H.; Sidek, H. A. A.; Rammah, Y. S.; El-Mallawany, R.; Halimah, M. K.; Matori, K. A.; Zaid, M. H. M.

2018-03-01

Binary (1 - x)(TeO2) - x(PbO), x = 0, 0.10, 0.15, 0.20, 0.25, 0.30 mol% glass system was fabricated using melt quenching method. X-ray diffraction (XRD) technique was employed to confirm the amorphous nature. The microanalysis of the major components was performed using energy dispersive EDX and X-ray spectrometry. Both the molar volume and the density were measured. FTIR and UV spectra were recorded at 400-4000 cm-1 and 220-800 nm, respectively. The optical band gap (Eopt), Urbach's energy (Eu), index of refraction (n) were calculated using absorption spectrum fitting (ASF) and derivation of absorption spectrum fitting (DASF) methods. Molar refraction Rm and molecular polarizability αm have been calculated according to (ASF) method.

Measurement of average density and relative volumes in a dispersed two-phase fluid

DOEpatents

Sreepada, Sastry R.; Rippel, Robert R.

1992-01-01

An apparatus and a method are disclosed for measuring the average density and relative volumes in an essentially transparent, dispersed two-phase fluid. A laser beam with a diameter no greater than 1% of the diameter of the bubbles, droplets, or particles of the dispersed phase is directed onto a diffraction grating. A single-order component of the diffracted beam is directed through the two-phase fluid and its refraction is measured. Preferably, the refracted beam exiting the fluid is incident upon a optical filter with linearly varing optical density and the intensity of the filtered beam is measured. The invention can be combined with other laser-based measurement systems, e.g., laser doppler anemometry.

Diffraction inspired unidirectional and bidirectional beam splitting in defect-containing photonic structures without interface corrugations

DOE Office of Scientific and Technical Information (OSTI.GOV)

Colak, Evrim; Serebryannikov, Andriy E., E-mail: andser@amu.edu.pl; Usik, P. V.

2016-05-21

It is shown that strong diffractions and related dual-beam splitting can be obtained at transmission through the nonsymmetric structures that represent two slabs of photonic crystal (PhC) separated by a single coupled-cavity type defect layer, while there are no grating-like corrugations at the interfaces. The basic operation regimes include unidirectional and bidirectional splitting that occur due to the dominant contribution of the first positive and first negative diffraction orders to the transmission, which is typically connected with different manifestations of the asymmetric transmission phenomenon. Being the main component of the resulting transmission mechanism, diffractions appear owing to the effect exertedmore » by the defect layer that works like an embedded diffractive element. Two mechanisms can co-exist in one structure, which differ, among others, in that whether dispersion allows coupling of zero order to a wave propagating in the regular, i.e., defect-free PhC segments or not. The possibility of strong diffractions and efficient splitting related to it strongly depend on the dispersion properties of the Floquet-Bloch modes of the PhC. Existence of one of the studied transmission scenarios is not affected by location of the defect layer.« less

Thermoelectric properties of Co₄Sb₁₂ with Bi₂Te₃ nanoinclusions.

PubMed

Ghosh, Sanyukta; Bisht, Anuj; Karati, Anirudha; Rogl, Gerda; Rogl, Peter F; Murty, B S; Suwas, Satyam; Mallik, Ramesh Chandra

2018-01-08

The figure of merit (zT) of a thermoelectric material can be enhanced by incorporation of nanoinclusions into bulk material. The presence of bismuth telluride (Bi2Te3) nanoinclusions in Co4Sb12 leads to lower phonon thermal conductivity by introducing interfaces and defects; it enhances the average zT between 300-700 K. In the current study, Bi2Te3 nanoparticles were dispersed into bulk Co4Sb12 by ball-milling. The bulk was fabricated by spark plasma sintering (SPS). The presence of Bi2Te3 dispersion in Co4Sb12 was confirmed by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and electron back scattered diffraction (EBSD) technique. Energy dispersive spectroscopy (EDS) showed antimony (Sb) as an impurity phase for higher contents of Bi2Te3 in the sample. The Seebeck coefficient (S) and electrical conductivity () were measured in the temperature range of 350 - 673 K. The negative value of S indicates that most of the charge carriers were electrons. A decrease in S and increase in with Bi2Te3 content are due to the increased carrier concentration, as confirmed by Hall measurement. The thermal conductivity, measured between 423 - 673 K, decreased due to the increased phonon scattering at interfaces. A maximum zT of 0.17 was achieved at 523 K and it did not vary much throughout the temperature range. The experimental results of composites were compared by using effective medium theories. © 2018 IOP Publishing Ltd.

Theory of dispersive microlenses

NASA Technical Reports Server (NTRS)

Herman, B.; Gal, George

1993-01-01

A dispersive microlens is a miniature optical element which simultaneously focuses and disperses light. Arrays of dispersive mircolenses have potential applications in multicolor focal planes. They have a 100 percent optical fill factor and can focus light down to detectors of diffraction spot size, freeing up areas on the focal plane for on-chip analog signal processing. Use of dispersive microlenses allows inband color separation within a pixel and perfect scene registration. A dual-color separation has the potential for temperature discrimination. We discuss the design of dispersive microlenses and present sample results for efficient designs.

A pseudo-tetragonal tungsten bronze superstructure: a combined solution of the crystal structure of K6.4(Nb,Ta)(36.3)O94 with advanced transmission electron microscopy and neutron diffraction.

PubMed

Paria Sena, Robert; Babaryk, Artem A; Khainakov, Sergiy; Garcia-Granda, Santiago; Slobodyanik, Nikolay S; Van Tendeloo, Gustaaf; Abakumov, Artem M; Hadermann, Joke

2016-01-21

The crystal structure of the K6.4Nb28.2Ta8.1O94 pseudo-tetragonal tungsten bronze-type oxide was determined using a combination of X-ray powder diffraction, neutron diffraction and transmission electron microscopy techniques, including electron diffraction, high angle annular dark field scanning transmission electron microscopy (HAADF-STEM), annular bright field STEM (ABF-STEM) and energy-dispersive X-ray compositional mapping (STEM-EDX). The compound crystallizes in the space group Pbam with unit cell parameters a = 37.468(9) Å, b = 12.493(3) Å, c = 3.95333(15) Å. The structure consists of corner sharing (Nb,Ta)O6 octahedra forming trigonal, tetragonal and pentagonal tunnels. All tetragonal tunnels are occupied by K(+) ions, while 1/3 of the pentagonal tunnels are preferentially occupied by Nb(5+)/Ta(5+) and 2/3 are occupied by K(+) in a regular pattern. A fractional substitution of K(+) in the pentagonal tunnels by Nb(5+)/Ta(5+) is suggested by the analysis of the HAADF-STEM images. In contrast to similar structures, such as K2Nb8O21, also parts of the trigonal tunnels are fractionally occupied by K(+) cations.

Characterization and electron-energy-loss spectroscopy on NiV and NiMo superlattices

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mahmood, S.H.

1986-01-01

NiV superlattices with periods (A) ranging from 15 to 80 A, and NiMo superlattices with from 14 to 110 A were studied using X-ray Diffraction (XRD), Electron Diffraction (ED), Energy-Dispersive X-Ray (EDX) microanalysis, and Electron Energy Loss Spectroscopy (EELS). Both of these systems have sharp superlattice-to-amorphous (S-A) transitions at about empty set = 17A. Superlattices with empty set around the S-A boundary were found to have large local variations in the in-plane grain sizes. Except for a few isolated regions, the chemical composition of the samples were found to be uniform. In samples prepared at Argonne National Laboratory (ANL), mostmore » places studied with EELS showed changes in the EELS spectrum with decreasing empty set. An observed growth in a plasmon peak at approx. 10ev in both NiV and NiMo as empty set decreased down to 19 A is attributed to excitation of interface plasmons. Consistent with this attribution, the peak height shrank in the amorphous samples. The width of this peak is consistent with the theory. The sift in this peak down to 9 ev with decreasing empty set in NiMo is not understood.« less

Off-axis holographic lens spectrum-splitting photovoltaic system for direct and diffuse solar energy conversion.

PubMed

Vorndran, Shelby D; Chrysler, Benjamin; Wheelwright, Brian; Angel, Roger; Holman, Zachary; Kostuk, Raymond

2016-09-20

This paper describes a high-efficiency, spectrum-splitting photovoltaic module that uses an off-axis volume holographic lens to focus and disperse incident solar illumination to a rectangular shaped high-bandgap indium gallium phosphide cell surrounded by strips of silicon cells. The holographic lens design allows efficient collection of both direct and diffuse illumination to maximize energy yield. We modeled the volume diffraction characteristics using rigorous coupled-wave analysis, and simulated system performance using nonsequential ray tracing and PV cell data from the literature. Under AM 1.5 illumination conditions the simulated module obtained a 30.6% conversion efficiency. This efficiency is a 19.7% relative improvement compared to the more efficient cell in the system (silicon). The module was also simulated under a typical meteorological year of direct and diffuse irradiance in Tucson, Arizona, and Seattle, Washington. Compared to a flat panel silicon module, the holographic spectrum splitting module obtained a relative improvement in energy yield of 17.1% in Tucson and 14.0% in Seattle. An experimental proof-of-concept volume holographic lens was also fabricated in dichromated gelatin to verify the main characteristics of the system. The lens obtained an average first-order diffraction efficiency of 85.4% across the aperture at 532 nm.

Phase transformation from cubic ZnS to hexagonal ZnO by thermal annealing

NASA Astrophysics Data System (ADS)

Mahmood, K.; Asghar, M.; Amin, N.; Ali, Adnan

2015-03-01

We have investigated the mechanism of phase transformation from ZnS to hexagonal ZnO by high-temperature thermal annealing. The ZnS thin films were grown on Si (001) substrate by thermal evaporation system using ZnS powder as source material. The grown films were annealed at different temperatures and characterized by X-ray diffraction (XRD), photoluminescence (PL), four-point probe, scanning electron microscope (SEM) and energy dispersive X-ray diffraction (EDX). The results demonstrated that as-deposited ZnS film has mixed phases but high-temperature annealing leads to transition from ZnS to ZnO. The observed result can be explained as a two-step process: (1) high-energy O atoms replaced S atoms in lattice during annealing process, and (2) S atoms diffused into substrate and/or diffused out of the sample. The dissociation energy of ZnS calculated from the Arrhenius plot of 1000/T versus log (resistivity) was found to be 3.1 eV. PL spectra of as-grown sample exhibits a characteristic green emission at 2.4 eV of ZnS but annealed samples consist of band-to-band and defect emission of ZnO at 3.29 eV and 2.5 eV respectively. SEM and EDX measurements were additionally performed to strengthen the argument.

Synthesis and Characterization of the First Liquid Single Source Precursors for the Deposition of Ternary Chalcopyrite (CuInS2) Thin Film Materials

NASA Technical Reports Server (NTRS)

Banger, Kulbinder K.; Cowen, Jonathan; Hepp, Aloysius

2002-01-01

Molecular engineering of ternary single source precursors based on the [{PBu3}2Cu(SR')2In(SR')2] architecture have afforded the first liquid CIS ternary single source precursors (when R = Et, n-Pr), which are suitable for low temperature deposition (< 350 C). Thermogravimetric analyses (TGA) and modulated-differential scanning calorimetry (DSC) confirm their liquid phase and reduced stability. X-ray diffraction studies, energy dispersive analyzer (EDS), and scanning electron microscopy (SEM) support the formation of the single-phase chalcopyrite CuInS2 at low temperatures.

Characterisation of mineral deposition systems associated with rock art in the Kimberley region of northwest Australia.

PubMed

Green, Helen; Gleadow, Andrew; Finch, Damien

2017-10-01

This data article contains mineralogical and chemical data from mineral accretions sampled from rock art shelters in the Kimberley region of north west Australia. The accretions were collected both on and off pigment and engraved rock art of varying styles observed in the Kimberley with an aim of providing a thorough understanding of the formation and preservation of such materials in the context of dating [1]. This contribution includes processed powder X-ray Diffraction data, Scanning Electron Microscopy energy dispersive spectroscopy data, and Laser Ablation ICP-MS trace element mapping data.

Boehmite nanostructures preparation by hydrothermal method from anodic aluminium oxide membrane.

PubMed

Yang, X; Wang, J Y; Pan, H Y

2009-02-01

Boehmite nanostructures were successfully synthesized from porous anodic aluminium oxide (AAO) membrane by a simple and efficient hydro-thermal method. The experiment used high purity alumina as raw material, and the whole reaction process avoided superfluous impurities to be introduced. Thus, the purity of Boehmite products was ensured. The examinations of the morphology and structure were carried out by atomic force microscope (AFM), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Composition of the specimens was analyzed using energy dispersive X-ray spectroscope (EDX) and X-ray diffraction (XRD). Based on these observations the growth process was analyzed.

Structural, optical and dielectric properties of graphene oxide

NASA Astrophysics Data System (ADS)

Bhargava, Richa; Khan, Shakeel

2018-05-01

The Modified Hummers method has been used to synthesize Graphene oxide nanoparticles. Microstructural analyses were carried out by X-ray diffraction and Fourier transform infrared spectroscopy. Optical properties were studied by UV-visible spectroscopy in the range of 200-700 nm. The energy band gap was calculated with the help of Tauc relation. The frequency dependence of dielectric constant and dielectric loss were studied over a range of the frequency 75Hz to 5MHz at room temperature. The dispersion in dielectric constant can be explained with the help of Maxwell-Wagner model in studied nanoparticles.

Annealing effects in plated-wire memory elements. I - Interdiffusion of copper and Permalloy.

NASA Technical Reports Server (NTRS)

Knudson, C. I.; Kench, J. R.

1971-01-01

Results of investigations using X-ray diffraction and electron-beam microprobe techniques have shown that copper and Permalloy platings interdiffuse at low temperatures when plated-wire memory elements are annealed for times as short as 50 hr. Measurable interdiffusion between Permalloy platings and gold substrates does not occur in similar conditions. Both magnetic and compositional changes during aging are found to occur by a thermally activated process with activation energies around 38 kcal/mol. It is shown, however, that copper-diffusion and magnetic-dispersion changes during aging are merely concurrent processes, neither being the other's cause.

The effect of ultrasonic irradiation on the crystallinity of nano-hydroxyapatite produced via the wet chemical method.

PubMed

Barbosa, Michelle C; Messmer, Nigel R; Brazil, Tayra R; Marciano, Fernanda R; Lobo, Anderson O

2013-07-01

Nanohydroxyapatite (nHAp) powders were produced via aqueous precipitation by adopting four different experimental conditions, assisted or non-assisted by ultrasound irradiation (UI). The nHAp powders were characterized by X-ray diffraction, energy-dispersive X-ray fluorescence, Raman and attenuated total reflection Fourier transform infrared spectroscopies, which showed typical surface chemical compositions of nHAp. Analysis found strong connections between UI and the crystallization process, crystal growth properties, as well as correlations between calcination and substitution reactions. Copyright © 2013 Elsevier B.V. All rights reserved.

Composition, speciation and distribution of iron minerals in Imperata cylindrica.

PubMed

Amils, Ricardo; de la Fuente, Vicenta; Rodríguez, Nuria; Zuluaga, Javier; Menéndez, Nieves; Tornero, Jesús

2007-05-01

A comparative study of the roots, rhizomes and leaves of an iron hyperaccumulator plant, Imperata cylindrica, isolated from the banks of an extreme acidic environment, using complementary techniques: Mösbauer spectroscopy (MS), X-ray diffraction (XRD), scanning electron microscopy (SEM) coupled to energy-dispersive X-ray microanalysis (EDAX) and transmission electron microscopy (TEM), has shown that two main biominerals, jarosite and ferrihydrate-ferritin, accumulate in the different tissues. Jarosite accumulates mainly in roots and rhizomes, while ferritin has been detected in all the structures. A model of iron management in I. cylindrica is presented.

Ionic liquid-templated preparation of mesoporous silica embedded with nanocrystalline sulfated zirconia

NASA Astrophysics Data System (ADS)

Ward, Antony J.; Pujari, Ajit A.; Costanzo, Lorenzo; Masters, Anthony F.; Maschmeyer, Thomas

2011-12-01

A series of mesoporous silicas impregnated with nanocrystalline sulphated zirconia was prepared by a sol-gel process using an ionic liquid-templated route. The physicochemical properties of the mesoporous sulphated zirconia materials were studied using characterisation techniques such as inductively coupled optical emission spectroscopy, X-ray diffraction, transmission electron microscopy, energy-dispersive X-ray microanalysis, elemental analysis and X-ray photoelectron spectroscopy. Analysis of the new silicas indicates isomorphous substitution of silicon with zirconium and reveals the presence of extremely small (< 10 nm) polydispersed zirconia nanoparticles in the materials with zirconium loadings from 27.77 to 41.4 wt.%.

Inelastic neutron scattering experiments with the monochromatic imaging mode of the RITA-II spectrometer

NASA Astrophysics Data System (ADS)

Bahl, C. R. H.; Lefmann, K.; Abrahamsen, A. B.; Rønnow, H. M.; Saxild, F.; Jensen, T. B. S.; Udby, L.; Andersen, N. H.; Christensen, N. B.; Jakobsen, H. S.; Larsen, T.; Häfliger, P. S.; Streule, S.; Niedermayer, Ch.

2006-05-01

Recently a monochromatic multiple data taking mode has been demonstrated for diffraction experiments using a RITA type cold neutron spectrometer with a multi-bladed analyser and a position-sensitive detector. Here, we show how this mode can be used in combination with a flexible radial collimator to perform real inelastic neutron scattering experiments. We present the results from inelastic powder, single crystal dispersion and single crystal constant energy mapping experiments. The advantages and complications of performing these experiments are discussed along with a comparison between the imaging mode and the traditional monochromatic focussing mode.

Large-Scale Synthesis of Tin-Doped Indium Oxide Nanofibers Using Water as Solvent

NASA Astrophysics Data System (ADS)

Altecor, Aleksey; Mao, Yuanbing; Lozano, Karen

2012-09-01

Here we report the successful fabrication of tin-doped indium oxide (ITO) nanofibers using a scalable Forcespinning™ method. In this environmentally-friendly process, water was used as the only solvent for both Polyvinylpyrrolidone (PVP, the sacrificial polymer) and the metal chloride precursor salts. The obtained precursor nanofiber mats were calcinated at temperatures ranging from 500-800°C to produce ITO nanofibers with diameters as small as 400 nm. The developed ITO nanofibers were characterized by scanning electron microscopy, energy-dispersive X-ray spectroscopy, X-ray photoelectron spectroscopy and X-ray diffraction analysis.

Pressure dependence of the optical phonon frequencies and the transverse effective charge in AlSb

NASA Astrophysics Data System (ADS)

Ves, S.; Strössner, K.; Cardona, M.

1986-02-01

The first order Raman scattering by TO and LO phonons has been measured in AlSb under hydrostatic' pressures up to its phase transition. The Raman frequencies increase nearly linear while the transverse effective charge e ∗T are compared with estimates based on pseudopotential and on LCAO calculation. In order to obtain from the measured pressure dependence the corresponding volume coefficients the bulk modulus B O and its pressure derivative BOˌ = {dBO}/{dP} was measured by energy-dispersive X-ray diffraction (B O = 55.1 GPa and BOˌ = 4.55 ).

Zinc sulfide in intestinal cell granules of Ancylostoma caninum adults

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gianotti, A.J.; Clark, D.T.; Dash, J.

1991-04-01

A source of confusion has existed since the turn of the century about the reddish brown, weakly birefringent 'sphaerocrystals' located in the intestines of strongyle nematodes, Strongylus and Ancylostoma. X-ray diffraction and energy dispersive spectrometric analyses were used for accurate determination of the crystalline order and elemental composition of the granules in the canine hookworm Ancylostoma caninum. The composition of the intestinal pigmented granules was identified unequivocally as zinc sulfide. It seems most probable that the granules serve to detoxify high levels of metallic ions (specifically zinc) present due to the large intake of host blood.

Structural and optical properties of furfurylidenemalononitrile thin films

NASA Astrophysics Data System (ADS)

Ali, H. A. M.

2013-03-01

Thin films of furfurylidenemalononitrile (FMN) were deposited on different substrates at room temperature by thermal evaporation technique under a high vacuum. The structure of the powder was confirmed by Fourier transformation infrared (FTIR) technique. The unit cell dimensions were determined from X-ray diffraction (XRD) studies. The optical properties were investigated using spectrophotometric measurements of the transmittance and reflectance at normal incidence of light in the wavelength range from 200 to 2500 nm. The refractive index (n), the absorption index (k) and the absorption coefficient (α) were calculated. The analysis of the spectral behavior of the absorption coefficient in the absorption region revealed an indirect allowed transition. The refractive index dispersion was analyzed using the single oscillator model. Some dispersion parameters were estimated. Complex dielectric function and optical conductivity were determined. The influence of the irradiation with high-energy X-rays (6 MeV) on the studied properties was also investigated.

Non-Noble Metal Oxide Catalysts for Methane Catalytic Combustion: Sonochemical Synthesis and Characterisation

PubMed Central

Jędrzejczyk, Roman J.; Dziedzicka, Anna; Kuterasiński, Łukasz; Sitarz, Maciej

2017-01-01

The aim of this study was to obtain nanocrystalline mixed metal-oxide–ZrO2 catalysts via a sonochemically-induced preparation method. The effect of a stabiliser’s addition on the catalyst parameters was investigated by several characterisation methods including X-ray Diffraction (XRD), nitrogen adsorption, X-ray fluorescence (XRF), scanning electron microscopy (SEM) equipped with energy dispersive X-ray spectrometer (EDS), transmission electron microscopy (TEM) and µRaman. The sonochemical preparation method allowed us to manufacture the catalysts with uniformly dispersed metal-oxide nanoparticles at the support surface. The catalytic activity was tested in a methane combustion reaction. The activity of the catalysts prepared by the sonochemical method was higher than that of the reference catalysts prepared by the incipient wetness method without ultrasonic irradiation. The cobalt and chromium mixed zirconia catalysts revealed their high activities, which are comparable with those presented in the literature. PMID:28686190

Micro-XRF for characterization of Moroccan glazed ceramics and Portuguese tiles

NASA Astrophysics Data System (ADS)

Guilherme, A.; Manso, M.; Pessanha, S.; Zegzouti, A.; Elaatmani, M.; Bendaoud, R.; Coroado, J.; dos Santos, J. M. F.; Carvalho, M. L.

2013-02-01

A set of enamelled terracotta samples (Zellij) collected from five different monuments in Morocco were object of study. With the aim of characterizing these typically Moroccan artistic objects, X-ray spectroscopic techniques were used as analytical tool to provide elemental and compound information. A lack of information about these types of artistic ceramics is found by the research through international scientific journals, so this investigation is an opportunity to fulfill this gap. For this purpose, micro-Energy Dispersive X-ray Fluorescence (μ-EDXRF), and wavelength dispersive X-ray Fluorescence (WDXRF) and X-ray Diffraction (XRD) were the chosen methods. As complementary information, a comparison with other sort of artistic pottery objects is given, more precisely with Portuguese glazed wall tiles (Azulejos), based in the Islamic pottery traditions. Differences between these two types of decorative pottery were found and presented in this manuscript.

Synthesis and anti-fungal effect of silver nanoparticles–chitosan composite particles

PubMed Central

Wang, Lung-Shuo; Wang, Chih-Yu; Yang, Chih-Hui; Hsieh, Chen-Ling; Chen, Szu-Yu; Shen, Chi-Yen; Wang, Jia-Jung; Huang, Keng-Shiang

2015-01-01

Silver nanoparticles have been used in various fields, and several synthesis processes have been developed. The stability and dispersion of the synthesized nanoparticles is vital. The present article describes a novel approach for one-step synthesis of silver nanoparticles–embedded chitosan particles. The proposed approach was applied to simultaneously obtain and stabilize silver nanoparticles in a chitosan polymer matrix in-situ. The diameter of the synthesized chitosan composite particles ranged from 1.7 mm to 2.5 mm, and the embedded silver nanoparticles were measured to be 15±3.3 nm. Further, the analyses of ultraviolet-visible spectroscopy, energy dispersive spectroscopy, and X-ray diffraction were employed to characterize the prepared composites. The results show that the silver nanoparticles were distributed over the surface and interior of the chitosan spheres. The fabricated spheres had macroporous property, and could be used for many applications such as fungicidal agents in the future. PMID:25878501

Synthesis and Characterization of Multi Wall Carbon Nanotubes (MWCNT) Reinforced Sintered Magnesium Matrix Composites

NASA Astrophysics Data System (ADS)

Vijaya Bhaskar, S.; Rajmohan, T.; Palanikumar, K.; Bharath Ganesh Kumar, B.

2016-04-01

Metal matrix composites (MMCs) reinforced with ceramic nano particles (less than 100 nm), termed as metal matrix nano composites (MMNCs), can overcome those disadvantages associated with the conventional MMCs. MMCs containing carbon nanotubes are being developed and projected for diverse applications in various fields of engineering like automotive, avionic, electronic and bio-medical sectors. The present investigation deals with the synthesis and characterization of hybrid magnesium matrix reinforced with various different wt% (0-0.45) of multi wall carbon nano tubes (MWCNT) and micro SiC particles prepared through powder metallurgy route. Microstructure and mechanical properties such as micro hardness and density of the composites were examined. Microstructure of MMNCs have been investigated by scanning electron microscope, X-ray diffraction and energy dispersive X-ray spectroscopy (EDS) for better observation of dispersion of reinforcement. The results indicated that the increase in wt% of MWCNT improves the mechanical properties of the composite.

Oxidation and emittance of superalloys in heat shield applications

NASA Technical Reports Server (NTRS)

Wiedemann, K. E.; Clark, R. K.; Unnam, J.

1986-01-01

Recently developed superalloys that form alumina coatings have a high potential for heat shield applications for advanced aerospace vehicles at temperatures above 1095C. Both INCOLOY alloy MA 956 (of the Inco Alloys International, Inc.), an iron-base oxide-dispersion-strengthened alloy, and CABOT alloy No. 214 (of the Cabot Corporation), an alumina-forming nickel-chromium alloy, have good oxidation resistance and good elevated temperature strength. The oxidation resistance of both alloys has been attributed to the formation of a thin alumina layer (alpha-Al2O3) at the surface. Emittance and oxidation data were obtained for simulated Space Shuttle reentry conditions using a hypersonic arc-heated wind tunnel. The surface oxides and substrate alloys were characterized using X-ray diffraction and scanning and transmission electron microscopy with an energy-dispersive X-ray analysis unit. The mass loss and emittance characteristics of the two alloys are discussed.

Organic holographic polymer dispersed liquid crystal distributed feedback laser from different diffraction orders

NASA Astrophysics Data System (ADS)

Liu, Minghuan; Liu, Yonggang; Zhang, Guiyang; Peng, Zenghui; Li, Dayu; Ma, Ji; Xuan, Li

2016-11-01

Holographic polymer dispersed liquid crystal (HPDLC) based distributed feedback (DFB) lasers were prepared with poly (-methoxy-5-(2‧-ethyl-hexyloxy)-1,4-phenylene-vinylene) (MEH-PPV) film as the active medium layer. The HPDLC grating film was fabricated via holographic induced photopolymerization. The pure film spectra of MEH-PPV and the amplified spontaneous emission (ASE) spectrum were investigated. The laser device was single-longitudinal mode operation. The tunability of the HPDLC DFB laser was achieved by selecting different grating periods. The lasing performances were also characterized and compared from different diffraction orders. The lasing threshold increased with the diffraction order and the third order laser possessed the largest conversion efficiency in this device. The experimental results were in good agreement with the theoretical calculations.

Intercalated chitosan/hydroxyapatite nanocomposites: Promising materials for bone tissue engineering applications.

PubMed

Nazeer, Muhammad Anwaar; Yilgör, Emel; Yilgör, Iskender

2017-11-01

Preparation and characterization of chitosan/hydroxyapatite (CS/HA) nanocomposites displaying an intercalated structure is reported. Hydroxyapatite was synthesized through sol-gel process. Formic acid was introduced as a new solvent to obtain stable dispersions of nano-sized HA particles in polymer solution. CS/HA dispersions with HA contents of 5, 10 and 20% by weight were prepared. Self-assembling of HA nanoparticles during the drying of the solvent cast films led to the formation of homogeneous CS/HA nanocomposites. Composite films were analyzed by scanning electron microscopy (SEM), atomic force microscopy (AFM), energy dispersive X-rays (EDX) analysis, Fourier transform infrared (FTIR) spectroscopy, X-rays diffraction (XRD) analysis and thermogravimetric analysis (TGA). SEM and AFM confirmed the presence of uniformly distributed HA nanoparticles on the chitosan matrix surface. XRD patterns and cross-sectional SEM images showed the formation of layered nanocomposites. Complete degradation of chitosan matrix in TGA experiments, led to the formation of nanoporous 3D scaffolds containing hydroxyapatite, β-tricalcium phosphate and calcium pyrophosphate. CS/HA composites can be considered as promising materials for bone tissue engineering applications. Copyright © 2017 Elsevier Ltd. All rights reserved.

Microscopy of Alloy Formation on Arc Plasma Sintered Oxide Dispersion Strengthen (ODS) Steel

NASA Astrophysics Data System (ADS)

Bandriyana, B.; Sujatno, A.; Salam, R.; Dimyati, A.; Untoro, P.

2017-07-01

The oxide dispersed strengthened (ODS) alloys steel developed as structure material for nuclear power plants (NPP) has good resistant against creep due to their unique microstructure. Microscopy investigation on the microstructure formation during alloying process especially at the early stages was carried out to study the correlation between structure and property of ODS alloys. This was possible thanks to the arc plasma sintering (APS) device which can simulate the time dependent alloying processes. The ODS sample with composition of 88 wt.% Fe and 12 wt.% Cr powder dispersed with 1 wt.% ZrO2 nano powder was mixed in a high energy milling, isostatic compressed to form sample coins and then alloyed in APS. The Scanning Electron Microscope (SEM) with X-ray Diffraction Spectroscopy (EDX) line scan and mapping was used to characterize the microstructure and elemental composition distribution of the samples. The alloying process with unification of each Fe and Cr phase continued by the alloying formation of Fe-Cr by inter-diffusion of both Fe and Cr and followed by the improvement of the mechanical properties of hardness.

Ex Situ Investigation of Anisotropic Interconnection in Silicon-Titanium-Nickel Alloy Anode Material

DOE PAGES

Cho, Jong -Soo; Alaboina, Pankaj Kumar; Kang, Chan -Soon; ...

2017-03-10

Herein we investigate the nanostructural evolution of Silicon-Titanium-Nickel (Si-Ti-Ni) ternary alloy material synthesized by melt spinning process for advanced lithium-ion battery anode. The synthesized material was found to have nano-Silicon particles dispersed in the Ti 4Ni 4Si 7 (STN) alloy buffering matrix and was characterized by X-ray diffraction (XRD), High resolution- transmission electron microscope (HR-TEM), Scanning transmission electron microscopes - energy dispersive X-ray spectrometer (STEM-EDS), and electrochemical performance test. The role of STN matrix is to accommodate the volume expansion stresses of the dispersed Si nanoparticles. However, an interesting behavior was observed during cycling. The Si nanoparticles were observed tomore » form interconnection channels growing through the weak STN matrix cracks and evolving to a network isolating the STN matrix into small puddles. In conclusion, this unique nanostructural evolution of Si particles and isolation of the STN matrix failing to offer significant buffering effect to the grown Si network eventually accelerates more volume expansions during cycling due to less mechanical confinement and leads to performance degradation and poor cycle stability.« less

High diffraction efficiency of three-layer diffractive optics designed for wide temperature range and large incident angle.

PubMed

Mao, Shan; Cui, Qingfeng; Piao, Mingxu; Zhao, Lidong

2016-05-01

A mathematical model of diffraction efficiency and polychromatic integral diffraction efficiency affected by environment temperature change and incident angle for three-layer diffractive optics with different dispersion materials is put forward, and its effects are analyzed. Taking optical materials N-FK5 and N-SF1 as the substrates of multilayer diffractive optics, the effect on diffraction efficiency and polychromatic integral diffraction efficiency with intermediate materials POLYCARB is analyzed with environment temperature change as well as incident angle. Therefore, three-layer diffractive optics can be applied in more wide environmental temperature ranges and larger incident angles for refractive-diffractive hybrid optical systems, which can obtain better image quality. Analysis results can be used to guide the hybrid imaging optical system design for optical engineers.

Processing thermally labile drugs by hot-melt extrusion: The lesson with gliclazide.

PubMed

Huang, Siyuan; O'Donnell, Kevin P; Delpon de Vaux, Sophie M; O'Brien, John; Stutzman, John; Williams, Robert O

2017-10-01

The formation of molecularly dispersed amorphous solid dispersions by the hot-melt extrusion technique relies on the thermal and mechanical energy inputs, which can cause chemical degradation of drugs and polymeric carriers. Additionally, drug degradation may be exacerbated as drugs convert from a more stable crystalline form to a higher energy amorphous form. Therefore, it is imperative to study how drug degrades and evaluate methods to minimize drug degradation during the extrusion process. In this work, gliclazide was used as a model thermally labile drug for the degradation kinetics and process optimization studies. Preformulation studies were conducted using thermal analyses, and liquid chromatography-mass spectroscopy to identify drug degradation pathways and to determine initial extrusion conditions. Formulations containing 10% drug and 90% AFFINISOL™ HPMC HME 100LV were then extruded using a twin screw extruder, and the extrudates were characterized using X-ray powder diffraction, modulated dynamic scanning calorimetry, and potency testing to evaluate physicochemical properties. The energies of activation for both amorphous gliclazide, crystalline gliclazide, and gliclazide solution were calculated using the Arrhenius equation to further guide the extrusion optimization process. Preformulation studies identify two hydrolysis degradation pathways of gliclazide at elevated temperatures. The activation energy study indicates a significantly higher degradation rate for the amorphous gliclazide compared to the crystalline form. After optimization of the hot-melt extrusion process, including improved screw designs, machine setup, and processing conditions, gliclazide amorphous solid dispersion with ∼95% drug recovery was achieved. The ability to process thermally labile drugs and polymers using hot-melt extrusion will significantly expand the possible applications of this manufacturing process. Copyright © 2017 Elsevier B.V. All rights reserved.

Optical-diffraction method for determining crystal orientation

DOEpatents

Sopori, B.L.

1982-05-07

Disclosed is an optical diffraction technique for characterizing the three-dimensional orientation of a crystal sample. An arbitrary surface of the crystal sample is texture etched so as to generate a pseudo-periodic diffraction grating on the surface. A laser light beam is then directed onto the etched surface, and the reflected light forms a farfield diffraction pattern in reflection. Parameters of the diffraction pattern, such as the geometry and angular dispersion of the diffracted beam are then related to grating shape of the etched surface which is in turn related to crystal orientation. This technique may be used for examining polycrystalline silicon for use in solar cells.

Novel anode catalyst for direct methanol fuel cells.

PubMed

Basri, S; Kamarudin, S K; Daud, W R W; Yaakob, Z; Kadhum, A A H

2014-01-01

PtRu catalyst is a promising anodic catalyst for direct methanol fuel cells (DMFCs) but the slow reaction kinetics reduce the performance of DMFCs. Therefore, this study attempts to improve the performance of PtRu catalysts by adding nickel (Ni) and iron (Fe). Multiwalled carbon nanotubes (MWCNTs) are used to increase the active area of the catalyst and to improve the catalyst performance. Electrochemical analysis techniques, such as energy dispersive X-ray spectrometry (EDX), X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), and X-ray photoelectron spectroscopy (XPS), are used to characterize the kinetic parameters of the hybrid catalyst. Cyclic voltammetry (CV) is used to investigate the effects of adding Fe and Ni to the catalyst on the reaction kinetics. Additionally, chronoamperometry (CA) tests were conducted to study the long-term performance of the catalyst for catalyzing the methanol oxidation reaction (MOR). The binding energies of the reactants and products are compared to determine the kinetics and potential surface energy for methanol oxidation. The FESEM analysis results indicate that well-dispersed nanoscale (2-5 nm) PtRu particles are formed on the MWCNTs. Finally, PtRuFeNi/MWCNT improves the reaction kinetics of anode catalysts for DMFCs and obtains a mass current of 31 A g(-1) catalyst.

Novel Anode Catalyst for Direct Methanol Fuel Cells

PubMed Central

Basri, S.; Kamarudin, S. K.; Daud, W. R. W.; Yaakob, Z.; Kadhum, A. A. H.

2014-01-01

PtRu catalyst is a promising anodic catalyst for direct methanol fuel cells (DMFCs) but the slow reaction kinetics reduce the performance of DMFCs. Therefore, this study attempts to improve the performance of PtRu catalysts by adding nickel (Ni) and iron (Fe). Multiwalled carbon nanotubes (MWCNTs) are used to increase the active area of the catalyst and to improve the catalyst performance. Electrochemical analysis techniques, such as energy dispersive X-ray spectrometry (EDX), X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), and X-ray photoelectron spectroscopy (XPS), are used to characterize the kinetic parameters of the hybrid catalyst. Cyclic voltammetry (CV) is used to investigate the effects of adding Fe and Ni to the catalyst on the reaction kinetics. Additionally, chronoamperometry (CA) tests were conducted to study the long-term performance of the catalyst for catalyzing the methanol oxidation reaction (MOR). The binding energies of the reactants and products are compared to determine the kinetics and potential surface energy for methanol oxidation. The FESEM analysis results indicate that well-dispersed nanoscale (2–5 nm) PtRu particles are formed on the MWCNTs. Finally, PtRuFeNi/MWCNT improves the reaction kinetics of anode catalysts for DMFCs and obtains a mass current of 31 A g−1 catalyst. PMID:24883406

Effects of copper on the preparation and characterization of Na-Ca-P borate glasses.

PubMed

Shailajha, S; Geetha, K; Vasantharani, P; Sheik Abdul Kadhar, S P

2015-03-05

Glasses in the system Na2O-CaO-B2O3-P2O5: CuO have been prepared by melt quenching at 1200°C and rapidly cooling at room temperature. The structural, optical and thermal properties have been investigated using X-ray diffraction (XRD), ultraviolet-visible (UV-VIS) spectroscopy, thermogravimetric-differential thermal analysis (TG-DTA), Fourier transform infrared (FTIR) spectroscopy, high resolution scanning electron microscopy (HRSEM) with energy dispersive X-ray (EDX) spectroscopy and high resolution transmission electron microscope (HRTEM) with energy dispersive X-ray (EDAX). The amorphous and crystalline nature of these samples was verified by XRD. Glass transition, crystallization and thermal stability were determined by TG-DTA investigations. Direct optical energy band gaps before and after doping with different percents of copper oxide were evaluated from 4.81eV to 2.99eV indicated the role of copper in the glassy matrix by UV spectra. FTIR spectrum reveals characteristic absorption bands due to various groups of triangular and tetrahedral borate network. Due to the amorphous nature, the particles like agglomerates on the glass surface were investigated by the HRSEM analysis. The crystalline nature of the samples in XRD is confirmed by SAED pattern using HRTEM. Copyright © 2014 Elsevier B.V. All rights reserved.

Diffraction of a plane wave on two-dimensional conductive structures and a surface wave

NASA Astrophysics Data System (ADS)

Davidovich, Mikhael V.

2018-04-01

We consider the structures type of two-dimensional electron gas in the form of a thin conductive, in particular, graphene films described by tensor conductivity, which are isolated or located on the dielectric layers. The dispersion equation for hybrid modes, as well as scattering parameters. We show that free wave (eigenwaves) problem follow from the problem of diffraction when linking the amplitude of the current of the linear equations are unsolvable, i.e., the determinant of this system is zero. As a particular case the dispersion equation follow from the conditions of matching (with zero reflection coefficient).

Spectral diffraction efficiency characterization of broadband diffractive optical elements.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Choi, Junoh; Cruz-Cabrera, Alvaro Augusto; Tanbakuchi, Anthony

Diffractive optical elements, with their thin profile and unique dispersion properties, have been studied and utilized in a number of optical systems, often yielding smaller and lighter systems. Despite the interest in and study of diffractive elements, the application has been limited to narrow spectral bands. This is due to the etch depths, which are optimized for optical path differences of only a single wavelength, consequently leading to rapid decline in efficiency as the working wavelength shifts away from the design wavelength. Various broadband diffractive design methodologies have recently been developed that improve spectral diffraction efficiency and expand the workingmore » bandwidth of diffractive elements. We have developed diffraction efficiency models and utilized the models to design, fabricate, and test two such extended bandwidth diffractive designs.« less

Construction of a Cordyceps sinensis exopolysaccharide-conjugated selenium nanoparticles and enhancement of their antioxidant activities.

PubMed

Xiao, Yidong; Huang, Qilin; Zheng, Zhaomin; Guan, Han; Liu, Shiyu

2017-06-01

A Cordyceps sinensis exopolysaccharide (EPS)-conjugated selenium nanoparticles (SeNPs) were successfully constructed through the reduction of SeO 3 2- . The EPS-SeNPs were characterized in terms of formation, morphology, size, Se distribution and phase by UV-vis, FT-IR, transmission electron microscopy (TEM), dynamic light scattering (DLS), energy dispersive X-ray (EDX) and wide angle X-ray diffraction (WAXD) measurements. Results revealed that the SeNPs conjugated to EPS were amorphous and could be well dispersed at a size range of 80-125nm. The interactions between the OH groups of EPS and SeNPs substituted for intermolecular interaction in native EPS to form new CO⋯Se bonds, resulting in good dispersion of SeNPs in the EPS matrix. Besides, the EPS-SeNPs at different Se/P ratios exhibited significant scavenging ability on superoxide anion radical (O 2 - ) and ABTS radical cation (ABTS + ) when compared to pure EPS, indicating that the conjugated SeNPs reinforced antioxidant effect of EPS. This work not only provides a simple and efficient way to construct well-dispersed SeNPs in aqueous system, and demonstrates the vital role of the EPS as a biopolymer template for dispersion, stabilization and size control of SeNPs, but also finds the EPS-SeNPs can potentially serve as a good antioxidant towards O 2 - and ABTS + . Copyright © 2017 Elsevier B.V. All rights reserved.

Effects of Starting Precursor Ratio on Optoelectrical Properties and Blue Emission of Nanostructured C-ZnS Thin Films Prepared by Spin Coating

NASA Astrophysics Data System (ADS)

Rahimzadeh, N.; Ghodsi, F. E.; Mazloom, J.

2018-02-01

Nanocrystalline cubic zinc sulfide (C-ZnS) thin films have been elaborated by sol-gel spin-coating of Zn(Ac)/thiourea starting precursors at different molar ratios, and their structural, morphological, compositional, optical, electrical, and photoluminescence properties comprehensively investigated. x-ray diffraction results showed that the samples had dominant cubic structure and their crystallinity improved with increasing S content. Morphological characterization of the C-ZnS thin films was carried out by field-emission scanning electron microscopy (FESEM), revealing that the films were smooth with spherical grains included in clusters. Energy-dispersive x-ray and Fourier-transform infrared spectra of ZnS compounds did not show any evidence of impurities. Optical characterization revealed increases of the average optical transmittance and bandgap (from 3.2 eV to 3.56 eV) with increasing S content. The refractive index in the visible region increased with the S content, while the extinction coefficient decreased. The compositional dependence of the optical dispersion parameters (oscillator and dispersion energy), dielectric constant, and surface energy loss function of the films was evaluated. Electrical characterization of the films was carried out using Hall-effect measurements. The ZnS thin films exhibited n-type conductivity, and the electrical resistivity decreased with increasing carrier concentration and mobility due to enhanced crystallite size and reduced structural disorder. Photoluminescence (PL) measurements indicated a blue-shift of the near-band-edge emission. The blue emission peaks centered at about 438 nm and 487 nm were enhanced due to transitions involving interstitial S atoms, surface states, and zinc vacancies.

In vitro digestibility, crystallinity, rheological, thermal, particle size and morphological characteristics of pinole, a traditional energy food obtained from toasted ground maize.

PubMed

Carrera, Y; Utrilla-Coello, R; Bello-Pérez, A; Alvarez-Ramirez, J; Vernon-Carter, E J

2015-06-05

Flour obtained from toasted ground maize grains is widely consumed by different ethnic groups of Northern Mexico and Southwest USA as an energy source. In this work the in vitro digestibility, crystallinity, rheological, thermal, particle size distribution and morphological characteristics of toasted ground white and blue maize flours were studied. X-ray diffraction studies showed that the crystallinity content was reduced, but that the hydrolysis rate and the in vitro digestibility of starch were greatly improved by the toasting process. The relative amount of rapidly digestible starch showed an important increase at the expense of resistant starch content reduction. The thermal properties of white maize starch increased slightly, but those of the blue maize starch decreased slightly after toasting. Aqueous dispersions formed with 10% (w/w) flour were heated at 90°C for 5min to induce starch gelling, in order to resemble thin porridges. The dispersed gels exhibited higher elastic modulus (G') than loss modulus (G'') in the linear viscoelastic region, with blue maize dispersions displaying higher moduli magnitudes. At higher shear strain amplitudes, G' decreased but G'' first increased and then decreased (overshoot phenomenon). The effects of toasting on the structure and functionality of maize starch are explained on the basis of limited gelatinization of the granules. The results in this work provide insights for understanding the extensive use of pinole by impoverished ethnic groups, and more recently by high performance ultra-runners and athletes, as an energy food. Copyright © 2015 Elsevier Ltd. All rights reserved.

X-Ray Diffraction Reference Intensity Ratios of Amorphous and Poorly Crystalline Phases: Implications for CheMin on the Mars Science Laboratory

NASA Technical Reports Server (NTRS)

Morris, R. V.; Achilles, C. N.; Chipera, S. J.; Ming, D. W.; Rampe, E. B.

2013-01-01

The CheMin instrument on the Mars Science Laboratory (MSL) rover Curiosity is an X-ray diffraction (XRD) and X-ray fluorescence (XRF) instrument capable of providing the mineralogical and chemical compositions of rocks and soils on the surface of Mars. CheMin uses a microfocus X-ray tube with a Co target, transmission geometry, and an energy-discriminating X-ray sensitive CCD to produce simultaneous 2-D XRD patterns and energy-dispersive X-ray histograms from powdered samples. Piezoelectric vibration of the cell is used to randomize the sample to reduce preferred orientation effects. Instrument details are provided in [1, 2, 3]. Analyses of rock and soil samples by the Mars Exploration Rovers (MER) show nanophase ferric oxide (npOx) is a significant component of the Martian global soil [4] and is thought to be one of the major contributing phases that the Curiosity rover will encounter if a soil sample is analyzed in Gale Crater. Because of the nature of this material, npOx will likely contribute to an X-ray amorphous or short-order component of a XRD pattern measured by the CheMin instrument.

Cadmium sulphide (CdS) thin films deposited by chemical bath deposition (CBD) and dip coating techniques—a comparative study

NASA Astrophysics Data System (ADS)

Khimani, Ankurkumar J.; Chaki, Sunil H.; Malek, Tasmira J.; Tailor, Jiten P.; Chauhan, Sanjaysinh M.; Deshpande, M. P.

2018-03-01

The CdS thin films were deposited on glass slide substrates by Chemical Bath Deposition and dip coating techniques. The films thickness variation with deposition time showed maximum films deposition at 35 min for both the films. The energy dispersive analysis of x-ray showed both the films to be stoichiometric. The x-ray diffraction analysis confirmed the films possess hexagonal crystal structure. The transmission electron, scanning electron and optical microscopy study showed the films deposition to be uniform. The selected area electron diffraction exhibited ring patterns stating the films to be polycrystalline in nature. The atomic force microscopy images showed surface formed of spherical grains, hills and valleys. The recorded optical absorbance spectra analysis revealed the films possess direct optical bandgap having values of 2.25 eV for CBD and 2.40 eV for dip coating. The refractive index (η), extinction coefficient (k), complex dielectric constant (ε) and optical conductivity (σ 0) variation with wavelength showed maximum photon absorption till the respective wavelengths corresponding to the optical bandgap energy values. The recorded photoluminescence spectra showed two emission peaks. All the obtained results have been discussed in details.

Rare earth substitution on structural and optical behaviour of CdSe thin films

NASA Astrophysics Data System (ADS)

Singh, Sarika; Shrivastava, A. K.; Tapdiya, Swati

2018-05-01

A series of Sm2+,Gd2+ doped with Cadmium selenide CdSe (x =0.01) has been prepared by using Chemical bath deposition technique. Structural, Optical and Morphological studies were performed using X-ray diffraction (XRD), UV-Visible spectrometer, Raman Studies and Scanning Electron Microscopy (SEM). XRD patterns confirm the samples with Sm,Gd ions, some diffraction peaks appeared which belongs to the cubic phase structure. The values of lattice parameter (a) decreased and particle size decrease on doping. Morphology of the grown films reveals that surface are homogeneous and uniformly spread on the substrates. The elemental analysis of CdSe doped Sm and Gd (1%) different composition was analyzed by Energy Dispersive X-Rays (EDX). The optical values of some important parameters of the studied films were calculated by UVstudy are determined from transmission spectra at wavelength 200 to 900nm. Optical band gap Eg was calculated by tauc relation. Energy band gap of CdSe doped with Sm and Gd varies at 1.8eV and 1.9eV respectively. Bandgap In Raman analysis, a prominent peak shows that confirmation of nano crystalline phase. And intensity of peaks was decreasing after doping.

Structural, Morphological, Differential Scanning Calorimetric and Thermogravimetric Studies of Ball Milled Fe Doped Nanoscale La0.67Sr0.33MnO3 Manganite

NASA Astrophysics Data System (ADS)

Astik, Nidhi; Jha, Prafulla K.; Pratap, Arun

2018-03-01

The ball milling route has been used to produce the La0.67Sr0.33Mn0.85Fe0.15O3 (LSMFO) nanocrystalline sample from oxide precursors. The sample was characterized using x-ray diffraction (XRD), a scanning electron microscope (SEM), energy dispersive x-ray spectroscopy (EDAX), differential scanning calorimetry (DSC) and thermogravimetric (TGA) measurements. The x-ray diffraction confirms the phase purity of sample and shows that the sample crystallizes in the rhombohedral perovskite structure with a R-3c space group. The scanning electron micrograph shows the presence of well-faceted crystallites of LSMFO. The EDAX spectrum demonstrates the molar ratio of different elements of nanocrystalline LSMFO. Furthermore, the crystallite size using the Debye-Scherrer formula and William-Hall analysis has been found as 24 nm and 29 nm, respectively. Our results support the idea that a good quality nanocrystalline LSMFO sample can be obtained using the ball milling route. We also discuss the DSC and TGA curves and analyse the results in terms of phase transition, calcination temperature and activation barrier energies.

Toward in situ x-ray diffraction imaging at the nanometer scale

NASA Astrophysics Data System (ADS)

Zatsepin, Nadia A.; Dilanian, Ruben A.; Nikulin, Andrei Y.; Gable, Brian M.; Muddle, Barry C.; Sakata, Osami

2008-08-01

We present the results of preliminary investigations determining the sensitivity and applicability of a novel x-ray diffraction based nanoscale imaging technique, including simulations and experiments. The ultimate aim of this nascent technique is non-destructive, bulk-material characterization on the nanometer scale, involving three dimensional image reconstructions of embedded nanoparticles and in situ sample characterization. The approach is insensitive to x-ray coherence, making it applicable to synchrotron and laboratory hard x-ray sources, opening the possibility of unprecedented nanometer resolution with the latter. The technique is being developed with a focus on analyzing a technologically important light metal alloy, Al-xCu (where x is 2.0-5.0 %wt). The mono- and polycrystalline samples contain crystallographically oriented, weakly diffracting Al2Cu nanoprecipitates in a sparse, spatially random dispersion within the Al matrix. By employing a triple-axis diffractometer in the non-dispersive setup we collected two-dimensional reciprocal space maps of synchrotron x-rays diffracted from the Al2Cu nanoparticles. The intensity profiles of the diffraction peaks confirmed the sensitivity of the technique to the presence and orientation of the nanoparticles. This is a fundamental step towards in situ observation of such extremely sparse, weakly diffracting nanoprecipitates embedded in light metal alloys at early stages of their growth.

Electrical relaxation, optical and magnetic studies of nanocrystalline lithium ferrite synthesized by different chemical routes

NASA Astrophysics Data System (ADS)

Cheruku, Rajesh; Govindaraj, G.; Vijayan, Lakshmi

2017-12-01

The nanocrystalline lithium ferrite was synthesized by wet chemical methods such as solution combustion technique, sol-gel, and hydrothermal for a comparative study. Different characterization techniques like x-ray powder diffraction and thermal analysis were employed to confirm the structure and phase. Temperature-dependent Raman analysis was employed to classify the phonon modes associated with precise atomic motions existing in the synthesized materials. Morphology of sample surface was explored by scanning electron microscopy, and elemental analysis was done by energy dispersive spectroscopy analysis. The nanocrystalline nature of the materials was confirmed through transmission electron microscopy. Magnetic properties of these samples were explored through a vibrating sample magnetometer. Ac electrical impedance spectroscopy data were investigated using two Cole-Cole functions, and activation energies were calculated for all materials. Among them, solution combustion prepared lithium ferrite shows the highest conductivity and lowest activation energy.

High Pressure Strength Study on NaCl

NASA Astrophysics Data System (ADS)

Mi, Z.; Shieh, S. R.; High Pressure Mineral Physics Group

2010-12-01

Yield strength is regarded as one important property related to rheological characteristics of minerals in the Earth’s interior. The strength study of NaCl, a popular pressure medium in static high pressure experiments, has been carried out under non-hydrostatic conditions in a diamond anvil cell up to 43 GPa at room temperature using radial energy dispersive X-ray diffraction technique. Phase transformation from B1 (rock salt structure) to B2 (CsCl structure) starts at 29.4 GPa, and is complete at 32.1 GPa. Bulk modulus obtained by third order Birch-Manurgham equation of state is 25.5 GPa with pressure derivative 4.6 for B1 phase, and 30.78 GPa with pressure derivative 4.32 GPa for B2 phase, which are in a good agreement with previous studies. The differential stress of NaCl B1 phase shows very gentle increase with pressure, which indicates that NaCl is a very good pressure-transmitting medium at pressure below 30 GPa. However, the differential stress increases more abruptly for B2 phase and this may imply that NaCl can no longer be regarded as a “soft” pressure medium at very high pressures. For B1 phase, (111) is the strongest plane and (200) is the weakest plane, while (200) becomes the strongest plane in B2 phase. Pure NaCl is weaker than mixture MgO and NaCl, which indicates that soft material become stronger when mixed with hard material. The yield strength of B2 obtained through energy dispersive X-ray diffraction technique increase linearly, while the value derived by pressure gradient method shows jagged trend.

Conservation of Moroccan manuscript papers aged 150, 200 and 800 years. Analysis by infrared spectroscopy (ATR-FTIR), X-ray diffraction (XRD), and scanning electron microscopy energy dispersive spectrometry (SEM-EDS).

PubMed

Hajji, Latifa; Boukir, Abdellatif; Assouik, Jamal; Lakhiari, Hamid; Kerbal, Abdelali; Doumenq, Pierre; Mille, Gilbert; De Carvalho, Maria Luisa

2015-02-05

The preservation of manuscripts and archive materials is a serious problem for librarians and restorers. Paper manuscript is subjected to numerous degradation factors affecting their conservation state. This research represents an attempt to evaluate the conservation restoration process applied in Moroccan libraries, especially the alkaline treatment for strengthening weakened paper. In this study, we focused on six samples of degraded and restored paper taken from three different Moroccan manuscripts aged 150, 200 and 800 years. In addition, the Japanese paper used in restoration has been characterized. A modern paper was also analyzed as reference. A three-step analytical methodology based on infrared spectroscopy (ATR-FTIR), X-ray diffraction (XRD) and scanning electron microscopy coupled to energy dispersive spectrometry (SEM-EDS) analysis was developed before and after restoration in order to determine the effect of the consolidation treatment on the paper structure. The results obtained by XRD and ATR-FTIR disclosed the presence of barium sulfate (BaSO4) in all restored paper manuscripts. The presence of calcium carbonate (CaCO3) in all considered samples was confirmed by FTIR spectroscopy. The application of de-acidification treatment causes significant changes connected with the increase of intensity mostly in the region 1426 cm(-1), assigned to the asymmetric and symmetric CO stretching mode of calcite, indicating the effectiveness of de-acidification procedure proved by the rise of the alkaline reserve content allowing the long term preservation of paper. Observations performed by SEM magnify the typical paper morphology and the structure of fibbers, highlighting the effect of the restoration process, manifested by the reduction of impurities. Copyright © 2014 Elsevier B.V. All rights reserved.

Silicon supported lipid-DNA thin film structures at varying temperature studied by energy dispersive X-ray diffraction and neutron reflectivity.

PubMed

Domenici, F; Castellano, C; Dell'Unto, F; Albinati, A; Congiu, A

2011-11-01

Non-viral gene transfection by means of lipid-based nanosystems, such as solid supported lipid assemblies, is often limited due to their lack of stability and the consequent loss of efficiency. Therefore not only a detailed thermo-lyotropic study of these DNA-lipid complexes is necessary to understand their interaction mechanisms, but it can also be considered as a first step in conceiving and developing new transfection biosystems. The aim of our study is a structural characterization of 1,2-dioleoyl-sn-glycero-3-phosphatidylcholine (DOPC)-dimethyl-dioctadecyl-ammonium bromide (DDAB)-DNA complex at varying temperature using the energy dispersive X-ray diffraction (EDXD) and neutron reflectivity (NR) techniques. We have shown the formation of a novel thermo-lyotropic structure of DOPC/DDAB thin film self-organized in multi-lamellar planes on (100)-oriented silicon support by spin coating, thus enlightening its ability to include DNA strands. Our NR measurements indicate that the DOPC/DDAB/DNA complex forms temperature-dependent structures. At 65°C and relative humidity of 100% DNA fragments are buried between single lamellar leaflets constituting the hydrocarbon core of the lipid bilayers. This finding supports the consistency of the hydrophobic interaction model, which implies that the coupling between lipid tails and hypo-hydrated DNA single strands could be the driving force of DNA-lipid complexation. Upon cooling to 25°C, EDXD analysis points out that full-hydrated DOPC-DDAB-DNA can switch in a different metastable complex supposed to be driven by lipid heads-DNA electrostatic interaction. Thermotropic response analysis also clarifies that DOPC has a pivotal role in promoting the formation of our observed thermophylic silicon supported lipids-DNA assembly. Copyright © 2011 Elsevier B.V. All rights reserved.

Self catalytic growth of indium oxide (In2O3) nanowires by resistive thermal evaporation.

PubMed

Kumar, R Rakesh; Rao, K Narasimha; Rajanna, K; Phani, A R

2014-07-01

Self catalytic growth of Indium Oxide (In2O3) nanowires (NWs) have been grown by resistive thermal evaporation of Indium (In) in the presence of oxygen without use of any additional metal catalyst. Nanowires growth took place at low substrate temperature of 370-420 degrees C at an applied current of 180-200 A to the evaporation boat. Morphology, microstructures, and compositional studies of the grown nanowires were performed by employing field emission scanning electron microscopy (FESEM), X-Ray diffraction (XRD), transmission electron microscopy (TEM), energy dispersive X-ray spectroscopy (EDS) and X-ray photoelectron spectroscopy (XPS) respectively. Nanowires were uniformly grown over the entire Si substrate and each of the nanowire is capped with a catalyst particle at their end. X-ray diffraction study reveals the crystalline nature of the grown nanowires. Transmission electron microscopy study on the nanowires further confirmed the single crystalline nature of the nanowires. Energy dispersive X-ray analysis on the nanowires and capped nanoparticle confirmed that Indium act as catalyst for In2O3 nanowires growth. A self catalytic Vapor-Liquid-Solid (VLS) growth mechanism was responsible for the growth of In2O3 nanowires. Effect of oxygen partial pressure variation and variation of applied currents to the evaporation boat on the nanowires growth was systematically studied. These studies concluded that at oxygen partial pressure in the range of 4 x 10(-4), 6 x 10(-4) mbar at applied currents to the evaporation boat of 180-200 A were the best conditions for good nanowires growth. Finally, we observed another mode of VLS growth along with the standard VLS growth mode for In2O3 nanowires similar to the growth mechanism reported for GaAs nanowires.

Structural and mechanical properties of hydroxyapatite coatings formed by ion-beam assisted deposition

NASA Astrophysics Data System (ADS)

Zykova, A.; Safonov, V.; Dudin, S.; Yakovin, S.; Donkov, N.; Ghaemi, M. H.; Szkodo, M.; Antoszkiewicz, M.; Szyfelbain, M.; Czaban, A.

2018-03-01

The ion-beam assisted deposition (IBAD) is an advanced method capable of producing crystalline coatings at low temperatures. We determined the characteristics of hydroxyapatite Ca10(PO4)6(OH)2 target and coatings formed by IBAD using X-ray photoemission spectroscopy (XPS), X-ray diffraction (XRD), scanning electron microscopy (SEM), atomic force microscopy (AFM) and energy dispersive X-ray (EDX). The composition of the coatings’ cross-section and surface was close to those of the target. The XPS spectra showed that the binding energy values of Ca (2p1/2, 2p3/2), P (2p3/2), and O 1s levels are related to the hydroxyapatite phase. The coatings demonstrate an optimal H/E ratio, and a good resistance to scratch tests.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ovcharov, A. V.; Karateev, I. A.; Mikhutkin, A. A.

The surface microstructure of Ni–W alloy tapes, which are used as substrates to form films of high-temperature superconductors and photovoltaic devices, has been studied. Several samples of a Ni{sub 95}W{sub 5} tape (Evico) annealed under different conditions were analyzed using scanning electron microscopy, energy-dispersive X-ray microanalysis, electron diffraction, and electron energy-loss spectroscopy. NiWO{sub 4} precipitates are found on the surface of annealed samples. The growth of precipitates at a temperature of 950°C is accompanied by the formation of pores on the surface or under an oxide film. Depressions with a wedge-shaped profile are found at the grain boundaries. Annealing inmore » a reducing atmosphere using a specially prepared chamber allows one to form a surface free of nickel tungstate precipitates.« less

Flake like V{sub 2}O{sub 5} nanoparticles for ethanol sensing at room temperature

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chitra, M.; Uthayarani, K.; Rajasekaran, N.

2016-05-23

The versatile redox property of vanadium oxide explores it in various applications like catalysis, electrochromism, electrochemistry, energy storage, sensors, microelectronics, batteries etc., In this present work, vanadium oxide was prepared via hydrothermal route followed by calcination. The structural and lattice parameters were analysed from the powder X-ray diffraction (XRD) pattern. The morphology and the composition of the sample were obtained from Field emission Scanning electron microscopic (FeSEM) and Energy Dispersive X-ray (EDAX) Spectrometric analysis respectively. The sensitivity, response – recovery time of the sample towards ethanol (0 ppm – 300 ppm) sensing at room temperature was measured and the present investigation onmore » vanadium oxide nanoparticles over the flakes shows better sensitivity (30%) at room temperature.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mazuritskiy, M. I., E-mail: mazurmik@gmail.com; Lerer, A. M.; Makhno, P. V.

The angular distribution of the X-ray intensity at the exit of microchannel plates at grazing incidence of monochromatic radiation on the walls of microcapillaries has been investigated. The angles and energies of the primary radiation quanta at which the synchrotron beam excites X-ray fluorescence propagating inside polycapillary structures have been determined. The angular dependences of the intensity distribution of X-rays transmitted through the microcapillaries have been studied theoretically and experimentally for energies corresponding to the region of anomalous dispersion near the L{sub 2,3} absorption edges of silicon. The propagation of waves in hollow polycapillary waveguides, the excitation of X-ray fluorescence,more » and the X-ray diffraction at the exit of microchannel plates have been modeled mathematically. The mathematical model takes into account the presence of a transition layer on the microchannel surface.« less

Optical and structural properties of CsI thin film photocathode

NASA Astrophysics Data System (ADS)

Triloki; Rai, R.; Singh, B. K.

2015-06-01

In the present work, the performance of a cesium iodide thin film photocathode is studied in detail. The optical absorbance of cesium iodide films has been analyzed in the spectral range from 190 nm to 900 nm. The optical band gap energy of 500 nm thick cesium iodide film is calculated from the absorbance data using a Tauc plot. The refractive index is estimated from the envelope plot of transmittance data using Swanepoel's method. The absolute quantum efficiency measurement has been carried out in the wavelength range from 150 nm to 200 nm. The crystallographic nature and surface morphology are investigated by X-ray diffraction and transmission electron microscopy techniques. In addition, the elemental composition result obtained by energy dispersive X-ray analysis is also reported in the present work.

Quantum X waves with orbital angular momentum in nonlinear dispersive media

NASA Astrophysics Data System (ADS)

Ornigotti, Marco; Conti, Claudio; Szameit, Alexander

2018-06-01

We present a complete and consistent quantum theory of generalised X waves with orbital angular momentum in dispersive media. We show that the resulting quantised light pulses are affected by neither dispersion nor diffraction and are therefore resilient against external perturbations. The nonlinear interaction of quantised X waves in quadratic and Kerr nonlinear media is also presented and studied in detail.

Molecularly designed lipid microdomains for solid dispersions using a polymer/inorganic carrier matrix produced by hot-melt extrusion.

PubMed

Adler, Camille; Schönenberger, Monica; Teleki, Alexandra; Kuentz, Martin

2016-02-29

Amorphous solid dispersions have for many years been a focus in oral formulations, especially in combination with a hot-melt extrusion process. The present work targets a novel approach with a system based on a fatty acid, a polymer and an inorganic carrier. It was intended to adsorb the acidic lipid by specific molecular interactions onto the solid carrier to design disorder in the alkyl chains of the lipid. Such designed lipid microdomains (DLM) were created as a new microstructure to accommodate a compound in a solid dispersion. Vibrational spectroscopy, X-ray powder diffraction, atomic force microscopy as well as electron microscopic imaging were employed to study a system of stearic acid, hydroxypropylcellulose and aluminum magnesium silicate. β-carotene was used as a poorly water-soluble model substance that is difficult to formulate with conventional solid dispersion formulations. The results indicated that the targeted molecular excipient interactions indeed led to DLMs for specific compositions. The different methods provided complementary aspects and important insights into the created microstructure. The novel delivery system appeared to be especially promising for the formulation of oral compounds that exhibit both high crystal energy and lipophilicity. Copyright © 2015 Elsevier B.V. All rights reserved.

High Pressure X-Ray Diffraction Studies of Nanocrystalline Materials

NASA Technical Reports Server (NTRS)

Palosz, B.; Stel'makh, S.; Grzanka, E.; Gierlotka, S.; Palosz, W.

2004-01-01

Experimental evidence obtained for a variety of nanocrystalline materials suggest that the crystallographic structure of a very small size particle deviates from that in the bulk crystals. In this paper we show the effect of the surface of nanocrystals on their structure by the analysis of generation and distribution of macro- and micro-strains at high pressures and their dependence on the grain size in nanocrystalline powders of Sic. We studied the structure of Sic nanocrystals by in-situ high-pressure powder diffraction technique using synchrotron and neutron sources and hydrostatic or isostatic pressure conditions. The diffraction measurements were done in HASYLAB at DESY using a Diamond Anvil Cell (DAC) in the energy dispersive geometry in the diffraction vector range up to 3.5 - 4/A and under pressures up to 50 GPa at room temperature. In-situ high pressure neutron diffraction measurements were done at LANSCE in Los Alamos National Laboratory using the HIPD and HIPPO diffractometers with the Paris-Edinburgh and TAP-98 cells, respectively, in the diffraction vector range up to 26 Examination of the response of the material to external stresses requires nonstandard methodology of the materials characterization and description. Although every diffraction pattern contains a complete information on macro- and micro-strains, a high pressure experiment can reveal only those factors which contribute to the characteristic diffraction patterns of the crystalline phases present in the sample. The elastic properties of powders with the grain size from several nm to micrometers were examined using three methodologies: (l), the analysis of positions and widths of individual Bragg reflections (used for calculating macro- and micro-strains generated during densification) [I], (2). the analysis of the dependence of the experimental apparent lattice parameter, alp, on the diffraction vector Q [2], and (3), the atomic Pair Distribution Function (PDF) technique [3]. The results of our studies show, that Sic nanocrystals have the features of two phases, each with its distinct elastic properties. and under pressures up to 8 GPa.

Local structure of ion pair interaction in lapatinib amorphous dispersions characterized by synchrotron x-ray diffraction and pair distribution function analysis

DOE PAGES

de Araujo, Gabriel L. B.; Benmore, Chris J.; Byrn, Stephen R.

2017-04-11

For many years, the idea of analyzing atom-atom contacts in amorphous drug-polymer systems has been of major interest, because this method has always had the potential to differentiate between amorphous systems with domains and amorphous systems which are molecular mixtures. In this study, local structure of ionic and noninonic interactions were studied by High-Energy X-ray Diffraction and Pair Distribution Function (PDF) analysis in amorphous solid dispersions of lapatinib in hypromellose phthalate (HPMCP) and hypromellose (HPMC-E3). The strategy of extracting lapatinib intermolecular drug interactions from the total PDF x-ray pattern was successfully applied allowing the detection of distinct nearest neighbor contactsmore » for the HPMC-E3 rich preparations showing that lapatinib molecules do not cluster in the same way as observed in HPMC-P, where ionic interactions are present. Orientational correlations up to nearest neighbor molecules at about 4.3 Å were observed for polymer rich samples; both observations showed strong correlation to the stability of the systems. Lasty, the superior physical stability of 1:3 LP:HPMCP was consistent with the absence of significant intermolecular interactions in (ΔD inter LP(r)) in the range of 3.0 to 6.0 Å, which are attributed to C-C, C-N and C-O nearest neighbor contacts present in drug-drug interactions.« less

Local structure of ion pair interaction in lapatinib amorphous dispersions characterized by synchrotron x-ray diffraction and pair distribution function analysis

DOE Office of Scientific and Technical Information (OSTI.GOV)

de Araujo, Gabriel L. B.; Benmore, Chris J.; Byrn, Stephen R.

For many years, the idea of analyzing atom-atom contacts in amorphous drug-polymer systems has been of major interest, because this method has always had the potential to differentiate between amorphous systems with domains and amorphous systems which are molecular mixtures. In this study, local structure of ionic and noninonic interactions were studied by High-Energy X-ray Diffraction and Pair Distribution Function (PDF) analysis in amorphous solid dispersions of lapatinib in hypromellose phthalate (HPMCP) and hypromellose (HPMC-E3). The strategy of extracting lapatinib intermolecular drug interactions from the total PDF x-ray pattern was successfully applied allowing the detection of distinct nearest neighbor contactsmore » for the HPMC-E3 rich preparations showing that lapatinib molecules do not cluster in the same way as observed in HPMC-P, where ionic interactions are present. Orientational correlations up to nearest neighbor molecules at about 4.3 Å were observed for polymer rich samples; both observations showed strong correlation to the stability of the systems. Lasty, the superior physical stability of 1:3 LP:HPMCP was consistent with the absence of significant intermolecular interactions in (ΔD inter LP(r)) in the range of 3.0 to 6.0 Å, which are attributed to C-C, C-N and C-O nearest neighbor contacts present in drug-drug interactions.« less

Local Structure of Ion Pair Interaction in Lapatinib Amorphous Dispersions characterized by Synchrotron X-Ray diffraction and Pair Distribution Function Analysis

NASA Astrophysics Data System (ADS)

de Araujo, Gabriel L. B.; Benmore, Chris J.; Byrn, Stephen R.

2017-04-01

For many years, the idea of analyzing atom-atom contacts in amorphous drug-polymer systems has been of major interest, because this method has always had the potential to differentiate between amorphous systems with domains and amorphous systems which are molecular mixtures. In this study, local structure of ionic and noninonic interactions were studied by High-Energy X-ray Diffraction and Pair Distribution Function (PDF) analysis in amorphous solid dispersions of lapatinib in hypromellose phthalate (HPMCP) and hypromellose (HPMC-E3). The strategy of extracting lapatinib intermolecular drug interactions from the total PDF x-ray pattern was successfully applied allowing the detection of distinct nearest neighbor contacts for the HPMC-E3 rich preparations showing that lapatinib molecules do not cluster in the same way as observed in HPMC-P, where ionic interactions are present. Orientational correlations up to nearest neighbor molecules at about 4.3 Å were observed for polymer rich samples; both observations showed strong correlation to the stability of the systems. Finally, the superior physical stability of 1:3 LP:HPMCP was consistent with the absence of significant intermolecular interactions in (Δ) in the range of 3.0 to 6.0 Å, which are attributed to C-C, C-N and C-O nearest neighbor contacts present in drug-drug interactions.

Synthesis of novel CeO2-BiVO4/FAC composites with enhanced visible-light photocatalytic properties.

PubMed

Zhang, Jin; Wang, Bing; Li, Chuang; Cui, Hao; Zhai, Jianping; Li, Qin

2014-09-01

To utilize visible light more effectively in photocatalytic reactions, a fly ash cenosphere (FAC)-supported CeO2-BiVO4 (CeO2-BiVO4/FAC) composite photocatalyst was prepared by modified metalorganic decomposition and impregnation methods. The physical and photophysical properties of the composite have been characterized by X-ray diffraction (XRD), scanning electron microscope (SEM) and energy dispersive X-ray spectroscopy (EDX), X-ray photoelectron spectroscopy (XPS), and UV-Visible diffuse reflectance spectra. The XRD patterns exhibited characteristic diffraction peaks of both BiVO4 and CeO2 crystalline phases. The XPS results showed that Ce was present as both Ce(4+) and Ce(3+) oxidation states in CeO2 and dispersed on the surface of BiVO4 to constitute a p-n heterojunction composite. The absorption threshold of the CeO2-BiVO4/FAC composite shifted to a longer wavelength in the UV-Vis absorption spectrum compared to the pure CeO2 and pure BiVO4. The composites exhibited enhanced photocatalytic activity for Methylene Blue (MB) degradation under visible light irradiation. It was found that the 7.5wt.% CeO2-BiVO4/FAC composite showed the highest photocatalytic activity for MB dye wastewater treatment. Copyright © 2014. Published by Elsevier B.V.

Effect of Cu2+ substitution on the structural, optical and magnetic behaviour ofchemically derived manganese ferrite nanoparticles

NASA Astrophysics Data System (ADS)

Vasuki, G.; Balu, T.

2018-06-01

Mixed spinel copper manganese ferrite (CuXMn1‑XFe2O4, X = 0, 0.25, 0.5, 0.75, 1) nanoparticles were synthesized by chemical co-precipitation technique. From the powder x-ray diffraction analysis the lattice constant, volume of unit cell, x-ray density, hopping lengths, crystallite size, surface area, dislocation density and microstrain were calculated. The substitution of Cu2+ ions shows a considerable reduction in the crystallite size of manganese ferrite from 34 nm to 22 nm. Further a linear fit of Williamson-Hall plot has been drawn to determine the microstrain and crystallite size. The crystallite size and morphology were further observed through high resolution transmission electron microscope and scanning electron microscope. The diffraction rings observed from selected area electron diffraction pattern exhibits the crystalline nature of all the samples. The energy dispersive x-ray analysis shows the composition of all the elements incorporated in the synthesized nanomaterials. FTIR studies reveal the absorption peaks that correspond to the metal-oxygen vibrations in the tetrahedral and octahedral sites. From the UV–vis absorption spectra the band gap energy, refractive index and optical dielectric constant were determined. Magnetic studies carried out using vibrating sample magnetometer shows interesting behaviour in the variation of magnetisation and coercivity. Peculiar magnetic behaviour is observed when Cu2+ ions are substituted in manganese ferrites. All the synthesized materials have very low value of squareness ratio which attributes to the superparamagnetic behaviour.

Portable X-ray diffractometer equipped with XRF for archaeometry

NASA Astrophysics Data System (ADS)

Uda, M.; Ishizaki, A.; Satoh, R.; Okada, K.; Nakajima, Y.; Yamashita, D.; Ohashi, K.; Sakuraba, Y.; Shimono, A.; Kojima, D.

2005-09-01

A portable X-ray diffractometer equipped with an X-ray fluorescence spectrometer was improved so as to get a diffraction pattern and a fluorescence spectrum simultaneously in air from one and the same small area on a specimen. Here, diffraction experiments were performed in two modes, i.e. an angle rotation mode and an energy dispersive mode. In the latter a diffraction pattern and a fluorescence spectrum were simultaneously recorded in a short time, 100 s or less, on one display. The diffractometer was tested in the field to confirm its performance. Targets chosen for this purpose were a bronze mirror from the Eastern Han Dynasty (25-220), and a stupa and its pedestal which are part of the painted statue of "Tamonten holding a stupa" from the Heian Period (794-1192), enshrined in the Engyouji temple founded in 996. The bronze mirror was identified as a product of the Han Dynasty from its chemical composition and the existence of the δ phase in the Cu-Sn alloy. The stupa and its pedestal were decorated with gold powder and gold leaf, respectively. From the XRF data of the pedestal, the underlying layer of gold leaf seems to have been painted with emerald green.

Resonance surface plasmon spectroscopy by tunable enhanced light transmission through nanostructured gratings and thin films

NASA Astrophysics Data System (ADS)

Yeh, Wei-Hsun

Surface plasmon resonance (SPR) is a powerful tool in probing interfacial events in that any changes of effective refractive index in the interface directly impact the behavior of surface plasmons, an electromagnetic wave, travelling along the interface. Surface plasmons (SPs) are generated only if the momemtum of incident light matches that of SPs in the interface. This thesis focuses on tuning the behavior of SPs by changing the topology of diffraction gratings, monitoring the thickness of thin films by diffraction gratings, and use of dispersion images to analyze complex optical responses of SPs through diffraction gratings. Chapter 1 covers the background/principle of SPR, comprehensive literature review, sensor applications, control of SPR spectral responses, and sensitivity of SPR. In Chapter 2, we illustrate a chirped grating with varying surface topology along its spatial position. We demonstrated that the features of nanostructure such as pitch and amplitude significantly impact the behavior of enhanced transmission. In addition, we also illustrate the sensing application of chirped grating and the results indicate that the chirped grating is a sensitive and information rich SPR platform. In chapter 3, we used a commercial DVD diffraction grating as a SPR coupler. A camera-mounted microscope with Bertrend lens attachment is used to observe the enhanced transmission. We demonstrate that this system can monitor the SPR responses and track the thickness of a silicon monoxide film without using a spectrophotometer. Surface plasmons are a result of collective oscillation of free electrons in the metal/dielectric interface. Thus, the interaction of SPs with delocalized electrons from molecular resonance is complex. In chapter 4, we perform both experimental and simulation works to address this complex interaction. Detailed examination and analysis show nontypical SPR responses. For p-polarized light, a branch of dispersion curve and quenching of SPs in the Q band of zinc phthalocyanine are observed. For both p- and s-polarized light, additional waveguided modes are observed and the wavelength from different guided modes are dispersed. Diffraction gratings can provide complicated optical information about SPs. Both front side (air/metal) and back side (metal/substrate) provide SPR signals simultaneously. In chapter 5, we use dispersion images to analyze the complicated optical responses of SPR from an asymmetrical diffraction grating consisting of three layers (air/gold/polycarbonate). We illustrate that clear identification of SPR responses from several diffraction orders at front side and back side can be achieved by the use of dispersion images. Theoretical prediction and experimental results show consistency. We also show that only the behavior of SPs from the front side is impacted by the deposition of Langmuir-Blodgett dielectric films. In chapter 6, we construct a diffraction grating that has a fixed pitch and several amplitudes on its surface by using interference lithography. The purpose of this work is to examine how the amplitude impacts the behavior of transmission peaks. Different amplitudes are successfully fabricated by varying development time in the lithography process. We observed that largest (optimized) enhanced transmission peak shows as the amplitude approach a critical value. Transmission is not maximized below or beyond a critical amplitude. We also found that transmission enhancements are strongly affected by the diffraction efficiencies. A maximum enhancement is observed as diffraction efficiency is largest where amplitude reaches the critical value. The experimental results are then compared to the simulation. (Abstract shortened by UMI.)

Applied optics. Multiwavelength achromatic metasurfaces by dispersive phase compensation.

PubMed

Aieta, Francesco; Kats, Mikhail A; Genevet, Patrice; Capasso, Federico

2015-03-20

The replacement of bulk refractive optical elements with diffractive planar components enables the miniaturization of optical systems. However, diffractive optics suffers from large chromatic aberrations due to the dispersion of the phase accumulated by light during propagation. We show that this limitation can be overcome with an engineered wavelength-dependent phase shift imparted by a metasurface, and we demonstrate a design that deflects three wavelengths by the same angle. A planar lens without chromatic aberrations at three wavelengths is also presented. Our designs are based on low-loss dielectric resonators, which introduce a dense spectrum of optical modes to enable dispersive phase compensation. The suppression of chromatic aberrations in metasurface-based planar photonics will find applications in lightweight collimators for displays, as well as chromatically corrected imaging systems. Copyright © 2015, American Association for the Advancement of Science.

Physicochemical characterization and aerosol dispersion performance of organic solution advanced spray-dried cyclosporine A multifunctional particles for dry powder inhalation aerosol delivery

PubMed Central

Wu, Xiao; Zhang, Weifen; Hayes, Don; Mansour, Heidi M

2013-01-01

In this systematic and comprehensive study, inhalation powders of the polypeptide immunosuppressant drug – cyclosporine A – for lung delivery as dry powder inhalers (DPIs) were successfully designed, developed, and optimized. Several spray drying pump rates were rationally chosen. Comprehensive physicochemical characterization and imaging was carried out using scanning electron microscopy, hot-stage microscopy, differential scanning calorimetry, powder X-ray diffraction, Karl Fischer titration, laser size diffraction, and gravimetric vapor sorption. Aerosol dispersion performance was conducted using a next generation impactor with a Food and Drug Administration-approved DPI device. These DPIs displayed excellent aerosol dispersion performance with high values in emitted dose, respirable fraction, and fine particle fraction. In addition, novel multifunctional inhalation aerosol powder formulations of cyclosporine A with lung surfactant-mimic phospholipids were also successfully designed and developed by advanced organic solution cospray drying in closed mode. The lung surfactantmimic phospholipids were 1,2-dipalmitoyl-sn-glycero-3-phosphocholine and 1,2-dipalmitoyl-snglycero- 3-(phosphor-rac-1-glycerol). These cyclosporine A lung surfactant-mimic aerosol powder formulations were comprehensively characterized. Powder X-ray diffraction and differential scanning calorimetry confirmed that the phospholipid bilayer structure in the solid state was preserved following advanced organic solution spray drying in closed mode. These novel multifunctional inhalation powders were optimized for DPI delivery with excellent aerosol dispersion performance and high aerosol performance parameters. PMID:23569375

Structural, morphological and optical properties of ZnSe quantum dot thin films.

PubMed

Zedan, I T; Azab, A A; El-Menyawy, E M

2016-02-05

ZnSe powder was prepared via hydrothermal technique using zinc acetate and sodium selenite as source materials. The prepared ZnSe powder was used for preparing film with different thickness values (95, 135 and 230 nm) via thermal evaporation technique. X-ray diffraction showed that the prepared powder has cubic zinc-blende structure with a space group, F43m. The high resolution transmittance electron microscope results show that the films are composed of spherical-shaped nanoparticles with a diameter in the range of 2-8 nm. The optical properties of ZnSe films with differing thicknesses are investigated by means of spectrophotometric measurements of the photoluminescence, transmittance and reflectance. The absorption coefficient of the films is calculated and the optical band gap is estimated. The refractive index of the films is determined and its normal dispersion behavior is analyzed on the basis of a single oscillator model, in which oscillator energy, dispersion energy and dielectric constant at high frequency are evaluated. Drude model is also applied to determine the lattice dielectric constant and the ratio of the carriers' concentration to their effective mass. Copyright © 2015 Elsevier B.V. All rights reserved.

Synthesis and characterization of molybdenum catalysts supported on {gamma}-Al{sub 2}O{sub 3}-CeO{sub 2} composite oxides

DOE Office of Scientific and Technical Information (OSTI.GOV)

Farooq, Muhammad; Ramli, Anita; Subbarao, Duvvuri

2012-09-26

The physical and chemical properties of a catalyst play a vital role in various industrial applications. Molybdenum catalysts supported on {gamma}-Al{sub 2}O{sub 3} and {gamma}-Al{sub 2}O{sub 3}-CeO{sub 2} mixed oxides with varying loading of CeO{sub 2} (5, 10, 15, 20 wt% with respect to {gamma}-Al{sub 2}O{sub 3}) were prepared by wet impregnation method. The physiochemical properties of these synthesized Mo catalysts were studied with various characterization techniques such as X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), temperature-programmed reduction (TPR), field emission scanning electron microscopy-energy dispersive analysis (FESEM-EDX) and X-ray fluorescence spectrometer (XRF). The results showed that the addition of CeO{submore » 2} into the support affected the binding energies of the elements and reducibility of the metal oxides formed after calcination of catalyst samples due to the change in metal-support interaction. Further, the characterization techniques showed that the active metal was well dispersed on the surface of support material.« less

Functionalized MIL-101 with imidazolium-based ionic liquids for the cycloaddition of CO2 and epoxides under mild condition

NASA Astrophysics Data System (ADS)

Liu, Dan; Li, Gang; Liu, Haiou

2018-01-01

A kind of multi-functional sites metal-organic framework (MOF) composite (MIL-101-IMBr) was successfully prepared by post-synthesis modification of MIL-101 with imidazolium-based ionic liquids. The ionic liquids not only functionalize as basic sites but also provide halide anions, which serve as a nucleophile in cycloaddition reaction. The prepared functional MOF materials were characterized by X-ray diffraction, fourier transform infrared spectroscopy, scanning electron microscopy, energy dispersive spectroscopy, N2 adsorption-desorption and CO2 temperature programmed desorption. The results of fourier transform infrared spectroscopy and energy dispersive spectroscopy show that the MIL-101-IMBr composite was successfully synthesized. The N2 adsorption-desorption results clearly demonstrated that the modified composites still preserve high BET surface area and total pore volume. The composite exhibits high catalytic activity for the cycloaddition of CO2 with epoxides under mild and co-catalyst free conditions. The conversion of propylene oxide was 95.8% and the selectivity of cyclic carbonate was 97.6% under 0.8 MPa at 80 °C for 4 h. Moreover, the catalyst can be used for at least five times.

A standards-based method for compositional analysis by energy dispersive X-ray spectrometry using multivariate statistical analysis: application to multicomponent alloys.

PubMed

Rathi, Monika; Ahrenkiel, S P; Carapella, J J; Wanlass, M W

2013-02-01

Given an unknown multicomponent alloy, and a set of standard compounds or alloys of known composition, can one improve upon popular standards-based methods for energy dispersive X-ray (EDX) spectrometry to quantify the elemental composition of the unknown specimen? A method is presented here for determining elemental composition of alloys using transmission electron microscopy-based EDX with appropriate standards. The method begins with a discrete set of related reference standards of known composition, applies multivariate statistical analysis to those spectra, and evaluates the compositions with a linear matrix algebra method to relate the spectra to elemental composition. By using associated standards, only limited assumptions about the physical origins of the EDX spectra are needed. Spectral absorption corrections can be performed by providing an estimate of the foil thickness of one or more reference standards. The technique was applied to III-V multicomponent alloy thin films: composition and foil thickness were determined for various III-V alloys. The results were then validated by comparing with X-ray diffraction and photoluminescence analysis, demonstrating accuracy of approximately 1% in atomic fraction.

Additive assisted hydrothermal synthesis, characterization and optical properties of one dimensional DyPO4:Ce3+ nanostructures

NASA Astrophysics Data System (ADS)

Khajuria, H.; Kumar, M.; Singh, R.; Ladol, J.; Nawaz Sheikh, H.

2018-05-01

One dimensional nanostructures of cerium doped dysprosium phosphate (DyPO4:Ce3+) were synthesized via hydrothermal route in the presence of different surfactants [sodium dodecyl sulfate (SDS), dodecyl sulfosuccinate (DSS), polyvinyl pyrollidone (PVP)] and solvent [ethylene glycol and water]. The prepared nanostructures were characterized by Powder X-ray diffraction (PXRD), Fourier transform infrared spectroscopy (FTIR), Field emission scanning electron microscopy (FE-SEM), Transmission electron microscopy (TEM), energy dispersive spectroscopy (EDS), UV-VIS-NIR absorption spectrophotometer and photoluminescence (PL) studies. The PXRD and FTIR results indicate purity, good crystallinity and effective doping of Ce3+ in nanostructures. SEM and TEM micrographs display nanorods, nanowires and nanobundles like morphology of DyPO4:Ce3+. Energy-dispersive X-ray spectra (EDS) of DyPO4:Ce3+nanostructures confirm the presence of dopant. UV-VIS-NIR absorption spectra of prepared compounds are used to calculate band gap and explore their optical properties. Luminescent properties of DyPO4:Ce3+ was studied by using PL emission spectra. The effect of additives and solvents on the uniformity, morphology and optical properties of the nanostructures were studied in detail.

Momentum microscopy of ? single crystals with detailed surface characterisation

NASA Astrophysics Data System (ADS)

Ellguth, M.; Tusche, C.; Iga, F.; Suga, S.

2016-11-01

We report the in situ preparation of surfaces of the proposed topological Kondo insulator SmB? by controlled cycles of Ar ion sputtering and annealing. The procedure provides a reproducible way for the preparation of Sm- or B-rich surface terminations by low (?1080 ?C) or high (?1200 ?C) temperature annealing. The surface quality and termination were checked by low energy electron diffraction and Auger electron spectroscopy. Photoemission studies were carried out using momentum microscopy and two laboratory light sources providing polarised radiation with an energy of 6 eV (fourth harmonic of a pulsed Ti:Sapphire laser) and unpolarised radiation with an energy of 21.2 eV (He-I line of a gas discharge lamp). Full dispersions of electronic states in a wide two-dimensional momentum space were obtained by momentum microscopy from the in situ prepared Sm-terminated surface. The shape of the Fermi surface is discussed based on the sections through the bulk Brillouin zone sampled by the different photon energies.

Analytical characterization of a new mobile X-ray fluorescence and X-ray diffraction instrument combined with a pigment identification case study

NASA Astrophysics Data System (ADS)

Van de Voorde, Lien; Vekemans, Bart; Verhaeven, Eddy; Tack, Pieter; De Wolf, Robin; Garrevoet, Jan; Vandenabeele, Peter; Vincze, Laszlo

2015-08-01

A new, commercially available, mobile system combining X-ray diffraction and X-ray fluorescence has been evaluated which enables both elemental analysis and phase identification simultaneously. The instrument makes use of a copper or molybdenum based miniature X-ray tube and a silicon-Pin diode energy-dispersive detector to count the photons originating from the samples. The X-ray tube and detector are both mounted on an X-ray diffraction protractor in a Bragg-Brentano θ:θ geometry. The mobile instrument is one of the lightest and most compact instruments of its kind (3.5 kg) and it is thus very useful for in situ purposes such as the direct (non-destructive) analysis of cultural heritage objects which need to be analyzed on site without any displacement. The supplied software allows both the operation of the instrument for data collection and in-depth data analysis using the International Centre for Diffraction Data database. This paper focuses on the characterization of the instrument, combined with a case study on pigment identification and an illustrative example for the analysis of lead alloyed printing letters. The results show that this commercially available light-weight instrument is able to identify the main crystalline phases non-destructively, present in a variety of samples, with a high degree of flexibility regarding sample size and position.

Analysis of a nanocrystalline polymer dispersion of ebselen using solid-state NMR, Raman microscopy, and powder X-ray diffraction.

PubMed

Vogt, Frederick G; Williams, Glenn R

2012-07-01

Nanocrystalline drug-polymer dispersions are of significant interest in pharmaceutical delivery. The purpose of this work is to demonstrate the applicability of methods based on two-dimensional (2D) and multinuclear solid-state NMR (SSNMR) to a novel nanocrystalline pharmaceutical dispersion of ebselen with polyvinylpyrrolidone-vinyl acetate (PVP-VA), after initial characterization with other techniques. A nanocrystalline dispersion of ebselen with PVP-VA was prepared and characterized by powder X-ray diffraction (PXRD), confocal Raman microscopy and mapping, and differential scanning calorimetry (DSC), and then subjected to detailed 1D and 2D SSNMR analysis involving ¹H, ¹³C, and ⁷⁷Se isotopes and ¹H spin diffusion. PXRD was used to show that dispersion contains nanocrystalline ebselen in the 35-60 nm size range. Confocal Raman microscopy and spectral mapping were able to detect regions where short-range interactions may occur between ebselen and PVP-VA. Spin diffusion effects were analyzed using 2D SSNMR experiments and are able to directly detect interactions between ebselen and the surrounding PVP-VA. The methods used here, particularly the 2D SSNMR methods based on spin diffusion, provided detailed structural information about a nanocrystalline polymer dispersion of ebselen, and should be useful in other studies of these types of materials.

Monolayer dispersion of CoO on Al2O3 probed by positronium atom

NASA Astrophysics Data System (ADS)

Liu, Z. W.; Zhang, H. J.; Chen, Z. Q.

2014-02-01

CoO/Al2O3 catalysts were prepared by wet impregnation method with CoO contents ranging from 0 wt% to 24 wt%. X-ray diffraction and X-ray photoelectron spectroscopy measurements suggest formation of CoO after calcined in N2. Quantitative X-ray diffraction analysis indicates monolayer dispersion capacity of CoO in CoO/Al2O3 catalysts to be about 3 wt%. Positron annihilation lifetime and coincidence Doppler broadening measurements were performed to study the dispersion state of CoO on Al2O3. The positron lifetime measurements reveal two long lifetime components τ3 and τ4, which correspond to ortho-positronium annihilation lifetime in microvoids and large pores, respectively. It was found that the positronium atom is very sensitive to the dispersion state of CoO on Al2O3. The presence of CoO significantly decreases both the lifetime and the intensity of τ4. Detailed analysis of the coincidence Doppler broadening measurements suggests that with the CoO content lower than the monolayer dispersion, spin conversion reaction of positronium is induced by CoO. When the cobalt content is higher than the monolayer dispersion capacity, inhibition of positronium formation becomes the dominate effect.

Solid dispersions of Myricetin with enhanced solubility: Formulation, characterization and crystal structure of stability-impeding Myricetin monohydrate crystals

NASA Astrophysics Data System (ADS)

Mureşan-Pop, M.; Pop, M. M.; Borodi, G.; Todea, M.; Nagy-Simon, T.; Simon, S.

2017-08-01

Three solid dispersion forms of Myricetin combined with the Polyvinylpyrrolidone were successfully prepared by spray drying method, and characterized by X-ray powder diffraction, thermal analysis, infrared spectroscopy and optical microscopy. Zeta potential measurements provided indications on solid dispersions stability in aqueous suspension related to their storage at elevated temperature and relative humidity, which depends on the Myricetin load. By increase of Myricetin load, the stability of the solid dispersion is impeded due to growth of Myricetin monohydrate crystals. The amorphous dispersions with 10% and 50% Myricetin load are stable and, compared to pure Myricetin, their aqueous solubility is enhanced by a factor of 47 and 13, respectively. The dispersion with 80% Myricetin load is unstable on storage, and this behavior acts in conjunction with the development of Myricetin monohydrate crystals. Single-crystal X-ray diffraction results obtained for Myricetin monohydrate reveal a structure of an infinite 2D network of hydrogen-bonded molecules involving all six hydroxyl groups of Myricetin. The water molecules are positioned in between the infinite chains, and contribute via H-bonds to robust crystal packing. The calculated needle-like morphology of monohydrate form is in agreement with the optical microscopy results. The study shows that the solid amorphous dispersions with up to 50% Myricetin load are a viable option for achieving substantial solubility improvement of Myricetin, and supports their potential use in pharmaceutical applications.

Investigation on structural, optical and electrical properties of polythiophene-Al2O3 composites

NASA Astrophysics Data System (ADS)

Vijeth, H.; Yesappa, L.; Niranjana, M.; Ashokkumar, S. P.; Devendrappa, H.

2018-05-01

The polythiophene (PTH) and polythiophene-Al2O3 composites prepared by in situ chemical polymerisation in the presence of anionic surfactant camphor sulfonic acid (CSA). The formation of composite is confirmed by X-ray Diffraction (XRD) and Energy Dispersive X-ray spectroscopy (EDX) analysis. The surface morphology was studied using Field Emission Electron Microscopy (FESEM). Optical properties was studied using UV-visible spectroscopy, it observed decrease in the band gap reveals material has potential application in optical devices. The dielectric constant and AC conductivity of composite have been studied for different temperature in the frequency range 1 kHz -1 MHz.

Characterization of mineral coatings associated with a Pleistocene-Holocene rock art style: The Northern Running Figures of the East Alligator River region, western Arnhem Land, Australia.

PubMed

King, Penelope L; Troitzsch, Ulrike; Jones, Tristen

2017-02-01

This data article contains mineralogic and chemical data from mineral coatings associated with rock art from the East Alligator River region. The coatings were collected adjacent to a rock art style known as the "Northern Running Figures" for the purposes of radiocarbon dating (doi:10.1016/j.jasrep.2016.11.016; (T. Jones, V. Levchenko, P.L. King, U. Troitzsch, D. Wesley, 2017) [1]). This contribution includes raw and processed powder X-ray Diffraction data, Scanning Electron Microscopy energy dispersive spectroscopy data, and Fourier Transform infrared spectral data.

Optical properties of hydrothermally synthesized TGA-capped CdS nanoparticles: controlling crystalline size and phase

NASA Astrophysics Data System (ADS)

Tavakoli Banizi, Zoha; Seifi, Majid

2017-10-01

TGA-capped CdS nanoparticles were obtained in the presence of thioglycolic acid (TGA) as capping agent via a facile hydrothermal method at relatively low temperature and over a short duration. As-synthesized TGA-capped CdS nanoparticles were characterized by x-ray diffraction, scanning electron microscopy, transmission electron microscopy, Fourier transform infrared spectra, photoluminescence spectroscopy, Ultraviolet-visible spectroscopy and energy-dispersive x-ray spectroscopy. The products had spherical shapes, although their crystalline size and phase was dependent on temperature and time of the reaction. Photoluminescence spectra showed that the fluorescence intensity decreased when increasing the reaction time and temperature.

Ionic liquid-templated preparation of mesoporous silica embedded with nanocrystalline sulfated zirconia

PubMed Central

2011-01-01

A series of mesoporous silicas impregnated with nanocrystalline sulphated zirconia was prepared by a sol-gel process using an ionic liquid-templated route. The physicochemical properties of the mesoporous sulphated zirconia materials were studied using characterisation techniques such as inductively coupled optical emission spectroscopy, X-ray diffraction, transmission electron microscopy, energy-dispersive X-ray microanalysis, elemental analysis and X-ray photoelectron spectroscopy. Analysis of the new silicas indicates isomorphous substitution of silicon with zirconium and reveals the presence of extremely small (< 10 nm) polydispersed zirconia nanoparticles in the materials with zirconium loadings from 27.77 to 41.4 wt.%. PMID:21711725

DOE Office of Scientific and Technical Information (OSTI.GOV)

Huang Wanzhen; Xu Zhude; Liu Run

Hierarchical flower-like MoS{sub 2} spheres with high purity were synthesized by hydrothermal method using WO{sub 3} nanorods or H{sub 2}WO{sub 4} as an additive. The flower-like spheres were about 1 {mu}m in diameter and built up with MoS{sub 2} thin flakes with thickness of several nanometers. Energy disperse X-ray spectrum showed that the spheres were only composed of Mo and S with atomic ratio of 2:1. Powder X-ray diffraction result further indicated that the products were MoS{sub 2}. The reaction mechanism is discussed and suggested that tungstenic acid played an important role on the formation of flower-like MoS{sub 2} spheres.

Hydrothermal synthesis of uniform WO{sub 3} submicrospheres using thiourea as an assistant agent

DOE Office of Scientific and Technical Information (OSTI.GOV)

Su, X.T.; Xiao, F.; Lin, J.L.

2010-08-15

Nearly monodisperse tungsten trioxide submicrospheres have been synthesized with tungsten acid and HCl as the starting materials and thiourea as a structure-directing agent through a facile hydrothermal method. The obtained products were characterized by X-ray diffraction, transmission electron microscopy, scanning electron microscopy and energy dispersive X-ray, respectively. The results show that the WO{sub 3} submicrospheres are monodisperse with a diameter of about 800-1000 nm. The morphology of the products gradually evolutes from rods to spheres with increase of the reaction time. The formation mechanism of the WO{sub 3} submicrospheres is primarily discussed.

The nature of catalyst particles and growth mechanisms of GaN nanowires grown by Ni-assisted metal-organic chemical vapor deposition.

PubMed

Weng, Xiaojun; Burke, Robert A; Redwing, Joan M

2009-02-25

The structure and chemistry of the catalyst particles that terminate GaN nanowires grown by Ni-assisted metal-organic chemical vapor deposition were investigated using a combination of electron diffraction, high-resolution transmission electron microscopy, and x-ray energy dispersive spectrometry. The crystal symmetry, lattice parameter, and chemical composition obtained reveal that the catalyst particles are Ni(3)Ga with an ordered L 1(2) structure. The results suggest that the catalyst is a solid particle during growth and therefore favor a vapor-solid-solid mechanism for the growth of GaN nanowires under these conditions.

Solvent free tin oxide nanoparticle for gas sensing application

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ranjan, Pranay, E-mail: pranjan@iitp.ac.in; Thakur, Ajay D.; Centre for Energy and Environment, Indian Institute of Technology Patna, Patliputra, Patna 800013 India

2016-05-06

A new modified technique of synthesizing tin oxide nanoparticles with crystallite size of 2 nm to 6 nm has been developed. Surface area of the nanoparticle has been increased as we approached towards the Debye length. Such a techniques for approaching the Debye length is expected to bring remarkable changes in the properties of resistive based gas sensors. The technique used here is less toxic, economical and has high yield. Phase purity, size, shape and composition has been investigated using x-ray diffraction, micro Raman, scanning electron microscopy and energy dispersive x ray spectroscopy. While surface area has been calculated through Brunaur-Emmett-Teller (BET).

Multiferroic properties in NdFeO3-PbTiO3 solid solutions

NASA Astrophysics Data System (ADS)

Kumar, Sunil; Pal, Jaswinder; Kaur, Shubhpreet; Agrawal, P.; Singh, Mandeep; Singh, Anupinder

2018-05-01

The x(NdFeO3) - 1-x(PbTiO3) where x = 0.2 solid solution was prepared using solid state reaction route. The X-ray diffraction (XRD) data reveals the single phase formation. The microstructure shows grain growth with lesser porosity. The energy dispersive analysis confirms the presence of elements in stochiometric proportion. The polarization vs. Electric field loop estabilished a ferroelectric type behavior but lossy in nature. This lossy nature may be due to the presence of large leakage current in solid solution. The Magnetization vs. Magnetic field plot exhibits a unsaturated hysteriss loop indicates that the sample is not purely ferromagnetic.

Multi-element germanium detectors for synchrotron applications

NASA Astrophysics Data System (ADS)

Rumaiz, A. K.; Kuczewski, A. J.; Mead, J.; Vernon, E.; Pinelli, D.; Dooryhee, E.; Ghose, S.; Caswell, T.; Siddons, D. P.; Miceli, A.; Baldwin, J.; Almer, J.; Okasinski, J.; Quaranta, O.; Woods, R.; Krings, T.; Stock, S.

2018-04-01

We have developed a series of monolithic multi-element germanium detectors, based on sensor arrays produced by the Forschungzentrum Julich, and on Application-specific integrated circuits (ASICs) developed at Brookhaven. Devices have been made with element counts ranging from 64 to 384. These detectors are being used at NSLS-II and APS for a range of diffraction experiments, both monochromatic and energy-dispersive. Compact and powerful readout systems have been developed, based on the new generation of FPGA system-on-chip devices, which provide closely coupled multi-core processors embedded in large gate arrays. We will discuss the technical details of the systems, and present some of the results from them.

Influence of sodium bis(2-ethylhexyl) sulfosuccinate (AOT) on zinc electrodeposition

NASA Astrophysics Data System (ADS)

Lehr, I. L.; Saidman, S. B.

2012-03-01

This work is a study of the electrodeposition of zinc onto SAE 4140 steel electrodes using solutions containing zinc sulfate and bis(2-ethylhexyl) sodium sulfosuccinate (AOT). The influence of different parameters such as electrolyte concentration, electrodeposition time and temperature on the morphology of the electrodeposits was analyzed. The deposits were characterized by scanning electron microscopy (SEM), energy dispersive X-ray (EDX) and X-ray diffraction. The variation of open circuit potential over time in chloride solutions was also evaluated. The nucleation-growth process and consequently the morphology of the electrodeposits are modified in the presence of AOT. The surfactant induces the formation of a porous deposit.

Tailoring growth conditions for efficient tuning of band edge of CdS nanoparticles

DOE Office of Scientific and Technical Information (OSTI.GOV)

Susha, N.; Nair, Swapna S., E-mail: swapna.s.nair@gmail.com; Aravind, P. B.

2015-06-24

CdS nanoparticles are successively synthesized by chemical precipitation method. The samples prepared at different reaction time and temperature are characterized by X-ray diffraction, Diffuse reflectance spectroscopy, Photoluminescence spectroscopy ans Energy dispersive x-ray analysis. Visible color variation is noted from light yellow to orange, indicates the quantum confinement effect and the results are again got confirmed from the optical studies. A shift in absorption peak is observed towards the lower region of the visible spectra - the “blue shift”- upon decrease in reaction time and temperature. Blue emission observed in the photoluminescence spectrum confirms the grain size induced confinement.

Picosecond laser fabricated Ag, Au and Ag-Au nanoparticles for detecting ammonium perchlorate using a portable Raman spectrometer

NASA Astrophysics Data System (ADS)

Byram, Chandu; Moram, Sree Sathya Bharathi; Soma, Venugopal Rao

2018-04-01

In this paper, we present the results from fabrication studies of Ag, Au, and Ag-Au alloy nanoparticles (NPs) using picosecond laser ablation technique in the presence of liquid media. The alloy formation in the NPs was confirmed from UV-Visible measurements. The shape and crystallinity of NPs were investigated by using high resolution transmission electron microscopy (HRTEM), selected area diffraction pattern (SAED) and energy dispersive spectroscopy (EDS). The SERS effect of fabricated NPs was tested with methylene blue and an explosive molecule (ammonium perchlorate) using a portable Raman spectrometer and achieved EFs of ˜106.

Clean sub-8-fs pulses at 400 nm generated by a hollow fiber compressor for ultraviolet ultrafast pump-probe spectroscopy.

PubMed

Liu, Jun; Okamura, Kotaro; Kida, Yuichiro; Teramoto, Takahiro; Kobayashi, Takayoshi

2010-09-27

Clean 7.5 fs pulses at 400 nm with less than 3% energy in tiny satellite pulses were obtained by spectral broadening in a hollow fiber and dispersive compensating using a prism pair together with a deformable mirror system. As an example, this stable and clean pulse was used to study the ultrafast pump-probe spectroscopy of photoactive yellow protein. Moreover, the self-diffraction signal shows a smoothed and broadened laser spectrum and is expected to have a further clean laser pulse, which makes it more useful in the ultrafast pump-probe spectroscopy in the future.

Fabrication and characterization of photovoltaic cell with novel configuration ITO/n-CuIn3Se5/p-CIS/In

NASA Astrophysics Data System (ADS)

Geethu, R.; Jacob, R.; Sreenivasan, P. V.; Shripathi, T.; S, Okram G.; Philip, R. R.

2015-02-01

A novel configuration ITO/n-OVC CuIn3Se5/p-CIS/In solar cell has been fabricated by multisource vacuum co-evaporation technique on soda lime glass substrates. The pn junction is formed with ordered vacancy compound as the n counter part for the p type CuInSe2. The structural, compositional, hall coefficient, optical and electrical properties of the p and n layers have been studied respectively by X-ray diffraction, Energy Dispersive Analysis of X rays, optical absorbance and conductivity measurements. Current density-Voltage measurements enabled the determination of efficiency of the device.

Spectroscopic study of Pbs nano-structured layer prepared by Pld utilized as a Hall-effect magnetic sensor

NASA Astrophysics Data System (ADS)

Atwa, D. M.; Aboulfotoh, N.; El-magd, A. Abo; Badr, Y.

2013-10-01

Lead sulfide (PbS) nano-structured films have been grown on quartz substrates using PLD technique. The deposited films were characterized by several structural techniques, including scanning electron microscopy (SEM), transmission electron microscopy (TEM), and Selected-area electron diffraction patterns (SAED). The results prove the formation of cubic phase of PbS nanocrystals. Elemental analysis of the deposited films compared to the bulk target was obtained via laser induced fluorescence of the produced plasma particles and the energy dispersive X-ray "EDX" technique. The Hall coefficient measurements indicate an efficient performance of the deposited films as a magnetic sensor.

The use of radiation for the study of material of cultural heritage significance

NASA Astrophysics Data System (ADS)

Creagh, D. C.; Otieno-Alego, V.

2004-01-01

For the indigenous people of Northern Australia the expression of their experience of life, their "dreaming", is in the form of painting, usually on the bark stripped from trees growing in their tribal lands. These are often works of great beauty and the major collecting institutions in Australia and elsewhere have significant holdings of Aboriginal bark paintings. A wide range of analytical techniques (optical microscopy, FTIR microscopy, Raman microscopy, scanning electron microscopy and energy dispersive X-ray spectroscopy, and synchrotron radiation X-ray diffraction) has been used in a project to determine how best to conserve Aboriginal bark paintings.

Oxidation of a Silica-Containing Material in a Mach 0.3 Burner Rig

NASA Technical Reports Server (NTRS)

Nguyen, QuynhGiao N.; Cuy, Michael D.; Gray, Hugh R. (Technical Monitor)

2002-01-01

A primarily silica-containing material with traces of organic compounds, as well as aluminum and calcium additions, was exposed to a Mach 0.3 burner rig at atmospheric pressure using jet fuel. The sample was exposed for 5 continuous hours at 1370 C. Post exposure x-ray diffraction analyses indicate formation of cristobalite, quartz, NiO and Spinel (Al(Ni)CR2O4). The rig hardware is composed of a nickel-based superalloy with traces of Fe. These elements are indicated in the energy dispersive spectroscopy (EDS) results. This material was studied as a candidate for high temperature applications under an engine technology program.

Synthesis, characterizations and catalytic activities of CoFe2O4 nanoparticles

NASA Astrophysics Data System (ADS)

Verma, Divya; Sharma, Vikash; Parmar, Sarita; Okram, Gunadhor Singh; Jain, Shubha

2018-05-01

We report the synthesis of CoFe2O4 nanoparticles (NPs) through a novel one-step coprecipitation method. These NPs were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDAX), Fourier transform infrared (FTIR), and Raman spectroscopy. These nano ferrites were successfully used for the synthesis of 3, 4-dihydropyrimidin-2(1H)-ones and thiones. They can be easily recovered by simple filtration and their catalytic activity remains nearly unaltered even after 4 consecutive cycles, making them ecofriendly and widely applicable due to their efficiency, ease of handling, and cost effectiveness.

Hyperbranched-polymer dispersed nanocomposite volume gratings for holography and diffractive optics

NASA Astrophysics Data System (ADS)

Tomita, Yasuo; Takeuchi, Shinsuke; Oyaizu, Satoko; Urano, Hiroshi; Fukamizu, Taka-aki; Nishimura, Naoya; Odoi, Keisuke

2016-10-01

We review our experimental investigations of photopolymerizable nanoparticle-polymer composites (NPCs) for holography and diffractive optics. Various types of hyperbranched polymer (HBP) were systhesized and used as transporting organic nanoparticles. These HBPs include hyperbranched poly(ethyl methacrylate) (HPEMA), hyperbranched polystyrene (HPS) and hyperbranched triazine/aromatic polymer units (HTA) whose refractive indices are 1.51, 1.61 and 1.82, respectively. Each HBP was dispersed in (meth)acrylate monomer whose refractive index was so chosen that a refractive index difference between HBP and the formed polymer was large. Such monomer-HBP syrup was mixed with a titanocene photoinitiator for volume holographic recording in the green. We used a two-beam interference setup to write an unslanted transmission volume grating at grating spacing of 1 μm and at a wavelength of 532 nm. It is shown that NPC volume gratings with the saturated refractive index modulation amplitudes as large as 0.008, 0.004 and 0.02 can be recorded in NPCs incorporated with HPEMA, HPS and HTA at their optimum concentrations of 34, 34 and 25 vol.%, respectively. We show the usefulness of HBP-dispersed NPC volume gratings for holographic applications such as holographic data storage and diffractive optical devices.

Development of megestrol acetate solid dispersion nanoparticles for enhanced oral delivery by using a supercritical antisolvent process.

PubMed

Ha, Eun-Sol; Kim, Jeong-Soo; Baek, In-Hwan; Yoo, Jin-Wook; Jung, Yunjin; Moon, Hyung Ryong; Kim, Min-Soo

2015-01-01

In the present study, solid dispersion nanoparticles with a hydrophilic polymer and surfactant were developed using the supercritical antisolvent (SAS) process to improve the dissolution and oral absorption of megestrol acetate. The physicochemical properties of the megestrol acetate solid dispersion nanoparticles were characterized using scanning electron microscopy, differential scanning calorimetry, powder X-ray diffraction, and a particle-size analyzer. The dissolution and oral bioavailability of the nanoparticles were also evaluated in rats. The mean particle size of all solid dispersion nanoparticles that were prepared was <500 nm. Powder X-ray diffraction and differential scanning calorimetry measurements showed that megestrol acetate was present in an amorphous or molecular dispersion state within the solid dispersion nanoparticles. Hydroxypropylmethyl cellulose (HPMC) solid dispersion nanoparticles significantly increased the maximum dissolution when compared with polyvinylpyrrolidone K30 solid dispersion nanoparticles. The extent and rate of dissolution of megestrol acetate increased after the addition of a surfactant into the HPMC solid dispersion nanoparticles. The most effective surfactant was Ryoto sugar ester L1695, followed by D-α-tocopheryl polyethylene glycol 1000 succinate. In this study, the solid dispersion nanoparticles with a drug:HPMC:Ryoto sugar ester L1695 ratio of 1:2:1 showed >95% rapid dissolution within 30 minutes, in addition to good oral bioavailability, with approximately 4.0- and 5.5-fold higher area under the curve (0-24 hours) and maximum concentration, respectively, than raw megestrol acetate powder. These results suggest that the preparation of megestrol acetate solid dispersion nanoparticles using the supercritical antisolvent process is a promising approach to improve the dissolution and absorption properties of megestrol acetate.

Method for improve x-ray diffraction determinations of residual stress in nickel-base alloys

DOEpatents

Berman, Robert M.; Cohen, Isadore

1990-01-01

A process for improving the technique of measuring residual stress by x-ray diffraction in pieces of nickel-base alloys which comprises covering part of a predetermined area of the surface of a nickel-base alloy with a dispersion, exposing the covered and uncovered portions of the surface of the alloy to x-rays by way of an x-ray diffractometry apparatus, making x-ray diffraction determinations of the exposed surface, and measuring the residual stress in the alloy based on these determinations. The dispersion is opaque to x-rays and serves a dual purpose since it masks off unsatisfactory signals such that only a small portion of the surface is measured, and it supplies an internal standard by providing diffractogram peaks comparable to the peaks of the nickel alloy so that the alloy peaks can be very accurately located regardless of any sources of error external to the sample.

Diffraction enhanced kinetic depth X-ray imaging

NASA Astrophysics Data System (ADS)

Dicken, A.

An increasing number of fields would benefit from a single analytical probe that can characterise bulk objects that vary in morphology and/or material composition. These fields include security screening, medicine and material science. In this study the X-ray region is shown to be an effective probe for the characterisation of materials. The most prominent analytical techniques that utilise X-radiation are reviewed. The study then focuses on methods of amalgamating the three dimensional power of kinetic depth X-ray (KDFX) imaging with the materials discrimination of angular dispersive X-ray diffraction (ADXRD), thus providing KDEX with a much needed material specific counterpart. A knowledge of the sample position is essential for the correct interpretation of diffraction signatures. Two different sensor geometries (i.e. circumferential and linear) that are able to collect end interpret multiple unknown material diffraction patterns and attribute them to their respective loci within an inspection volume are investigated. The circumferential and linear detector geometries are hypothesised, simulated and then tested in an experimental setting with the later demonstrating a greater ability at discerning between mixed diffraction patterns produced by differing materials. Factors known to confound the linear diffraction method such as sample thickness and radiation energy have been explored and quantified with a possible means of mitigation being identified (i.e. via increasing the sample to detector distance). A series of diffraction patterns (following the linear diffraction approach) were obtained from a single phantom object that was simultaneously interrogated via KDEX imaging. Areas containing diffraction signatures matched from a threat library have been highlighted in the KDEX imagery via colour encoding and match index is inferred by intensity. This union is the first example of its kind and is called diffraction enhanced KDEX imagery. Finally an additional source of information obtained from object disparity is explored as an alternative means of calculating sample loci. This offers a greater level of integration between these two complimentary techniques as object disparity could be used to reinforce the results produced by the linear diffraction geometry.

High-throughput and in situ EDXRD investigation on the formation of two new metal aminoethylphosphonates - Ca(O{sub 3}PC{sub 2}H{sub 4}NH{sub 2}) and Ca(OH)(O{sub 3}PC{sub 2}H{sub 4}NH{sub 3}){center_dot}2H{sub 2}O

DOE Office of Scientific and Technical Information (OSTI.GOV)

Schmidt, Corinna; Feyand, Mark; Rothkirch, Andre

2012-04-15

The system Ca{sup 2+}/2-aminoethylphosphonic acid/H{sub 2}O/NaOH was systematically investigated using high-throughput methods. The experiments led to one new compound Ca(O{sub 3}PC{sub 2} H{sub 4}NH{sub 2}) (1) and the crystal structure was determined using in house X-ray powder diffraction data (monoclinic, P2{sub 1}/c, a=9.7753(3), b=6.4931(2), c=8.4473(2) A, {beta}=106.46(2) Degree-Sign , V=514.20(2) A{sup 3}, Z=4). The formation of 1 was investigated by in situ energy dispersive X-ray diffraction measurements (EDXRD) at beamline F3 at HASYLAB (light source DORIS III), DESY, Hamburg. An intermediate, Ca(OH)(O{sub 3}PC{sub 2}H{sub 4}NH{sub 3}){center_dot}2H{sub 2}O (2), was observed and could be isolated from the reaction mixture at ambientmore » temperatures by quenching the reaction. The crystal structure of 2 was determined from XRPD data using synchrotron radiation (monoclinic, P2{sub 1}/m, a=11.2193(7), b=7.1488(3), c=5.0635(2) A, {beta}=100.13(4) Degree-Sign , V=399.78(3) A{sup 3}, Z=2). - Graphical abstarct: The detailed in situ energy dispersive X-ray diffraction (EDXRD) investigation on the formation of the new inorganic-organic hybrid compound Ca(O{sub 3}PC{sub 2}H{sub 4}NH{sub 2}) leads to the discovery of a new crystalline intermediate phase. Both crystal structures were elucidated using X-ray powder diffraction data. Highlights: Black-Right-Pointing-Pointer High-throughput investigation led to new metal aminoethylphosphonate Ca(O{sub 3}PC{sub 2}H{sub 4}NH{sub 2}). Black-Right-Pointing-Pointer The formation of Ca(O{sub 3}PC{sub 2}H{sub 4}NH{sub 2}) was followed by in situ EDXRD measurements. Black-Right-Pointing-Pointer The crystalline intermediate Ca(O{sub 3}PC{sub 2}H{sub 4}NH{sub 3})(OH){center_dot}2H{sub 2}O was discovered. Black-Right-Pointing-Pointer Isolation of Ca(O{sub 3}PC{sub 2}H{sub 4}NH{sub 3})(OH){center_dot}2H{sub 2}O was accomplished by quenching experiments. Black-Right-Pointing-Pointer The structures were determined using X-ray powder diffraction data.« less

Ultrasonic irradiation-assisted synthesis of Bi2S3 nanoparticles in aqueous ionic liquid at ambient condition.

PubMed

de la Parra-Arciniega, Salomé M; Garcia-Gomez, Nora A; Garza-Tovar, Lorena L; García-Gutiérrez, Domingo I; Sánchez, Eduardo M

2017-05-01

In this work, an easy, fast and environmentally friendly method to obtain Bi 2 S 3 nanostructures with sphere-like morphology is introduced. The promising material was successfully synthesized by a sonochemical route in 20% 1-ethyl-3-methylimidazolium ethyl sulfate [EMIM][EtSO 4 ] ionic liquid solution (IL). Morphological studies by electron microscopy (SEM and TEM) show that the use of IL in the synthesis of Bi 2 S 3 favors the formation of nanocrystals non-agglomerated. Micro Raman and energy dispersive X-ray spectroscopy (EDXS) were used to determine the composition and purity of the synthesized material. X-ray powder diffraction (XRD) and selective area electron diffraction (SAED) revealed that ultrasonic radiation accelerated the crystallization of Bi 2 S 3 into orthorhombic bismuthinite structure. The band gap calculated from the diffuse reflectance spectra (DRS) was found to be 1.5eV. Copyright © 2016 Elsevier B.V. All rights reserved.

Catalytic Graphitization of Coal-Based Carbon Materials with Light Rare Earth Elements.

PubMed

Wang, Rongyan; Lu, Guimin; Qiao, Wenming; Yu, Jianguo

2016-08-30

The catalytic graphitization mechanism of coal-based carbon materials with light rare earth elements was investigated using X-ray diffraction, scanning electron microscopy, energy-dispersive X-ray spectroscopy, selected-area electron diffraction, and high-resolution transmission electron microscopy. The interface between light rare earth elements and carbon materials was carefully observed, and two routes of rare earth elements catalyzing the carbon materials were found: dissolution-precipitation and carbide formation-decomposition. These two simultaneous processes certainly accelerate the catalytic graphitization of carbon materials, and light rare earth elements exert significant influence on the microstructure and thermal conductivity of graphite. Moreover, by virtue of praseodymium (Pr), it was found that a highly crystallographic orientation of graphite was induced and formed, which was reasonably attributed to the similar arrangements of the planes perpendicular to (001) in both graphite and Pr crystals. The interface between Pr and carbon was found to be an important factor for the orientation of graphite structure.

Synthesis of silver nanoparticles using leaves of Catharanthus roseus Linn. G. Don and their antiplasmodial activities

PubMed Central

Ponarulselvam, S; Panneerselvam, C; Murugan, K; Aarthi, N; Kalimuthu, K; Thangamani, S

2012-01-01

Objective To develop a novel approach for the green synthesis of silver nanoparticles using aqueous leaves extracts of Catharanthus roseus (C. roseus) Linn. G. Don which has been proven active against malaria parasite Plasmodium falciparum (P. falciparum). Methods Characterizations were determined by using ultraviolet-visible (UV-Vis) spectrophotometry, scanning electron microscopy (SEM), energy dispersive X-ray and X-ray diffraction. Results SEM showed the formation of silver nanoparticles with an average size of 35–55 nm. X-ray diffraction analysis showed that the particles were crystalline in nature with face centred cubic structure of the bulk silver with the broad peaks at 32.4, 46.4 and 28.0. Conclusions It can be concluded that the leaves of C. roseus can be good source for synthesis of silver nanoparticle which shows antiplasmodial activity against P. falciparum. The important outcome of the study will be the development of value added products from medicinal plants C. roseus for biomedical and nanotechnology based industries. PMID:23569974

Latex-mediated synthesis of ZnS nanoparticles: green synthesis approach

NASA Astrophysics Data System (ADS)

Hudlikar, Manish; Joglekar, Shreeram; Dhaygude, Mayur; Kodam, Kisan

2012-05-01

A low-cost, green synthesis of ZnS nanoparticles is reported using 0.3 % latex solution prepared from Jatropha curcas L. ZnS nanoparticles were characterized by X-ray diffraction, selected area electron diffraction, transmission electron microscopy, energy dispersive analysis of X-rays, UV-vis optical absorption and photoluminescence techniques. Fourier Transform Infrared Spectroscopy was performed to find the role of cyclic peptides namely curcacycline A (an octapeptide), curcacycline B (a nonapeptide) and curcain (an enzyme) as a possible reducing and stabilizing agents present in the latex of J. curcas L. The average size of ZnS nanoparticles was found to be 10 nm. Latex of J. curcas L. itself acts as a source of sulphide (S-2) ions that are donated to Zn ions under present experimental conditions. Source of sulphide (S-2) ions is still unclear, but we speculate that cysteine or thiol residues present in enzyme curcain may be donating these sulphide (S-2) ions.

Electronic and geometric structure of thin CoO(100) films studied by angle-resolved photoemission spectroscopy and Auger electron diffraction

NASA Astrophysics Data System (ADS)

Heiler, M.; Chassé, A.; Schindler, K.-M.; Hollering, M.; Neddermeyer, H.

2000-05-01

We have prepared ordered thin films of CoO by evaporating cobalt in an O 2 atmosphere on to a heated (500 K) Ag(100) substrate. The geometric and electronic structure of the films was characterized by means of Auger electron diffraction (AED) and angle-resolved photoemission spectroscopy (ARUPS), respectively. The experimental AED results were compared with simulated data, which showed that the film grows in (100) orientation on the Ag(100) substrate. Synchrotron-radiation-induced photoemission investigations were performed in the photon energy range from 25 eV to 67 eV. The dispersion of the transitions was found to be similar to that of previous results on a single-crystal CoO(100) surface. The resonance behaviour of the photoemission lines in the valence-band region was investigated by constant-initial-state (CIS) spectroscopy. The implications of this behaviour for assignment of the photoemission lines to specific electronic transitions is discussed and compared with published theoretical models of the electronic structure.

Facile synthesis of hollow Co3O4 microspheres and its use as a rapid responsive CL sensor of combustible gases.

PubMed

Teng, Fei; Yao, Wenqing; Zheng, Youfei; Ma, Yutao; Xu, Tongguang; Gao, Guizhi; Liang, Shuhui; Teng, Yang; Zhu, Yongfa

2008-09-15

The hollow Co(3)O(4) microspheres (HCMs) were prepared by the carbonaceous templates, which did not need the surface pretreatment. The chemiluminescence (CL) and catalytic properties for CO oxidation over these hollow samples were evaluated. The samples were characterized by scanning electron microscopy (SEM), energy disperse spectra (EDS), transmission electron microscopy (TEM), selected area electron diffraction (ED), X-ray diffraction (XRD), temperature-programmed desorption (TPD) and N(2) adsorption. The influences of filter' band length, flow rate of gas, test temperature, and particle structure on CL intensities were mainly investigated. It was found that compared with the solid Co(3)O(4) particles (SCPs), HCMs had a stronger CL intensity, which was ascribed to its hollow structure; and that CL properties of the catalysts were well correlated with their reaction activities. Moreover, HCMs were used to fabricate a highly sensitive gas detector, which is a rapid and effective method for the selection of catalysts or the detection of environmental deleterious gases.

Au crystal growth on natural occurring Au-Ag aggregate elucidated by means of precession electron diffraction (PED)

NASA Astrophysics Data System (ADS)

Roqué Rosell, Josep; Portillo Serra, Joaquim; Aiglsperger, Thomas; Plana-Ruiz, Sergi; Trifonov, Trifon; Proenza, Joaquín A.

2018-02-01

In the present work, a lamella from an Au-Ag aggregate found in Ni-laterites has been examined using Transmission Electron Microscope to produce a series of Precision Electron Diffraction (PED) patterns. The analysis of the structural data obtained, coupled with Energy Dispersive X-ray microanalysis, made it possible to determine the orientation of twinned native gold growing on the Au-Ag aggregate. The native Au crystal domains are found to have grown at the outermost part of the aggregate whereas the inner core of the aggregate is an Au-Ag alloy (∼4 wt% Ag). The submicron structural study of the natural occurring Au aggregate points to the mobilization and precipitation of gold in laterites and provides insights on Au aggregates development at supergene conditions. This manuscript demonstrates the great potential of electron crystallographic analysis, and in particular, PED to study submicron structural features of micron sized mineral aggregates by using the example of a gold grain found in a Ni-laterite deposits.

Intramolecular π-π Interactions in Flexibly Linked Partially Fluorinated Bisarenes in the Gas Phase.

PubMed

Blomeyer, Sebastian; Linnemannstöns, Marvin; Nissen, Jan Hendrick; Paulus, Jannik; Neumann, Beate; Stammler, Hans-Georg; Mitzel, Norbert W

2017-10-16

Three compounds with phenyl and pentafluorophenyl rings bridged by (CH 2 ) 3 and (CH 2 ) 2 SiMe 2 units were synthesized by hydrosilylation and C-C coupling reactions. Their solid-state structures are dominated by intermolecular π stacking interactions, primarily leading to dimeric or chain-type aggregates. Analysis of free molecules in the gas phase by electron diffraction revealed the most abundant conformer to be significantly stabilized by intramolecular π-π interactions. For the silicon compounds, structures characterized by σ-π interactions between methyl and pentafluorophenyl groups are second lowest in energy and cannot be excluded completely by the gas electron diffraction experiments. C 6 H 5 (CH 2 ) 3 C 6 F 5 , in contrast, is present as a single conformer. The gas-phase structures served as a reference for the evaluation of a series of (dispersion-corrected) quantum-chemical calculations. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Tungsten tetraboride, an inexpensive superhard material

PubMed Central

Mohammadi, Reza; Lech, Andrew T.; Xie, Miao; Weaver, Beth E.; Yeung, Michael T.; Tolbert, Sarah H.; Kaner, Richard B.

2011-01-01

Tungsten tetraboride (WB4) is an interesting candidate as a less expensive member of the growing group of superhard transition metal borides. WB4 was successfully synthesized by arc melting from the elements. Characterization using powder X-ray diffraction (XRD) and energy-dispersive X-ray spectroscopy (EDX) indicates that the as-synthesized material is phase pure. The zero-pressure bulk modulus, as measured by high-pressure X-ray diffraction for WB4, is 339 GPa. Mechanical testing using microindentation gives a Vickers hardness of 43.3 ± 2.9 GPa under an applied load of 0.49 N. Various ratios of rhenium were added to WB4 in an attempt to increase hardness. With the addition of 1 at.% Re, the Vickers hardness increased to approximately 50 GPa at 0.49 N. Powders of tungsten tetraboride with and without 1 at.% Re addition are thermally stable up to approximately 400 °C in air as measured by thermal gravimetric analysis. PMID:21690363

Synthesis, Characterization, and Mechanism of Formation of Janus-Like Nanoparticles of Tantalum Silicide-Silicon (TaSi2/Si)

PubMed Central

Nomoev, Andrey V.; Bardakhanov, Sergey P.; Schreiber, Makoto; Bazarova, Dashima Zh.; Baldanov, Boris B.; Romanov, Nikolai A.

2014-01-01

Metal-semiconductor Janus-like nanoparticles with the composition tantalum silicide-silicon (TaSi2/Si) were synthesized for the first time by means of an evaporation method utilizing a high-power electron beam. The composition of the synthesized particles were characterized using high-resolution transmission electron microscopy (HRTEM), X-ray diffraction (XRD), selective area electron diffraction (SAED), and energy dispersive X-ray fluorescence (EDX) analysis. The system is compared to previously synthesized core-shell type particles in order to show possible differences responsible for the Janus-like structure forming instead of a core-shell architecture. It is proposed that the production of Janus-like as opposed to core-shell or monophase particles occurs due to the ability of Ta and Si to form compounds and the relative content of Ta and Si atoms in the produced vapour. Based on the results, a potential mechanism of formation for the TaSi2/Si nanoparticles is discussed. PMID:28346996

Synthesis, Characterization, and Mechanism of Formation of Janus-Like Nanoparticles of Tantalum Silicide-Silicon (TaSi₂/Si).

PubMed

Nomoev, Andrey V; Bardakhanov, Sergey P; Schreiber, Makoto; Bazarova, Dashima Zh; Baldanov, Boris B; Romanov, Nikolai A

2014-12-25

Metal-semiconductor Janus-like nanoparticles with the composition tantalum silicide-silicon (TaSi₂/Si) were synthesized for the first time by means of an evaporation method utilizing a high-power electron beam. The composition of the synthesized particles were characterized using high-resolution transmission electron microscopy (HRTEM), X-ray diffraction (XRD), selective area electron diffraction (SAED), and energy dispersive X-ray fluorescence (EDX) analysis. The system is compared to previously synthesized core-shell type particles in order to show possible differences responsible for the Janus-like structure forming instead of a core-shell architecture. It is proposed that the production of Janus-like as opposed to core-shell or monophase particles occurs due to the ability of Ta and Si to form compounds and the relative content of Ta and Si atoms in the produced vapour. Based on the results, a potential mechanism of formation for the TaSi₂/Si nanoparticles is discussed.

Controllable synthesis of protein-conjugated lead sulfide nanocubes by using bovine hemoglobin as a capping agent

NASA Astrophysics Data System (ADS)

Yang, Guangrui; Qin, Dezhi; Zhang, Li

2014-06-01

A simple, convenient, and controllable strategy was reported in this contribution for protein-assisted synthesis BHb-conjugated PbS nanocubes. Powder X-ray diffraction, energy disperse X-ray spectroscopy, transmission electron microscopy, high-resolution transmission electron microscopy, and selected-area electron diffraction characterizations were used to determine the structure and morphology of BHb-conjugated PbS nanocubes. The prepared PbS nanocrystals with cubic rock salt structure were uniform and monodispersed with homogeneous size around 12 nm. The results of Fourier transform infrared and circular dichroism assay proved that Pb2+/PbS had coordination interaction with functional groups of BHb besides physical-binding effect, and the secondary structure of protein significantly changed with this interaction. Thermogravimetric analysis results confirmed the existence of BHb in PbS nanocrystals and indicated that the conjugate bonds existed between PbS and BHb. A clear perspective was shown here that special nanostructure could be created by using proteins as a mediating template at the inorganic-organic interface.

Optical determination of crystal phase in semiconductor nanocrystals

PubMed Central

Lim, Sung Jun; Schleife, André; Smith, Andrew M.

2017-01-01

Optical, electronic and structural properties of nanocrystals fundamentally derive from crystal phase. This is especially important for polymorphic II–VI, III–V and I-III-VI2 semiconductor materials such as cadmium selenide, which exist as two stable phases, cubic and hexagonal, each with distinct properties. However, standard crystallographic characterization through diffraction yields ambiguous phase signatures when nanocrystals are small or polytypic. Moreover, diffraction methods are low-throughput, incompatible with solution samples and require large sample quantities. Here we report the identification of unambiguous optical signatures of cubic and hexagonal phases in II–VI nanocrystals using absorption spectroscopy and first-principles electronic-structure theory. High-energy spectral features allow rapid identification of phase, even in small nanocrystals (∼2 nm), and may help predict polytypic nanocrystals from differential phase contributions. These theoretical and experimental insights provide simple and accurate optical crystallographic analysis for liquid-dispersed nanomaterials, to improve the precision of nanocrystal engineering and improve our understanding of nanocrystal reactions. PMID:28513577

Fabrication and Characterization of Surrogate Fuel Particles Using the Spark Erosion Method

NASA Astrophysics Data System (ADS)

Metzger, Kathryn E.

In light of the disaster at the Fukushima Daiichi Nuclear Plant, the Department of Energy's Advanced Fuels Program has shifted its interest from enhanced performance fuels to enhanced accident tolerance fuels. Dispersion fuels possess higher thermal conductivities than traditional light water reactor fuel and as a result, offer improved safety margins. The benefits of a dispersion fuel are due to the presence of the secondary non-fissile phase (matrix), which serves as a barrier to fission products and improves the overall thermal performance of the fuel. However, the presence of a matrix material reduces the fuel volume, which lowers the fissile content of dispersion. This issue can be remedied through the development of higher density fuel phases or through an optimization of fuel particle size and volume loading. The latter requirement necessitates the development of fabrication methods to produce small, micron-order fuel particles. This research examines the capabilities of the spark erosion process to fabricate particles on the order of 10 μm. A custom-built spark erosion device by CT Electromechanica was used to produce stainless steel surrogate fuel particles in a deionized water dielectric. Three arc intensities were evaluated to determine the effect on particle size. Particles were filtered from the dielectric using a polycarbonate membrane filter and vacuum filtration system. Fabricated particles were characterized via field emission scanning electron microscopy (FESEM), laser light particle size analysis, energy-dispersive spectroscopy (EDS), X-ray diffraction analysis (XRD), and gas pycnometry. FESEM images reveal that the spark erosion process produces highly spherical particles on the order of 10 microns. These findings are substantiated by the results of particle size analysis. Additionally, EDS and XRD results indicate the presence of oxide phases, which suggests the dielectric reacted with the molten debris during particle formation.

Atmospheric dispersion corrector for the Large Sky Area Multi-Object Fibre Spectroscopic Telescope

NASA Astrophysics Data System (ADS)

Su, Ding-Qiang; Jia, Peng; Liu, Genrong

2012-02-01

The Large Sky Area Multi-Object Fibre Spectroscopic Telescope (LAMOST) is the largest, wide field-of-view (FOV) telescope (with an aperture of 4 m), and it is equipped with the highest number (4000) of optical fibres in the world. For the LAMOST North and the LAMOST South, the FOVs are 5° and 3.5°, respectively, and the linear diameters are 1.75 m and 1.22 m, respectively. A new type of atmospheric dispersion corrector (ADC) is put forward and designed for LAMOST. It is a segmented lens, which consists of many lens-prism strips. Although it is very large, its thickness is only 12 mm. Thus, the difficulty of obtaining a large optical glass is avoided, and the aberration caused by the ADC is small. By moving this segmented lens along the optical axis, different dispersions can be obtained. We discuss the effects of ADC's slits on the diffraction energy distribution and on the obstruction of light. We calculate and discuss the aberration caused by the ADC. All these results are acceptable. Such an ADC could also be used for other optical fibre spectroscopic telescopes, especially those which a have very large FOV.

Pilot-plant evaluation of TiO2 and TiO2-based hybrid photocatalysts for solar treatment of polluted water.

PubMed

Andronic, Luminita; Isac, Luminita; Miralles-Cuevas, Sara; Visa, Maria; Oller, Isabel; Duta, Anca; Malato, Sixto

2016-12-15

Materials with photocatalytic and adsorption properties for advanced wastewater treatment targeting reuse were studied. Making use of TiO 2 as a well-known photocatalyst, Cu 2 S as a Vis-active semiconductor, and fly ash as a good adsorbent, dispersed mixtures/composites were prepared to remove pollutants from wastewater. X-ray diffraction, scanning electron microscopy, energy-dispersive X-Ray spectroscopy, atomic force microscopy, band gap energy, point of zero charge (pH pzc ) and BET porosity were used to characterize the substrates. Phenol, imidacloprid and dichloroacetic acid were used as pollutants for photocatalytic activity of the new photocatalysts. Experiments using the new dispersed powders were carried out at laboratory scale in two solar simulators and under natural solar irradiation at the Plataforma Solar de Almería, in a Compound Parabolic Collector (CPC) for a comparative analysis of pollutants removal and mineralization efficiencies, and to identify features that could facilitate photocatalyst separation and reuse. The results show that radiation intensity significantly affects the phenol degradation rate. The composite mixture of TiO 2 and fly ash is 2-3 times less active than sol-gel TiO 2 . Photodegradation kinetic data on the highly active TiO 2 are compared for pollutants elimination. Photodegradation of dichloroacetic acid was fast and complete after 90min in the CPC, while after 150min imidacloprid and phenol removal was 90% and 56% respectively. Copyright © 2016 Elsevier B.V. All rights reserved.

Monolithic hybrid optics for focusing ultrashort laser pulses

NASA Astrophysics Data System (ADS)

Fuchs, U.

2014-03-01

Almost any application of ultrashort laser pulses involves focusing them in order to reach high intensities and/or small spot sizes as needed for micro-machining or Femto-LASIK. Hence, it is indispensable to be able to understand pulse front distortion caused by real world optics. Focusing causes pulse front distortion due to aberrations, dispersion and diffraction. Thus, the spatio-temporal profile of ultrashort laser is altered, which increases automatically the pulse duration and the focusing spot. Consequently, the main advantage of having ultrashort laser pulses - pulse durations way below 100 fs - can be lost in that one last step of the experimental set-up by focusing them unfavorable. Since compensating for dispersion, aberration and diffraction effects is quite complicated and not always possible, we pursue a different approach. We present a specially designed monolithic hybrid optics comprising refraction and diffraction effects for tight spatial and temporal focusing of ultrashort laser pulses. Both aims can be put into practice by having a high numerical aperture (NA = 0.35) and low internal dispersion at the same time. The focusing properties are very promising, due to a design, which provides diffraction limited focusing for 100 nm bandwidth at 780 nm center wavelength. Thus, pulses with durations as short as 10 fs can be focused without pulse front distortion. The outstanding performance of this optics is shown in theory and experimentally. Above that, such focusing optics are easily adapted to their special purpose - changing the center wavelength, achromatic bandwidth or even correcting for focusing into material is possible.

Detection Limit of Smectite by Chemin IV Laboratory Instrument: Preliminary Implications for Chemin on the Mars Science Laboratory Mission

NASA Technical Reports Server (NTRS)

Archilles, Cherie; Ming, D. W.; Morris, R. V.; Blake, D. F.

2011-01-01

The CheMin instrument on the Mars Science Laboratory (MSL) is an miniature X-ray diffraction (XRD) and X-ray fluorescence (XRF) instrument capable of detecting the mineralogical and elemental compositions of rocks, outcrops and soils on the surface of Mars. CheMin uses a microfocus-source Co X-ray tube, a transmission sample cell, and an energy-discriminating X-ray sensitive CCD to produce simultaneous 2-D XRD patterns and energy-dispersive X-ray histograms from powdered samples. CRISM and OMEGA have identified the presence of phyllosilicates at several locations on Mars including the four candidate MSL landing sites. The objective of this study was to conduct preliminary studies to determine the CheMin detection limit of smectite in a smectite/olivine mixed mineral system.

Steam Oxidation Behavior of Alloy 617 at 900 °C to 1100 °C

NASA Astrophysics Data System (ADS)

Liang, Zhiyuan; Wang, Yungang; Zhao, Qinxin

2018-07-01

The steam oxidation behavior of solid solution strengthened alloy 617 at 900 °C-1100 °C was investigated. The oxidation products were characterized by scanning electron microscopy, X-ray diffraction, and energy-dispersive spectroscopy. The results show that the oxidation kinetics of alloy 617 in steam followed the parabolic oxidation law. The calculated activity energy of alloy 617 was 223.47 kJ/mol. The oxidation products were mainly composed of external and internal scales and prior oxides at grain boundaries. External oxide scales were MnCr2O4, TiO2, and Cr2O3. Internal oxidation scales and prior oxides were Al2O3 and some Cr2O3 dissolved into Al2O3. The growth mechanism of oxide scales on alloy 617 is proposed.

Steam Oxidation Behavior of Alloy 617 at 900 °C to 1100 °C

NASA Astrophysics Data System (ADS)

Liang, Zhiyuan; Wang, Yungang; Zhao, Qinxin

2018-05-01

The steam oxidation behavior of solid solution strengthened alloy 617 at 900 °C-1100 °C was investigated. The oxidation products were characterized by scanning electron microscopy, X-ray diffraction, and energy-dispersive spectroscopy. The results show that the oxidation kinetics of alloy 617 in steam followed the parabolic oxidation law. The calculated activity energy of alloy 617 was 223.47 kJ/mol. The oxidation products were mainly composed of external and internal scales and prior oxides at grain boundaries. External oxide scales were MnCr2O4, TiO2, and Cr2O3. Internal oxidation scales and prior oxides were Al2O3 and some Cr2O3 dissolved into Al2O3. The growth mechanism of oxide scales on alloy 617 is proposed.

Using Flory-Huggins phase diagrams as a pre-formulation tool for the production of amorphous solid dispersions: a comparison between hot-melt extrusion and spray drying.

PubMed

Tian, Yiwei; Caron, Vincent; Jones, David S; Healy, Anne-Marie; Andrews, Gavin P

2014-02-01

Amorphous drug forms provide a useful method of enhancing the dissolution performance of poorly water-soluble drugs; however, they are inherently unstable. In this article, we have used Flory-Huggins theory to predict drug solubility and miscibility in polymer candidates, and used this information to compare spray drying and melt extrusion as processes to manufacture solid dispersions. Solid dispersions were prepared using two different techniques (hot-melt extrusion and spray drying), and characterised using a combination of thermal (thermogravimetric analysis and differential scanning calorimetry), spectroscopic (Fourier transform infrared spectroscopy (FTIR) and X-ray diffraction methods. Spray drying permitted generation of amorphous solid dispersions across a wider drug concentration than melt extrusion. Melt extrusion provided sufficient energy for more intimate mixing to be achieved between drug and polymer, which may improve physical stability. It was also confirmed that stronger drug-polymer interactions might be generated through melt extrusion. Remixing and dissolution of recrystallised felodipine into the polymeric matrices did occur during the modulated differential scanning calorimetry analysis, but the complementary information provided from FTIR confirms that all freshly prepared spray-dried samples were amorphous with the existence of amorphous drug domains within high drug-loaded samples. Using temperature-composition phase diagrams to probe the relevance of temperature and drug composition in specific polymer candidates facilitates polymer screening for the purpose of formulating solid dispersions. © 2013 Royal Pharmaceutical Society.

Structural characterization and optical constants of CuIn3Se5 vacuum and air annealed thin films

NASA Astrophysics Data System (ADS)

Segmane, N. E. H.; Abdelkader, D.; Amara, A.; Drici, A.; Akkari, F. Chaffar; Khemiri, N.; Bououdina, M.; Kanzari, M.; Bernède, J. C.

2018-01-01

Milled powder of ordered defect compound (ODC) CuIn3Se5 phase was successfully synthesized via milling process. Thin films of CuIn3Se5 were deposited onto glass substrates at room temperature by thermal evaporation technique. The obtained layers were annealed in vacuum and air atmosphere. The structural and compositional properties of the powder were analyzed using X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS). Powder XRD characterization, Rietveld analysis and chemical bounding confirm the tetragonal ordered defect compound phase formation with lattice constants a = 5.732 Å and c = 11.575 Å. Thin films were characterized by XRD, atomic force microscopy (AFM) and UV/Vis spectroscopy. Transmittance (T) and reflectance (R) spectra were measured in the spectral range of 300-1800 nm. The absorption coefficient α exhibits high values in the visible range and reaches a value of 105 cm-1. The band gap energy Eg of the annealed thin films is estimated to be approximately 1.75 eV. The refractive index n was estimated from transmittance data using Swanepoel's method. The refractive indices of the films as a function of wavelengths can be fitted with Cauchy dispersion equation. The oscillator energy E0, dispersion energy Ed, zero frequency refractive index n0, high frequency dielectric constant ε∞ and the carrier concentration per effective mass N/m∗ values were determined from the analysis of the experimental data using Wemple-DiDomenico and Spitzer-Fan models. We exploited the refractive index dispersion for the determination of the magneto-optical constant V, which characterizes the Faraday rotation. The nonlinear optical parameters namely nonlinear susceptibility χ(3), nonlinear refractive index and nonlinear absorption coefficient β are investigated for the first time for CuIn3Se5 material.

Morphology and dispersion of FeCo alloy nanoparticles dispersed in a matrix of IR pyrolized polyvinyl alcohol

NASA Astrophysics Data System (ADS)

Vasilev, A. A.; Dzidziguri, E. L.; Muratov, D. G.; Zhilyaeva, N. A.; Efimov, M. N.; Karpacheva, G. P.

2018-04-01

Metal-carbon nanocomposites consisting of FeCo alloy nanoparticles dispersed in a carbon matrix were synthesized by the thermal decomposition method of a precursor based on polyvinyl alcohol and metals salts. The synthesized powders were investigated by X-ray diffraction (XRD), X-ray fluorescent spectrometry (XRFS), transmission electron microscopy (TEM) and scanning electron microscopy (SEM). Surface characteristics of materials were measured by BET-method. The morphology and dispersity of metal nanoparticles were studied depending on the metals ratio in the composite.

Electroconductive Composites from Polystyrene Block Copolymers and Cu–Alumina Filler

PubMed Central

Nadeem, QuratulAin; Fatima, Tasneem; Prinsen, Pepijn; ur Rehman, Aziz; Gill, Rohama; Mahmood, Rashid; Luque, Rafael

2016-01-01

Technological advancements and development of new materials may lead to the manufacture of sustainable energy-conducting devices used in the energy sector. This research attempts to fabricate novel electroconductive and mechanically stable nanocomposites via an electroless deposition (ELD) technique using electrically insulating materials. Metallic Cu is coated onto Al2O3 by ELD, and the prepared filler is then integrated (2–14 wt %) into a matrix of polystyrene-block-poly(ethylene-ran-butylene)-block-polystyrene-graft-maleic anhydride (PS-b-(PE-r-B)-b-PS-g-MA). Considerable variations in composite phases with filler inclusion exist. The Cu crystallite growth onto Al2O3 was evaluated by X-ray diffraction (XRD) analysis and energy dispersive spectrometry (EDS). Scanning electron microscopy (SEM) depicts a uniform Cu coating on Al2O3, while homogeneous filler dispersion is exhibited in the case of composites. The electrical behavior of composites is enhanced drastically (7.7 × 10−5 S/cm) upon incorporation of Cu–Al2O3 into an insulating polymer matrix (4.4 × 10−16 S/cm). Moreover, mechanical (Young’s modulus, tensile strength and % elongation at break) and thermal (thermogravimetric analysis (TGA), derivative thermogravimetry (DTG), and differential scanning calorimetry (DSC)) properties of the nanocomposites also improve substantially. These composites are likely to meet the demands of modern high-strength electroconductive devices. PMID:28774110

Structural, linear and nonlinear optical properties of co-doped ZnO thin films

NASA Astrophysics Data System (ADS)

Shaaban, E. R.; El-Hagary, M.; Moustafa, El Sayed; Hassan, H. Shokry; Ismail, Yasser A. M.; Emam-Ismail, M.; Ali, A. S.

2016-01-01

Different compositions of Co-doped zinc oxide [(Zn(1- x)Co x O) ( x = 0, 0.02, 0.04, 0.06, 0.08 and 0.10)] thin films were evaporated onto highly clean glass substrates by thermal evaporation technique using a modified source. The structural properties investigated by X-ray diffraction revealed hexagonal wurtzite ZnO-type structure. The crystallite size of the films was found to decrease with increasing Co content. The optical characterization of the films has been carried out using spectral transmittance and reflectance obtained in the wavelength range from 300 to 2500 nm. The refractive index has been found to increase with increasing Co content. It was further found that optical energy gap decreases from 3.28 to 3.03 eV with increasing Co content from x = 0 to x = 0.10, respectively. The dispersion of refractive index has been analyzed in terms of Wemple-DiDomenico (WDD) single-oscillator model. The oscillator parameters, the single-oscillator energy ( E o), the dispersion energy ( E d), and the static refractive index ( n 0), were determined. The nonlinear refractive index of the Zn(1- x)Co x O thin films was calculated and revealed well correlation with the linear refractive index and WDD parameters which in turn depend on the density and molar volume of the system.

Effect of autoclave induced low-temperature degradation on the adhesion energy between yttria-stabilized zirconia veneered with porcelain.

PubMed

Li, Kai Chun; Waddell, J Neil; Prior, David J; Ting, Stephanie; Girvan, Liz; van Vuuren, Ludwig Jansen; Swain, Michael V

2013-11-01

To investigate the effect of autoclave induced low-temperature degradation on the adhesion energy between yttria-stabilized zirconia veneered with porcelain. The strain energy release rate using a four-point bending stable fracture test was evaluated for two different porcelains [leucite containing (VM9) and glass (Zirox) porcelain] veneered to zirconia. Prior to veneering the zirconia had been subjected to 0 (control), 1, 5, 10 and 20 autoclave cycles. The specimens were manufactured to a total bi-layer dimension of 30 mm × 8 mm × 3 mm. Subsequent scanning electron microscopy/energy dispersive spectrometry, electron backscatter diffraction and X-ray diffraction analysis were performed to identify the phase transformation and fracture behavior. The strain energy release rate for debonding of the VM9 specimens were significantly higher (p<0.05) compared to the Zirox specimens across all test groups. Increasing autoclave cycles lowered the strain energy release rate significantly (p<0.05) from 18.67 J/m(2) (control) to the lowest of 12.79 J/m(2) (cycle 10) for only the VM9 specimens. SEM analyses showed predominant cohesive fracture within the porcelain for all cycle groups. XRD analysis of the substrate prior to veneering confirmed a tetragonal to monoclinic phase transformation with increasing the number of autoclave cycles between 5 and 20. The monoclinic phase reverted back to tetragonal phase after undergoing conventional porcelain firing cycles. EBSD data showed significant changes of the grain size distribution between the control and autoclaved specimen (cycle 20). Increasing autoclave cycles only significantly decreased the adhesion of the VM9 layered specimens. In addition, a conventional porcelain firing schedule completely reverted the monoclinic phase back to tetragonal. Copyright © 2013 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Grism and immersion grating for space telescope

NASA Astrophysics Data System (ADS)

Ebizuka, Noboru; Oka, Kiko; Yamada, Akiko; Ishikawa, Mami; Kashiwagi, Masako; Kodate, Kashiko; Hirahara, Yasuhiro; Sato, Shuji; Kawabata, Koji S.; Wakaki, Moriaki; Morita, Shin-ya; Simizu, Tomoyuki; Yin, Shaohui; Omori, Hitoshi; Iye, Masanori

2017-11-01

The grism is a versatile dispersion element for an astronomical instrument ranging from ultraviolet to infrared. Major benefit of using a grism in a space application, instead of a reflection grating, is the size reduction of optical system because collimator and following optical elements could locate near by the grism. The surface relief (SR) grism is consisted a transmission grating and a prism, vertex angle of which is adjusted to redirect the diffracted beam straight along the direct vision direction at a specific order and wavelength. The volume phase holographic (VPH) grism consists a thick VPH grating sandwiched between two prisms, as specific order and wavelength is aligned the direct vision direction. The VPH grating inheres ideal diffraction efficiency on a higher dispersion application. On the other hand, the SR grating could achieve high diffraction efficiency on a lower dispersion application. Five grisms among eleven for the Faint Object Camera And Spectrograph (FOCAS) of the 8.2m Subaru Telescope with the resolving power from 250 to 3,000 are SR grisms fabricated by a replication method. Six additional grisms of FOCAS with the resolving power from 3,000 to 7,000 are VPH grisms. We propose "Quasi-Bragg grism" for a high dispersion spectroscopy with wide wavelength range. The germanium immersion grating for instance could reduce 1/64 as the total volume of a spectrograph with a conventional reflection grating since refractive index of germanium is over 4.0 from 1.6 to 20 μm. The prototype immersion gratings for the mid-InfraRed High dispersion Spectrograph (IRHS) are successfully fabricated by a nano-precision machine and grinding cup of cast iron with electrolytic dressing method.

Physicochemical characterization of solid dispersions of carbamazepine formulated by supercritical carbon dioxide and conventional solvent evaporation method.

PubMed

Sethia, Sundeep; Squillante, Emilio

2002-09-01

Solid dispersions of carbamazepine (CBZ) were formulated by supercritical fluid processing (SCP) and conventional solvent evaporation in polyethylene glycol (PEG) 8000 with either Gelucire 44/14 or vitamin E TPGS NF (d-alpha-tocopheryl PEG 1000 succinate). Formulations were evaluated by dissolution, scanning electron microscopy, powder X-ray diffraction, and differential scanning calorimetry, and excipient cytotoxicity in Caco-2 cells by MTS [3-(4,5-dimethylthiazol-2-yl)-5-(3-carboxymethoxyphenyl)-2-(4-sulfophenyl)-2H-tetrazolium, inner salt] assay. CBZ release was enhanced from supercritical fluid-treated CBZ and the CBZ/PEG 8000 (1:5), CBZ/PEG 8000/TPGS or Gelucire 44/14 (1:4:1) solid dispersions. The radically altered morphologies of SCP samples seen by scanning electron microscopy suggested polymorphic change that was confirmed by the X-ray diffraction and differential scanning calorimetry. Disappearance of the characteristic CBZ melting peak indicated that CBZ was dissolved inside the carrier system. Polymorphic change of CBZ during SCP led to faster dissolution. Therefore, SCP provides advantages over solid dispersions prepared by conventional processes. Copyright 2002 Wiley-Liss Inc.

Innovative diffraction gratings for high-resolution resonant inelastic soft x-ray scattering spectroscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Voronov, D.L.; Warwick, T.; Gullikson, E. M.

2016-07-27

High-resolution Resonant Inelastic X-ray Scattering (RIXS) requires diffraction gratings with very exacting characteristics. The gratings should provide both very high dispersion and high efficiency which are conflicting requirements and extremely challenging to satisfy in the soft x-ray region for a traditional grazing incidence geometry. To achieve high dispersion one should increase the groove density of a grating; this however results in a diffraction angle beyond the critical angle range and results in drastic efficiency loss. The problem can be solved by use of multilayer coated blazed gratings (MBG). In this work we have investigated the diffraction characteristics of MBGs viamore » numerical simulations and have developed a procedure for optimization of grating design for a multiplexed high resolution imaging spectrometer for RIXS spectroscopy to be built in sector 6 at the Advanced Light Source (ALS). We found that highest diffraction efficiency can be achieved for gratings optimized for 4{sup th} or 5{sup th} order operation. Fabrication of such gratings is an extremely challenging technological problem. We present a first experimental prototype of these gratings and report its performance. High order and high line density gratings have the potential to be a revolutionary new optical element that should have great impact in the area of soft x-ray RIXS.« less

UV shielding with visible transparency based properties of poly (styrene-co-acrylonitrile)/Ag doped ZnO nanocomposite

NASA Astrophysics Data System (ADS)

Singh, Rajender; Verma, Karan; Singh, Tejbir; Barman, P. B.; Sharma, Dheeraj

2018-02-01

Development of ultraviolet (UV) shielding with visible transparency based thermoplastic polymer nanocomposite (PNs) presents an important requisite in terms of their efficiency and cost. Present study contributed for the same approach by dispersion of Ag doped ZnO nanoparticles upto 10 wt% in poly (styrene-co-acrylonitrile) matrix by insitu emulsion polymerization method. The crystal and chemical structure of PNs has been analyzed by x-ray diffraction (XRD) and fourier infrared spectrometer (FTIR) techniques. The morphological and elemental information of synthesized nanomaterial has been studied by field emission scanning electron microscope (FESEM) and energy dispersive spectroscopy (EDS) technique. The optical properties of PNs has been studied by UV-visible spectroscopy technique. The incorporation of nanoparticles in polymer matrix absorb the complete UV light with visible transparency. The present reported polymer nanocomposite (PNs) have tuned refractive index with UV blocking and visible transparency based properties which can serve as a viable alternative as compared to related conventional materials.

Carbon Nanotubes Embedded in Oriented Polymer Nanofibers by Electrospinning

NASA Astrophysics Data System (ADS)

Cohen, Yachin; Dror, Yael; Khalfin, Rafail L.; Salalha, Wael; Yarin, Alexander L.; Zussman, Eyal

2004-03-01

The electrospinning process was used successfully to fabricate nanofibers of poly(ethylene oxide) [PEO] in which carbon nanotubes, either multi-walled (MWCNT) or single-walled (SWCNT) are embedded. MWCNTs were dispersed in water using SDS or Gum Arabic - a highly branched polyelectrolyte. Aqueous dispersion of SWCNT's was achieved using an alternating copolymer of styrene and maleic anhydride, hydrolyzed with NaOH. The focus of this work is on the development of axial orientations in the multi-component nanofibers. The degree of orientation of polymers, surfactants and nanotubes was studied using X-ray diffraction and transmission electron microscopy. Individual nanotubes were successfully embedded in the polymer nanofibers with good axial alignment. A high degree of alignment of PEO crystals and SDS layers was also found in the electrospun nanofibers containing SWCNT's. Oriented ropes of the nanofibers were fabricated in a converging electric field by a rotating disc with a tapered edge. These results can lead to further usage of the nanofibers with embedded carbon nanotubes in applications such as nano-scale energy storage devices.

Morphological Comparison of U3O8 Ore Concentrates from Canada Key Lake and Namibia Sources

DOE Office of Scientific and Technical Information (OSTI.GOV)

Schwartz, Daniel S.; Tandon, Lav; Martinez, Patrick Thomas

Uranium ore concentrates from two different sources were examined using scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS). The ore powders are referred to as Namibia (id. no. 90036, LIMS id. no. 18775) and Canada Key Lake (id. no. 90019, LIMS id. no. 18774). Earlier work identified the ores as the U₃O₈ phase of uranium oxide using x-ray diffraction. Both sets of powders were in the form of dark brown to black powder fines. However, the Canada Key Lake concentrates contained larger chunks of material on the millimeter scale that were easily visible to the unaided eye. The powdersmore » were mounted for SEM examination by hand dispersing a small amount onto conductive sticky tape. Two types of applicators were used and compared: a fine-tipped spatula and a foam-tipped applicator. The sticky tape was on a standard SEM “tee” mount, which was tapped to remove loose contamination before being inserted into the SEM.« less

Acquisition of a High Resolution Field Emission Scanning Electron Microscope for the Analysis of Returned Samples

NASA Technical Reports Server (NTRS)

Nittler, Larry R.

2003-01-01

This grant furnished funds to purchase a state-of-the-art scanning electron microscope (SEM) to support our analytical facilities for extraterrestrial samples. After evaluating several instruments, we purchased a JEOL 6500F thermal field emission SEM with the following analytical accessories: EDAX energy-dispersive x-ray analysis system with fully automated control of instrument and sample stage; EDAX LEXS wavelength-dispersive x-ray spectrometer for high sensitivity light-element analysis; EDAX/TSL electron backscatter diffraction (EBSD) system with software for phase identification and crystal orientation mapping; Robinson backscatter electron detector; and an in situ micro-manipulator (Kleindiek). The total price was $550,000 (with $150,000 of the purchase supported by Carnegie institution matching funds). The microscope was delivered in October 2002, and most of the analytical accessories were installed by January 2003. With the exception of the wavelength spectrometer (which has been undergoing design changes) everything is working well and the SEM is in routine use in our laboratory.

Large-scale synthesis and microwave absorption enhancement of actinomorphic tubular ZnO/CoFe2O4 nanocomposites.

PubMed

Cao, Jing; Fu, Wuyou; Yang, Haibin; Yu, Qingjiang; Zhang, Yanyan; Liu, Shikai; Sun, Peng; Zhou, Xiaoming; Leng, Yan; Wang, Shuangming; Liu, Bingbing; Zou, Guangtian

2009-04-09

Actinomorphic tubular ZnO/CoFe(2)O(4) nanocomposites were fabricated in large scale via a simple solution method at low temperature. The phase structures, morphologies, particle size, shell thickness, chemical compositions of the composites have been characterized by X-ray diffraction (XRD), field emission scanning electron microscope (FESEM), energy dispersive X-ray spectroscopy (EDS), and transmission electron microscopy (TEM). The as-synthesized nanocomposites were uniformly dispersed into the phenolic resin then the mixture was pasted on metal plate with the area of 200 mm x 200 mm as the microwave absorption test plate. The test of microwave absorption was carried out by the radar-absorbing materials (RAM) reflectivity far field radar cross-section (RCS) method. The range of microwave absorption is from 2 to 18 Hz and the best microwave absorption reach to 28.2 dB at 8.5 Hz. The results indicate that the composites are of excellence with respect to microwave absorption.

A microwave assisted one-pot route synthesis of bimetallic PtPd alloy cubic nanocomposites and their catalytic reduction for 4-nitrophenol

NASA Astrophysics Data System (ADS)

Zhang, Jian; Gan, Wei; Fu, Xucheng; Hao, Hequn

2017-10-01

We herein report a simple, rapid, and eco-friendly chemical route to the one-pot synthesis of bimetallic PtPd alloy cubic nanocomposites under microwave irradiation. During this process, water was employed as an environmentally benign solvent, while dimethylformamide served as a mild reducing agent, and polyvinylpyrrolidone was used as both a dispersant and a stabilizer. The structure, morphology, and composition of the resulting alloy nanocomposites were examined by x-ray diffraction, transmission electron microscopy, and energy dispersive x-ray spectroscopy. A detailed study was then carried out into the catalytic activity of the PtPd nanocomposites with a Pt:Pd molar ratio of 50:50 in the reduction of 4-nitrophenol (4-NP) by sodium borohydride as a model reaction. Compared with pristine Pt and Pd monometallic nanoparticles (PtNPs and PdNPs), the bimetallic PtPd alloy nanocomposites exhibited enhanced catalytic activities and were readily recyclable in the reduction of 4-NP due to synergistic effects.

Microstructure and properties of laser-clad high-temperature wear-resistant alloys

NASA Astrophysics Data System (ADS)

Yang, Yongqiang

1999-02-01

A 2-kW CO 2 laser with a powder feeder was used to produce alloy coatings with high temperature-wear resistance on the surface of steel substrates. To analyze the microstructure and microchemical composition of the laser-clad layers, a scanning electron microscope (SEM) equipped with an energy dispersive X-ray microanalysis system was employed. X-ray diffraction techniques were applied to characterize the phases formed during the cladding process. The results show that the microstructure of the cladding alloy consists mainly of many dispersed particles (W 2C, (W,Ti)C 1- x, WC), a lamellar eutectic carbide M 12C, and an (f.c.c) matrix. Hardness tested at room and high temperature showed that the laser-clad zone has a moderate room temperature hardness and relatively higher elevated temperature hardness. The application of the laser-clad layer to a hot tool was very successful, and its operational life span was prolonged 1 to 4 times.

The mechanical properties measurement of multiwall carbon nanotube reinforced nanocrystalline aluminum matrix composite

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sharma, Manjula, E-mail: manjula.physics@gmail.com; Pal, Hemant; Sharma, Vimal

Nanocrystalline aluminum matrix composite containing carbon nanotubes were fabricated using physical mixing method followed by cold pressing. The microstructure of the composite has been investigated using X-ray diffraction, scanning electron microscopy and energy dispersive spectroscopy techniques. These studies revealed that the carbon nanotubes were homogeneously dispersed throughout the metal matrix. The consolidated samples were pressureless sintered in inert atmosphere to further actuate a strong interface between carbon nanotubes and aluminum matrix. The nanoindentation tests carried out on considered samples showed that with the addition of 0.5 wt% carbon nanotubes, the hardness and elastic modulus of the aluminum matrix increased bymore » 21.2 % and 2 % repectively. The scratch tests revealed a decrease in the friction coefficient of the carbon nanotubes reinforced composite due to the presence of lubricating interfacial layer. The prepared composites were promising entities to be used in the field of sporting goods, construction materials and automobile industries.« less

Bimetal-organic frameworks for functionality optimization: MnFe-MOF-74 as a stable and efficient catalyst for the epoxidation of alkenes with H2O2.

PubMed

Yuan, Kuo; Song, Tianqun; Wang, Dawei; Zou, Ye; Li, Jinfeng; Zhang, Xiaotao; Tang, Zhiyong; Hu, Wenping

2018-01-25

In this work, we synthesized a series of microcrystalline Mn x N 100-x -MOF-74 (N = Fe, Co and Ni) materials by a one-pot reaction. Powder X-ray diffraction (PXRD) patterns of Mn x N 100-x -MOF-74 matched well with those of single-metal MOF-74, and the scanning electron microscopy (SEM) images exhibited homogeneous nanocrystallites aggregated together. The amounts and dispersion of metals were analyzed by using inductively coupled plasma (ICP) and energy-dispersive X-ray spectroscopy (EDS), separately. Mn x N 100-x -MOF-74 could remain crystalline and efficiently catalyze the epoxidation of alkenes in DMF with NaHCO 3 and 30% H 2 O 2 . In particular, Mn 29.39 Fe 70.61 -MOF-74 can achieve almost 100% conversion for styrene with 95.0% selectivity towards styrene oxide and be reused at least five times without loss of activity.

Photonic fractional Fourier transformer with a single dispersive device.

PubMed

Cuadrado-Laborde, C; Carrascosa, A; Díez, A; Cruz, J L; Andres, M V

2013-04-08

In this work we used the temporal analog of spatial Fresnel diffraction to design a temporal fractional Fourier transformer with a single dispersive device, in this way avoiding the use of quadratic phase modulators. We demonstrate that a single dispersive passive device inherently provides the fractional Fourier transform of an incident optical pulse. The relationships linking the fractional Fourier transform order and scaling factor with the dispersion parameters are derived. We first provide some numerical results in order to prove the validity of our proposal, using a fiber Bragg grating as the dispersive device. Next, we experimentally demonstrate the feasibility of this proposal by using a spool of a standard optical fiber as the dispersive device.

Optical diffraction by ordered 2D arrays of silica microspheres

NASA Astrophysics Data System (ADS)

Shcherbakov, A. A.; Shavdina, O.; Tishchenko, A. V.; Veillas, C.; Verrier, I.; Dellea, O.; Jourlin, Y.

2017-03-01

The article presents experimental and theoretical studies of angular dependent diffraction properties of 2D monolayer arrays of silica microspheres. High-quality large area defect-free monolayers of 1 μm diameter silica microspheres were deposited by the Langmuir-Blodgett technique under an accurate optical control. Measured angular dependencies of zeroth and one of the first order diffraction efficiencies produced by deposited samples were simulated by the rigorous Generalized Source Method taking into account particle size dispersion and lattice nonideality.

TS-1 supported highly dispersed sub-5 nm gold nanoparticles toward direct propylene epoxidation using H2 and O2

NASA Astrophysics Data System (ADS)

Li, Naixu; Chen, Yong; Shen, Quanhao; Yang, Bin; Liu, Ming; Wei, Lingfei; Tian, Wei; Zhou, Jiancheng

2018-05-01

We report a simple and efficient method for the preparation of highly dispersed Au nanoparticles (< 5 nm) on TS-1 substrate. The synthesis relies on the use of NaBH4 as a reductant for rapid Au atom generation, as well as PVA as a capping agent confining the particle size and dispersion. The samples were characterized by N2 physisorption, inductively coupled plasma mass spectrometry, power X-ray diffraction, scanning electron microscopy, transmission electron microscopy, energy-dispersive X-ray spectroscopy, X-ray photoelectron spectroscopy, CO pulse chemisorption and thermogravimetric analysis. The size of Au particles can be controlled in the range of 3-5 nm. The supported catalyst shows both good activity and selectivity for propylene oxide (PO) generation from direct propylene epoxidation. An optimal performance with PO formation rate of 102.94 gPO h-1 kg-1cat and selectivity of 84.83% is achieved over 2.0 wt% Au/TS-1 catalyst, which is prepared by controlling PVA/Au3+ mass ratio of 1.5/1 and NaBH4/Au3+ mole ratio of 5/1. After 50 h test at 200 °C, no significant decrement of both catalytic activity and PO selectivity can be observed, indicating the excellent thermally stability of the catalyst. Furthermore, a possible reaction mechanism is described on basis of the previous researches and our experimental results.

Stereospecific growth of densely populated rutile mesoporous TiO2 nanoplate films: a facile low temperature chemical synthesis approach

NASA Astrophysics Data System (ADS)

Lee, Go-Woon; Ambade, Swapnil B.; Cho, Young-Jin; Mane, Rajaram S.; Shashikala, V.; Yadav, Jyotiprakash; Gaikwad, Rajendra S.; Lee, Soo-Hyoung; Jung, Kwang-Deog; Han, Sung-Hwan; Joo, Oh-Shim

2010-03-01

We report for the first time, using a simple and environmentally benign chemical method, the low temperature synthesis of densely populated upright-standing rutile TiO2 nanoplate films onto a glass substrate from a mixture of titanium trichloride, hydrogen peroxide and thiourea in triply distilled water. The rutile TiO2 nanoplate films (the phase is confirmed from x-ray diffraction analysis, selected area electron diffraction, energy-dispersive x-ray analysis, and Raman shift) are 20-35 nm wide and 100-120 nm long. The chemical reaction kinetics for the growth of these upright-standing TiO2 nanoplate films is also interpreted. Films of TiO2 nanoplates are optically transparent in the visible region with a sharp absorption edge close to 350 nm, confirming an indirect band gap energy of 3.12 eV. The Brunauer-Emmet-Teller surface area, Barret-Joyner-Halenda pore volume and pore diameter, obtained from N2 physisorption studies, are 82 m2 g - 1, 0.0964 cm3 g - 1 and 3.5 nm, respectively, confirming the mesoporosity of scratched rutile TiO2 nanoplate powder that would be ideal for the direct fabrication of nanoscaled devices including upcoming dye-sensitized solar cells and gas sensors.

[Integration design and diffraction characteristics analysis of prism-grating-prism].

PubMed

He, Tian-Bo; Bayanheshig; Li, Wen-Hao; Kong, Peng; Tang, Yu-Guo

2014-01-01

Prism-grating-prism (PGP) module is the important dispersing component in the hyper spectral imager. In order to effectively predict the distribution of diffraction efficiency of the whole PGP component and its diffraction characteristics before fabrication, a method of the PGP integration design is proposed. From the point of view of the volume phase holographic grating (VPHG) design, combined with the restrictive correlation between the various parameters of prisms and grating, we compiled the analysis software for calculating the whole PGP's diffraction efficiency. Furthermore, the effects of the structure parameters of prisms and grating on the PGP's diffraction characteristics were researched in detail. In particular we discussed the Bragg wavelength shift behaviour of the grating and a broadband PGP spectral component with high diffraction efficiency was designed for the imaging spectrometers. The result of simulation indicated that the spectral bandwidth of the PGP becomes narrower with the dispersion coefficient of prism 1 material decreasing; Bragg wavelength shift characteristics broaden the bandwidth of VPHG both spectrally and angularly, higher angular selectivity is desirable for selection requirements of the prism 1 material, and it can be easily tuned to achieve spectral bandwidth suitable for imaging PGP spectrograph; the vertex angle of prism 1, the film thickness and relative permittivity modulation of the grating have a significant impact on the distribution of PGP's diffraction efficiency, so precision control is necessary when fabrication. The diffraction efficiency of the whole PGP component designed by this method is no less than 50% in the wavelength range from 400 to 1000 nm, the specific design parameters have been given in this paper that have a certain reference value for PGP fabrication.

Fluorescent light mediated a green synthesis of silver nanoparticles using the protein extract of weaver ant larvae.

PubMed

Khamhaengpol, Arunrat; Siri, Sineenat

2016-10-01

Alternative to crude plant extracts, a crude protein extract derived from animal cells is one of the potential sources of biomolecules for mediating a reduction of silver ions and a formation of silver nanoparticles (AgNPs) under a mild condition, which very few works have been reported. This work demonstrated a use of the protein extract of weaver ant larvae as a bio-facilitator for a simple, green synthesis of AgNPs under fluorescent light at room temperature. The protein extract of weaver ant larvae exhibited the reducing and antioxidant activities, which assisted a formation of AgNPs in the reaction containing only silver nitrate under light exposure. Transmission electron microscopy images revealed the dispersed, spherical AgNPs with an average size of 7.87±2.54nm. The maximum surface plasmon resonance (SPR) band of the synthesized AgNPs was at 435nm. The energy-dispersive X-ray analysis revealed that silver was a major element of the particles. The identity of AgNPs was confirmed by X-ray diffraction pattern, selected area electron diffraction and high resolution transmission electron microscopy analyses, which demonstrated the planes of face centered cubic silver. The synthesized AgNPs showed antibacterial activity against both Escherichia coli and Staphylococcus aureus with the minimum bactericidal concentration (MBC) values equally at 250μg/ml, suggesting their potential application as an effective antibacterial agent. Copyright © 2016 Elsevier B.V. All rights reserved.

Energy hyperspace for stacking interaction in AU/AU dinucleotide step: Dispersion-corrected density functional theory study.

PubMed

Mukherjee, Sanchita; Kailasam, Senthilkumar; Bansal, Manju; Bhattacharyya, Dhananjay

2014-01-01

Double helical structures of DNA and RNA are mostly determined by base pair stacking interactions, which give them the base sequence-directed features, such as small roll values for the purine-pyrimidine steps. Earlier attempts to characterize stacking interactions were mostly restricted to calculations on fiber diffraction geometries or optimized structure using ab initio calculations lacking variation in geometry to comment on rather unusual large roll values observed in AU/AU base pair step in crystal structures of RNA double helices. We have generated stacking energy hyperspace by modeling geometries with variations along the important degrees of freedom, roll, and slide, which were chosen via statistical analysis as maximally sequence dependent. Corresponding energy contours were constructed by several quantum chemical methods including dispersion corrections. This analysis established the most suitable methods for stacked base pair systems despite the limitation imparted by number of atom in a base pair step to employ very high level of theory. All the methods predict negative roll value and near-zero slide to be most favorable for the purine-pyrimidine steps, in agreement with Calladine's steric clash based rule. Successive base pairs in RNA are always linked by sugar-phosphate backbone with C3'-endo sugars and this demands C1'-C1' distance of about 5.4 Å along the chains. Consideration of an energy penalty term for deviation of C1'-C1' distance from the mean value, to the recent DFT-D functionals, specifically ωB97X-D appears to predict reliable energy contour for AU/AU step. Such distance-based penalty improves energy contours for the other purine-pyrimidine sequences also. © 2013 Wiley Periodicals, Inc. Biopolymers 101: 107-120, 2014. Copyright © 2013 Wiley Periodicals, Inc.

Scanning electron microscopy, x-ray diffraction, and electron microprobe analysis of calcific deposits on intrauterine contraceptive devices

DOE Office of Scientific and Technical Information (OSTI.GOV)

Khan, S.R.; Wilkinson, E.J.

Deposits found on intrauterine contraceptive devices (IUDs) were studied by scanning electron microscopy, x-ray diffraction, and energy dispersive x-ray microanalysis. All seven devices, including five plastic and two copper IUDs, were coated with a crust containing cellular, acellular, and fibrillar material. The cellular material was composed of erythrocytes, leukocytes, cells of epithelial origin, sperm, and bacteria. Some of the bacteria were filamentous, with acute-angle branching. The fibrillar material appeared to be fibrin. Most of the acellular material was amorphous; calcite was identified by x-ray diffraction, and x-ray microanalysis showed only calcium. Some of the acellular material, particularly that on themore » IUD side of the crust, was organized in spherulitic crystals and was identified as calcium phosphate by x-ray microanalysis. The crust was joined to the IUD surface by a layer of fibrillar and amorphous material. It is suggested that the initial event in the formation of calcific deposits on IUD surfaces is the deposition of an amorphous and fibrillar layer. Various types of cells present in the endometrial environment adhere to this layer and then calcify. Thus, the deposition of calcific material on the IUDs is a calcification phenomenon, not unlike the formation of plaque on teeth.« less

Holographic telescope

NASA Astrophysics Data System (ADS)

Odhner, Jefferson E.

2016-07-01

Holographic optical elements (HOEs) work on the principal of diffraction and can in some cases replace conventional optical elements that work on the principal of refraction. An HOE can be thinner, lighter, can have more functionality, and can be lower cost than conventional optics. An HOE can serve as a beam splitter, spectral filter, mirror, and lens all at the same time. For a single wavelength system, an HOE can be an ideal solution but they have not been widely accepted for multispectral systems because they suffer from severe chromatic aberration. A refractive optical system also suffers from chromatic aberration but it is generally not as severe. To color correct a conventional refractive optical system, a flint glass and a crown glass are placed together such that the color dispersion of the flint and the crown cancel each other out making an achromatic lens (achromat) and the wavelengths all focus to the same point. The color dispersion of refractive lenses and holographic lenses are opposite from each other. In a diffractive optical system, long wavelengths focus closer (remember for HOEs: RBM "red bends more") than nominal focus while shorter wavelengths focus further out. In a refractive optical system, it is just the opposite. For this reason, diffractives can be incorporated into a refractive system to do the color correction and often cut down on the number of optical elements used [1.]. Color correction can also be achieved with an all-diffractive system by combining a holographic optical element with its conjugate. In this way the color dispersion of the first holographic optical element can be cancelled by the color dispersion of the second holographic optic. It is this technique that will be exploited in this paper to design a telescope made entirely of holographic optical elements. This telescope could be more portable (for field operations) the same technique could be used to make optics light enough for incorporation into a UAV.

Evolution processes of the corrosion behavior and structural characteristics of plasma electrolytic oxidation coatings on AZ31 magnesium alloy

NASA Astrophysics Data System (ADS)

Chen, Dong; Wang, Ruiqiang; Huang, Zhiquan; Wu, Yekang; Zhang, Yi; Wu, Guorui; Li, Dalong; Guo, Changhong; Jiang, Guirong; Yu, Shengxue; Shen, Dejiu; Nash, Philip

2018-03-01

Evolution processes of the corrosion behavior and structural characteristics of the plasma electrolytic oxidation (PEO) coated AZ31 magnesium alloy were investigated by using scanning electron microscope (SEM) equipped with energy dispersive X-ray spectroscopy (EDS), X-ray diffraction (XRD), potentio-dynamic polarization curves and electrochemical impedance spectroscopy (EIS) measurements. Detached coating samples were fabricated by an electrochemical method and more details of the internal micro-structure of coatings were clearly observed on the fractured cross-section morphologies of the samples compared to general polished cross-section morphologies. Evolution mechanisms of the coating corrosion behavior in relation to the evolution of micro-structural characteristics were discussed in detail.

SnS thin films deposited by chemical bath deposition, dip coating and SILAR techniques

NASA Astrophysics Data System (ADS)

Chaki, Sunil H.; Chaudhary, Mahesh D.; Deshpande, M. P.

2016-05-01

The SnS thin films were synthesized by chemical bath deposition (CBD), dip coating and successive ionic layer adsorption and reaction (SILAR) techniques. In them, the CBD thin films were deposited at two temperatures: ambient and 70 °C. The energy dispersive analysis of X-rays (EDAX), X-ray diffraction (XRD), Raman spectroscopy, scanning electron microscopy (SEM) and optical spectroscopy techniques were used to characterize the thin films. The electrical transport properties studies on the as-deposited thin films were done by measuring the I-V characteristics, DC electrical resistivity variation with temperature and the room temperature Hall effect. The obtained results are deliberated in this paper.

Spectral characterization and white light generation by yttrium silicate nanopowders undoped and doped with Ytterbium(III) at different concentrations when excited by a laser diode at 975 nm

NASA Astrophysics Data System (ADS)

Cinkaya, Hatun; Eryurek, Gonul; Bilir, Gokhan; Collins, John; Di Bartolo, Baldassare

2017-01-01

We have studied nanophosphors of yttrium silicate (YSO) undoped and doped with different concentration of ytterbium (Yb3+) synthesized by using the sol-gel method. Structural and luminescence properties of the nanophosphors were studied experimentally by using different analytical techniques. For the structural analysis, we performed X-ray diffraction (XRD), Transmission Electron Microscopy (TEM) and Energy Dispersive X-ray Spectrometry (EDS) measurements. Upconversion (UC) and the white light (WL) emission properties were investigated by using the near infrared cw laser excitation of 975 nm. The spectral properties have been found to depend on several physical parameters.

Zeta-potential and particle size studies of silver sulphide nanoparticles

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sharma, Vikash, E-mail: vikash@csr.res.in; Tarachand,; Ganesan, V.

Silver sulfide (Ag{sub 2}S) nanoparticles (NPs) were prepared successfully for the first time using diethylene glycol (DEG) as a surfactant. X-ray diffraction (XRD) data revealed single phase nature of the compound and energy-dispersive X-ray (EDX) confirmed its nominal composition. Their sizes were 43 nm from XRD, 50 nm from atomic force microscopy (AFM) and 19 nm & 213 nm from dynamic light scattering (DLS); their differences have been discussed. Autotitration study of zeta potential of these NPs in deionized water by DLS at different pH values confirmed an isoelectric point at pH = 5.14 and their very unstable nature in deionized water.

Magnesium-Aluminum-Zirconium Oxide Amorphous Ternary Composite: A Dense and Stable Optical Coating

NASA Technical Reports Server (NTRS)

Sahoo, N. K.; Shapiro, A. P.

1998-01-01

In the present work, the process parameter dependent optical and structural properties of MgO-Al(2)O(3)-ZrO(2) ternary mixed-composite material have been investigated. Optical properties were derived from spectrophotometric measurements. The surface morphology, grain size distributions, crystallographic phases and process dependent material composition of films have been investigated through the use of Atomic Force Microscopy (AFM), X-ray diffraction analysis and Energy Dispersive X- ray (EDX) analysis. EDX analysis made evident the correlation between the optical constants and the process dependent compositions in the films. It is possible to achieve environmentally stable amorphous films with high packing density under certain optimized process conditions.

Crystallized alkali-silica gel in concrete from the late 1890s

DOE Office of Scientific and Technical Information (OSTI.GOV)

Peterson, Karl; Gress, David; Van Dam, Tom

The Elon Farnsworth Battery, a concrete structure completed in 1898, is in an advanced state of disrepair. To investigate the potential for rehabilitation, cores were extracted from the battery. Petrographic examination revealed abundant deposits of alkali silica reaction products in cracks associated with the quartz rich metasedimentary coarse aggregate. The products of the alkali silica reaction are variable in composition and morphology, including both amorphous and crystalline phases. The crystalline alkali silica reaction products are characterized by quantitative X-ray energy dispersive spectrometry (EDX) and X-ray diffraction (XRD). The broad extent of the reactivity is likely due to elevated alkali levelsmore » in the cements used.« less

Repulsive Interaction of Sulfide Layers on Compressor Impeller Blades Remanufactured Through Plasma Spray Welding

NASA Astrophysics Data System (ADS)

Chang, Y.; Zhou, D.; Wang, Y. L.; Huang, H. H.

2016-12-01

This study investigated the repulsive interaction of sulfide layers on compressor impeller blades remanufactured through plasma spray welding (PSW). Sulfide layers on the blades made of FV(520)B steel were prepared through multifarious corrosion experiments, and PSW was utilized to remanufacture blade specimens. The specimens were evaluated through optical microscopy, scanning electron microscopy, energy-dispersive spectroscopy, 3D surface topography, x-ray diffraction, ImageJ software analysis, Vicker's micro-hardness test and tensile tests. Results showed a large number of sulfide inclusions in the fusion zone generated by sulfide layers embodied into the molten pool during PSW. These sulfide inclusions seriously degraded the mechanical performance of the blades remanufactured through PSW.

Structural phase analysis and photoluminescence properties of Mg-doped TiO2 nanoparticles

NASA Astrophysics Data System (ADS)

Ali, T.; Ashraf, M. Anas; Ali, S. Asad; Ahmed, Ateeq; Tripathi, P.

2018-05-01

In this paper, we report the synthesis, characterization and photoluminescence properties of Mg-doped TiO2 nanoparticles (NPs). The samples were synthesized by sol-gel method and characterized using the standard analytical techniques such as X-ray diffraction (XRD), Transmission electron microscope (TEM), Energy dispersive X-ray spectroscopy (EDX), UV-visible and photoluminescence spectroscopy. The powder XRD spectra revealed that the synthesized samples are pure and crystalline in nature and showing tetragonal anatase phase of TiO2 NPs. UV-visible spectrum illustrates that an absorption edge shifts toward the visible region. This study may provide a new insight for making the nanomaterials which can be used in photocatalytic applications.

Ricinus communis-based biopolymer and epidermal growth factor regulations on bone defect repair: A rat tibia model

NASA Astrophysics Data System (ADS)

Mendoza-Barrera, C.; Meléndez-Lira, M.; Altuzar, V.; Tomás, S. A.

2003-01-01

We report the effect of the addition of an epidermal growth factor to a Ricinus communis-based biopolymer in the healing of a rat tibia model. Bone repair and osteointegration after a period of three weeks were evaluated employing photoacoustic spectroscopy and x-ray diffraction. A parallel study was performed at 1, 2, 3, 4, 5, 6, 7, and 8 weeks with energy dispersive x-ray spectroscopy. We conclude that the use of an epidermal growth factor (group EGF) in vivo accelerates the process of bony repair in comparison with other groups, and that the employment of the Ricinus communis-based biopolymer as a bone substitute decreases bone production.

Green synthesis of gold nanoparticles using aspartame and their catalytic activity for p-nitrophenol reduction

NASA Astrophysics Data System (ADS)

Wu, Shufen; Yan, Songjing; Qi, Wei; Huang, Renliang; Cui, Jing; Su, Rongxin; He, Zhimin

2015-05-01

We demonstrated a facile and environmental-friendly approach to form gold nanoparticles through the reduction of HAuCl4 by aspartame. The single-crystalline structure was illustrated by transmission electron microscopy (TEM) and X-ray diffraction (XRD). The energy-dispersive X-ray spectroscopy (EDS) and Fourier transform infrared (FTIR) results indicated that aspartame played a pivotal role in the reduction and stabilization of the gold crystals. The crystals were stabilized through the successive hydrogen-bonding network constructed between the water and aspartame molecules. Additionally, gold nanoparticles synthesized through aspartame were shown to have good catalytic activity for the reduction of p-nitrophenol to p-aminophenol in the presence of NaBH4.

National Synchrotron Light Source annual report 1991

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hulbert, S.L.; Lazarz, N.M.

1992-04-01

This report discusses the following research conducted at NSLS: atomic and molecular science; energy dispersive diffraction; lithography, microscopy and tomography; nuclear physics; UV photoemission and surface science; x-ray absorption spectroscopy; x-ray scattering and crystallography; x-ray topography; workshop on surface structure; workshop on electronic and chemical phenomena at surfaces; workshop on imaging; UV FEL machine reviews; VUV machine operations; VUV beamline operations; VUV storage ring parameters; x-ray machine operations; x-ray beamline operations; x-ray storage ring parameters; superconducting x-ray lithography source; SXLS storage ring parameters; the accelerator test facility; proposed UV-FEL user facility at the NSLS; global orbit feedback systems; and NSLSmore » computer system.« less

Synthesis and characterization of rare-earth-doped calcium tungstate nanocrystals

NASA Astrophysics Data System (ADS)

Suneeta, P.; Rajesh, Ch.; Ramana, M. V.

2018-02-01

In this paper, we report synthesis and characterization of rare-earth-ion-doped calcium tungstate (CaWO4) nanocrystals (NCs). Rare-earth ions, such as gadolinium (Gd), neodymium (Nd), praseodymium (Pr), samarium (Sm) and holmium (Ho), were successfully doped in the CaWO4 NCs by changing the synthesis conditions. The adopted synthesis route was found to be fast and eco-friendly. Structural characterizations, such as X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR) and compositional analysis, were performed using energy dispersive analysis of X-rays (EDAX) on as-synthesized NCs. The results indicate the size of the NCs ranging between 47 to 68nm and incorporation of rare-earth ions in CaWO4 NCs.

Study the Synthesis, Characterization and Immersion of Dense and Porous Bovine Hydroxyapatite Structures in Hank's Balanced Salt Solution

NASA Astrophysics Data System (ADS)

Eslami, N.; Mahmoodian, R.; Hamdi, M.; Khatir, Nadia Mahmoudi; Herliansyah, M. K.; Rafieerad, Ali Reza

2017-04-01

The bone-bonding potential of biomaterials is evaluated in vitro through examining the surface apatite formation in Hank's media to enhance biocompatibility, which is also applicable to facilitate in vivo osseointegration of implantable devices. Hence, bovine hydroxyapatite (BHA) bioceramic structures have been used in various biomedical applications such as orthopedic implants. In this article, the microstructure, in vitro bioactivity, and nanomechanical properties of the synthesized dense and porous BHA are investigated via scanning electron microscopy, x-ray diffraction, energy-dispersive x-ray spectroscopy, Fourier transform infrared spectroscopy, and nanoindentation analysis. From the obtained results, porous BHA mostly possesses adequate requirements for substitution as implants in the human body.

ZnO:Gd nanocrystals for fluorescent applications

DOE Office of Scientific and Technical Information (OSTI.GOV)

Divya, N. K., E-mail: divyank90@gmail.com; Pradyumnan, P. P.

2016-05-23

Gadolinium doped ZnO crystals within the solubility limit of gadolinium in ZnO matrix were prepared by solid state reaction technique. The method is relatively less expense and enables the production in large scale. The samples were characterised by X-ray diffraction (XRD), energy dispersive X-ray spectroscopy (EDS), scanning electron microscopy (SEM), UV/Vis diffuse reflectance spectroscopy and photoluminescence techniques. Fluorescent property studies of gadolinium doped ZnO at room temperature show enhanced visible light emission due to the defects and oxygen vacancies produced via doping. This work reports the impact of gadolinium doping in the structural, optical and luminescent properties of ZnO inmore » detail.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Riley, Brian J.; Kroll, Jared O.; Peterson, Jacob A.

This paper provides an overview of research evaluating the use of tellurite glass as a waste form for salt wastes from electrochemical processing. The capacities to immobilize different salts were evaluated including: a LiCl-Li2O oxide reduction salt (for oxide fuel) containing fission products, a LiCl-KCl eutectic salt (for metallic fuel) containing fission products, and SrCl2. Physical and chemical properties of the glasses were characterized by using X-ray diffraction, bulk density measurements, chemical durability tests, scanning electron microscopy, and energy dispersive X-ray emission spectroscopy. These glasses were found to accommodate high concentrations of halide salts and have high densities. However, improvementsmore » are needed to meet chemical durability requirements.« less

High-entropy alloys in hexagonal close-packed structure

DOE PAGES

Gao, Michael C.; Zhang, B.; Guo, S. M.; ...

2015-08-28

The microstructures and properties of high-entropy alloys (HEAs) based on the face-centered cubic and body-centered cubic structures have been studied extensively in the literature, but reports on HEAs in the hexagonal close-packed (HCP) structure are very limited. Using an efficient strategy in combining phase diagram inspection, CALPHAD modeling, and ab initio molecular dynamics simulations, a variety of new compositions are suggested that may hold great potentials in forming single-phase HCP HEAs that comprise rare earth elements and transition metals, respectively. Lastly, experimental verification was carried out on CoFeReRu and CoReRuV using X-ray diffraction, scanning electron microscopy, and energy dispersion spectroscopy.

Determining and Controlling the Magnesium Composition in CdTe/CdMgTe Heterostructures

DOE PAGES

LeBlanc, E. G.; Edirisooriya, M.; Ogedengbe, O. S.; ...

2017-06-05

The relationships between Mg composition, band gap, and lattice characteristics are investigated for Cd 1-xMg xTe barrier layers using a combination of cathodoluminescence, energy dispersive x-ray spectroscopy, variable angle spectral ellipsometry, and atom probe tomography. The use of a simplified, yet accurate, variable angle spectral ellipsometry analysis is shown to be appropriate for fast determination of composition in thin Cd 1-xMg xTe layers. The validity of using high-resolution x-ray diffraction for CdTe/Cd 1-xMg xTe double heterostructures is discussed. Furthermore, the stability of CdTe/Cd 1-xMg xTe heterostructures are investigated with respect to thermal processing.

Determining and Controlling the Magnesium Composition in CdTe/CdMgTe Heterostructures

DOE Office of Scientific and Technical Information (OSTI.GOV)

LeBlanc, E. G.; Edirisooriya, M.; Ogedengbe, O. S.

The relationships between Mg composition, band gap, and lattice characteristics are investigated for Cd 1-xMg xTe barrier layers using a combination of cathodoluminescence, energy dispersive x-ray spectroscopy, variable angle spectral ellipsometry, and atom probe tomography. The use of a simplified, yet accurate, variable angle spectral ellipsometry analysis is shown to be appropriate for fast determination of composition in thin Cd 1-xMg xTe layers. The validity of using high-resolution x-ray diffraction for CdTe/Cd 1-xMg xTe double heterostructures is discussed. Furthermore, the stability of CdTe/Cd 1-xMg xTe heterostructures are investigated with respect to thermal processing.

A Fiber-Optic System Generating Pulses of High Spectral Density

NASA Astrophysics Data System (ADS)

Abramov, A. S.; Zolotovskii, I. O.; Korobko, D. A.; Fotiadi, A. A.

2018-03-01

A cascade fiber-optic system that generates pulses of high spectral density by using the effect of nonlinear spectral compression is proposed. It is demonstrated that the shape of the pulse envelope substantially influences the degree of compression of its spectrum. In so doing, maximum compression is achieved for parabolic pulses. The cascade system includes an optical fiber exhibiting normal dispersion that decreases along the fiber length, thereby ensuring that the pulse envelope evolves toward a parabolic shape, along with diffraction gratings and a fiber spectral compressor. Based on computer simulation, we determined parameters of cascade elements leading to maximum spectral density of radiation originating from a subpicosecond laser pulse of medium energy.

Pseudomonas aeruginosa KUCD1, a possible candidate for cadmium bioremediation

PubMed Central

Sinha, Sangram; Mukherjee, Samir Kumar

2009-01-01

A cadmium (8 mM) resistant Pseudomonas aeruginosa strain KUCd1 exhibiting high Cd accumulation under in vitro aerobic condition has been reported. The isolate showed a significant ability to remove more than 75% and 89% of the soluble cadmium during the active growth phase from the growth medium and from Cd-amended industrial wastewater under growth supportive condition. Transmission electron microscopy (TEM) and energy dispersive X-ray spectroscopy (EDXS) suggest the presence of Cd in the cells from mid stationary phase. The cell fractionation study revealed membrane and periplasm to be the major accumulating site in this strain. The chemical nature of the accumulated Cd was studied by X-ray powder diffraction analysis. PMID:24031411

Synthesis of galium nitride thin films using sol-gel dip coating method

NASA Astrophysics Data System (ADS)

Hamid, Maizatul Akmam Ab; Ng, Sha Shiong

2017-12-01

In this research, gallium nitride (GaN) thin film were grown on silicon (Si) substrate by a low-cost sol-gel dip coating deposition method. The GaN precursor solution was prepared using gallium (III) nitrate hydrate powder, ethanol and diethanolamine as a starting material, solvent and surfactant respectively. The structural, morphological and optical characteristics of the deposited GaN thin film were investigated. Field-emission scanning electron microscopy observations showed that crack free and dense grains GaN thin films were formed. Energy dispersive X-ray analysis confirmed that the oxygen content in the deposited films was low. X-ray diffraction results revealed that deposited GaN thin films have hexagonal wurtzite structure.

Green synthesis and characterization of size tunable silica-capped gold core-shell nanoparticles

NASA Astrophysics Data System (ADS)

Wangoo, Nishima; Shekhawat, Gajendra; Wu, Jin-Song; Bhasin, Aman K. K.; Suri, C. R.; Bhasin, K. K.; Dravid, Vinayak

2012-08-01

Silica-coated gold nanoparticles (Au@SiO2) with controlled silica-shell thickness were prepared by a modified Stober's method using 10-nm gold nanoparticles (AuNPs) as seeds. The AuNPs were silica-coated with a sol-gel reaction using tetraethylorthosilicate (TEOS) as a silica source and ammonia as a catalyst. An increase in TEOS concentration resulted in an increase in shell thickness. The NPs were characterized by transmission electron microscopy, selected area electron diffraction, energy-dispersive X-ray spectroscopy, scanning near-field ultrasound holography and scanning transmission electron microscopy. The method required no surface modification and the synthesized core shell nanoparticles can be used for various types of biological applications.

Adsorption and oxidation of SO₂in a fixed-bed reactor using activated carbon produced from oxytetracycline bacterial residue and impregnated with copper.

PubMed

Zhou, Baohua; Yu, Lei; Song, Hanning; Li, Yaqi; Zhang, Peng; Guo, Bin; Duan, Erhong

2015-02-01

The SO₂removal ability (including adsorption and oxidation ability) of activated carbon produced from oxytetracycline bacterial residue and impregnated with copper was investigated. The activated carbon produced from oxytetracycline bacterial residue and modified with copper was characterized by x-ray diffraction, scanning electron microscopy, and energy-dispersive spectroscopy. The effects of the catalysts, SO₂concentration, weight hourly space velocity, and temperature on the SO₂adsorption and oxidation activity were evaluated. Activated carbon produced from oxytetracycline bacterial residue and used as catalyst supports for copper oxide catalysts provided high catalytic activity for the adsorbing and oxidizing of SO₂from flue gases.

Airborne asbestos in Colorado public schools.

PubMed

Chadwick, D A; Buchan, R M; Beaulieu, H J

1985-02-01

Levels of airborne asbestos for six Colorado public school facilities with sprayed-on asbestos materials were documented using three analytical techniques. Phase contrast microscopy showed levels up to the thousandths of a fiber per cubic centimeter (f/cc), scanning electron microscopy (SEM) up to the hundredths of a f/cc, and transmission electron microscopy coupled to selected area electron diffraction and energy dispersive X-ray analysis (TEM-SAED-EDXA) up to the tenths of an asbestos f/cc. Phase contrast microscopy was found to be an inadequate analytical technique for documenting the levels of airborne asbestos fibers in the schools: only large fibers which were not embedded in the filter were counted, and asbestos fibers were not distinguished from nonasbestos.

Effect of pressure on the atomic volume of Ga and Tl up to 68 GPa

NASA Astrophysics Data System (ADS)

Schulte, Olaf; Holzapfel, Wilfried B.

1997-04-01

The elemental metals Ga and Tl are studied under pressure in a diamond anvil cell by energy dispersive x-ray diffraction. While Tl remains in the high-pressure cF4 structure up to the highest pressures achieved, several phase transitions are observed in Ga. Different equation-of-state (EOS) forms are fitted to the experimental data. A detailed analysis of the data shows that a simple first-order EOS form can describe the isothermal pressure-volume behavior of all the phases for Ga as well as for Tl. Furthermore, a comparison of the structural behavior under pressure is made for all the group-IIIA elements of the Periodic Table.

Synthesis of trevorite to capture Tc

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tsui, Colin

2011-09-02

Spinel containing technetium can be used to prevent Tc volatilization during vitrification of radioactive waste. Spinel dissolves in glass at elevated temperatures. This study focuses on the synthesis of spinel and the retention of rhenium, a nonradioactive surrogate for Tc in the crystals. To produce trevorite, a nickel-iron spinel (NiFe2O4), Fe and Ni nitrates were mixed with alkali nitrates along with Al(OH)3 and heated to 500 to 800°C. The trevorite content in samples (up to 40 mass%) was measured with x-ray diffraction. Viable samples were rerun with KReO4. Scanning electron microscopy-energy dispersive spectroscopy detected that Re became partly immobilized inmore » spinel-forming crystals.« less

Synthesis and Characterization of YVO4-Based Phosphor Doped with Eu3+ Ions for Display Devices

NASA Astrophysics Data System (ADS)

Thakur, Shashi; Gathania, Arvind K.

2015-10-01

YVO4:Eu nanophosphor has been synthesized by the sol-gel method. Samples were characterized by x-ray diffraction (XRD), energy-dispersive x-ray spectroscopy, Fourier-transform infrared spectroscopy, ultraviolet-visible (UV-Vis) spectroscopy, photoluminescence, and Raman spectroscopy. The XRD profile confirms the tetragonal phase of the Eu3+-doped YVO4 nanophosphor. The efficiency of the prepared phosphor was analyzed by means of its emission spectral profile. We also observed rich red emission from the prepared phosphor on excitation by an ultraviolet source. The calculated Commission International de l'Éclairage coordinates reveal excellent color purity efficiency. Such luminescent powder is useful as red phosphor in display device applications.

The structure of N2 adsorbed on the rumpled NaCl(100) surface—A combined LEED and DFT-D study

NASA Astrophysics Data System (ADS)

Vogt, Jochen

2012-11-01

The structure of N2 physisorbed on the NaCl(100) single crystal surface is investigated by means of quantitative low-energy electron diffraction (LEED) in combination with dispersion corrected density functional theory (DFT-D). In the temperature range between 20 K and 45 K, a p(1 × 1) structure is observed in the LEED experiment. According to the structure analysis based on the measured diffraction spot intensity profiles, the N2 molecules are adsorbed over the topmost Na+ ions. The experimental distance of the lower nitrogen to the Na+ ion underneath is (2.55 ± 0.07) Å; the corresponding DFT-D value is 2.65 Å. The axes of the molecules are tilted (26 ± 3)° with respect to the surface normal, while in the zero Kelvin optimum structure from DFT-D, the molecules have a perpendicular orientation. The experimental monolayer heat of adsorption, deduced from a Fowler-Guggenheim kinetic model of adsorption is -(13.6 ± 1.6) kJ mol-1, including a lateral molecule-molecule interaction energy of -(2.0 ± 0.4) kJ mol-1. The zero Kelvin adsorption energy from DFT-D, including zero point energy correction, is -15.6 kJ mol-1; the molecule-molecule interaction is -2.4 kJ mol-1. While the rumpling of the NaCl(100) surface is unchanged upon adsorption of nitrogen, the best-fit root mean square thermal displacements of the ions in the topmost substrate layer are significantly reduced.

Effect of Electron Beam Irradiation on Structural and Optical Properties of Cu-Doped In2O3 Films Prepared by RF Magnetron Sputtering

NASA Astrophysics Data System (ADS)

Krishnan, R. Reshmi; Sanjeev, Ganesh; Prabhu, Radhakrishna; Pillai, V. P. Mahadevan

2018-02-01

Undoped and Cu-doped In2O3 films were prepared by radiofrequency magnetron sputtering technique. The effects of Cu doping and high-energy electron beam irradiation on the structural and optical properties of as-prepared films were investigated using techniques such as x-ray diffraction, x-ray photoelectron spectroscopy (XPS), lateral scanning electron microscopic image analysis, energy-dispersive x-ray (EDX) spectroscopy, micro-Raman, and ultraviolet-visible (UV-vis) spectroscopy. Moderate doping of Cu in In2O3 enhanced the intensity of (222) peak, indicating alignment of crystalline grains along <111>. Electron beam irradiation promoted orientation of crystalline grains along <111> in undoped and moderately Cu-doped films. EDX spectroscopic and XPS analyses revealed incorporation of Cu2+ ions in the lattice. The transmittance of Cu-doped films decreased with e-beam irradiation. Systematic reduction of the bandgap energy with increase in Cu doping concentration was seen in unirradiated and electron-beam-irradiated films.

Heavy-ion beam induced effects in enriched gadolinium target films prepared by molecular plating

NASA Astrophysics Data System (ADS)

Mayorov, D. A.; Tereshatov, E. E.; Werke, T. A.; Frey, M. M.; Folden, C. M.

2017-09-01

A series of enriched gadolinium (Gd, Z = 64) targets was prepared using the molecular plating process for nuclear physics experiments at the Cyclotron Institute at Texas A&M University. After irradiation with 48Ca and 45Sc projectiles at center-of-target energies of Ecot = 3.8-4.7 MeV/u, the molecular films displayed visible discoloration. The morphology of the films was examined and compared to the intact target surface. The thin films underwent a heavy-ion beam-induced density change as identified by scanning electron microscopy and α-particle energy loss measurements. The films became thinner and more homogenous, with the transformation occurring early on in the irradiation. This transformation is best described as a crystalline-to-amorphous phase transition induced by atomic displacement and destruction of structural order of the original film. The chemical composition of the thin films was surveyed using energy dispersive spectroscopy and X-ray diffraction, with the results confirming the complex chemistry of the molecular films previously noted in other publications.

Sealed-tube synthesis and phase diagram of Li{sub x}TiS{sub 2} (0 ≤ x ≤1)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhang, Ziping; National Laboratory for Superconductivity, Institute of Physics, Chinese Academy of Science, Beijing 100190; Dong, Cheng, E-mail: chengdon@aphy.iphy.ac.cn

2015-01-15

Graphical abstract: We reported a new method to prepare Li{sub x}TiS{sub 2} (0 ≤ x ≤ 1) at 600 °C in sealed tube using Li{sub 2}S aslithium source. A schematic phase diagram of the Li{sub x}TiS{sub 2} system has been constructed based on the DTA and XRD data. - Abstract: We reported a new method to prepare Li{sub x}TiS{sub 2} (0 ≤ x ≤ 1) at 600 °C in sealed tube using Li{sub 2}S as lithium source. The Li{sub x}TiS{sub 2} samples were characterized by powder X-ray diffraction, scanning electron microscopy, energy dispersive X-ray spectroscopy, and differential thermal analysis. Themore » variations of the lattice parameters with lithium content x in Li{sub x}TiS{sub 2} were determined by X-ray powder diffraction analysis for both 1T and 3R phases. The phase transition between low-temperature 1T phase and high-temperature 3R phase was confirmed by the powder X-ray diffraction analysis. Based on the differential thermal analysis and X-ray diffraction results, a schematic phase diagram of the Li{sub x}TiS{sub 2} system has been constructed, providing a guideline to synthesize Li{sub x}TiS{sub 2} in 1T structure or 3R structure.« less

Method for improving x-ray diffraction determinations of residual stress in nickel-base alloys

DOEpatents

Berman, R.M.; Cohen, I.

1988-04-26

A process for improving the technique of measuring residual stress by x-ray diffraction in pieces of nickel-base alloys is discussed. Part of a predetermined area of the surface of a nickel-base alloy is covered with a dispersion. This exposes the covered and uncovered portions of the surface of the alloy to x-rays by way of an x-ray diffractometry apparatus, making x-ray diffraction determinations of the exposed surface, and measuring the residual stress in the alloy based on these determinations. The dispersion is opaque to x-rays and serves a dual purpose, since it masks off unsatisfactory signals such that only a small portion of the surface is measured, and it supplies an internal standard by providing diffractogram peaks comparable to the peaks of the nickel alloy so that the alloy peaks can be very accurately located regardless of any sources of error external to the sample. 2 figs.

X-ray diffraction gratings: Precise control of ultra-low blaze angle via anisotropic wet etching

DOE Office of Scientific and Technical Information (OSTI.GOV)

Voronov, Dmitriy L.; Naulleau, Patrick; Gullikson, Eric M.

2016-07-25

Diffraction gratings are used from micron to nanometer wavelengths as dispersing elements in optical instruments. At shorter wavelengths, crystals can be used as diffracting elements, but due to the 3D nature of the interaction with light are wavelength selective rather than wavelength dispersing. There is an urgent need to extend grating technology into the x-ray domain of wavelengths from 1 to 0.1 nm, but this requires the use of gratings that have a faceted surface in which the facet angles are very small, typically less than 1°. Small facet angles are also required in the extreme ultra-violet and soft x-ray energymore » ranges in free electron laser applications, in order to reduce power density below a critical damage threshold. In this work, we demonstrate a technique based on anisotropic etching of silicon designed to produce very small angle facets with a high degree of perfection.« less

Hierarchical Co(OH)2 nanostructures/glassy carbon electrode derived from Co(BTC) metal-organic frameworks for glucose sensing

NASA Astrophysics Data System (ADS)

He, Juan; Lu, Xingping; Yu, Jie; Wang, Li; Song, Yonghai

2016-07-01

A novel Co(OH)2/glassy carbon electrode (GCE) has been fabricated via metal-organic framework (MOF)-directed method. In the strategy, the Co(BTC, 1,3,5-benzentricarboxylic acid) MOFs/GCE was firstly prepared by alternately immersing GCE in Co2+ and BTC solution based on a layer-by-layer method. And then, the Co(OH)2 with hierarchical flake nanostructure/GCE was constructed by immersing Co(BTC) MOFs/GCE into 0.1 M NaOH solution at room temperature. Such strategy improves the distribution of hierarchical Co(OH)2 nanostructures on electrode surface greatly, enhances the stability of nanomaterials on the electrode surface, and increases the use efficiency of the Co(OH)2 nanostructures. Scanning electron microscopy, energy dispersive X-ray spectroscopy, X-ray powder diffraction, energy dispersive spectroscopy, Fourier transform infrared spectroscopy, and Raman spectra were used to characterize the Co(BTC) MOFs/GCE and Co(OH)2/GCE. Based on the hierarchical Co(OH)2 nanostructures/GCE, a novel and sensitive nonenzymatic glucose sensor was developed. The good performance of the resulted sensor toward the detection of glucose was ascribed to hierarchical flake nanostructures, good mechanical stability, excellent distribution, and large specific surface area of Co(OH)2 nanostructures. The proposed preparation method is simple, efficient, and cheap .

Enhancement of Electrode Stability Using Platinum-Cobalt Nanocrystals on a Novel Composite SiCTiC Support.

PubMed

Millán, María; Zamora, Héctor; Rodrigo, Manuel A; Lobato, Justo

2017-02-22

PtCo alloy catalysts for high temperature PEMFCs (protonic exchange membrane fuel cells) were synthesized on a novel noncarbonaceous support (SiCTiC) using the impregnation method with NaBH 4 as the reducing agent at different synthesis temperatures to evaluate the effect of this variable on their physicochemical and electrochemical properties. The catalysts were characterized by inductively coupled plasma optical emission spectrometry, scanning electron microscopy-energy dispersive X-ray spectroscopy, X-ray diffraction, transmission electron microscope-energy dispersive X-ray,and temperature-programmed reduction. In addition, the electrochemical characterization (i.e., cyclic voltammetry, oxygen reduction reaction, and chronoamperometry) was carried out with a rotating disk electrode. For the cyclic voltammetry investigation, 400 cycles were performed in hot phosphoric acid and a half-cell to evaluate the stability of the synthesized catalysts. The catalyst synthesized on SiCTiC exhibited excellent durability compared to the catalyst synthesized on a Vulcan support. In addition, all synthesized catalysts exhibited better catalytic activity than that of the PtCo/C catalysts. The best results were observed for the catalyst synthesized at 80 °C due to its shorter Pt-Pt nearest-neighbor and higher alloy degree. Finally, a preliminary stability test was conducted in an HT-PEMFC, and promising results in terms of stability and performance were observed.

Structural and optical characterization of 1 µm of ternary alloy ZnCuSe thin films

NASA Astrophysics Data System (ADS)

Shaaban, E. R.; Hassan, H. Shokry; Aly, S. A.; Elshaikh, H. A.; Mahasen, M. M.

2016-08-01

Different compositions of Cu-doped ZnSe in ternary alloy Zn1- x Cu x Se thin films (with x = 0, 0.025, 0.05, 0.075 and 0.10) were evaporated (thickness 1 µm) onto glass substrate using electron beam evaporation method. The X-ray diffraction analysis for both powder and films indicated their polycrystalline nature with zinc blende (cubic) structure. The crystallite size was found to increase, while the lattice microstrain was decreased with increasing Cu dopant. The optical characterization of films was carried out using the transmittance spectra, where the refractive indices have been evaluated in transparent and medium transmittance regions using the envelope method, suggested by Swanepoel. The refractive index has been found to increase with increasing Cu content. The dispersion of refractive index has been analyzed in terms of the Wemple-DiDomenico single-oscillator model. The oscillator parameters, the single-oscillator energy E o, the dispersion energy E d and the static refractive index n 0, were estimated. The optical band gap was determined in strong absorption region of transmittance spectra and was found to increase from 2.702 to 2.821 eV with increasing the Cu content. This increase in the band gap was well explained by the Burstein-Moss effect.

Superparamagnetic behavior in Sn0.95Mg0.05O2 nanoparticles

NASA Astrophysics Data System (ADS)

Ahmed, Ateeq; Siddique, M. Naseem; Ali, Tinku; Tripathi, P.

2018-04-01

We have studied structural, optical and magnetic properties of Sn0.95Mg0.05O2 nanoparticles synthesized by sol-gel process. Single phase tetragonal structure of Mg doped SnO2 nanoparticles (NPs) have been inferred by X-ray diffraction, which involves Rietveld refinement analysis and average crystallite size is found to be 20.4 nm. Energy dispersive X -ray analysis confirmed the presence of Mg into host SnO2 lattice. The energy band gap is found to be wider (Eg = 3.73 eV) compared to the bulk (3.6 eV) which is due to the quantum confinement effect. The observed defects due to oxygen vacancies are studied by the photoluminescence study. The SQUID magnetometer measurements shows superparamagnetic behavior of Mg-doped SnO2 NPs at room temperature and they are single domain NPs. Our results suggest that it is possible to control the superparamagnetic properties through chemical composition.

A facile synthesis of zinc oxide/multiwalled carbon nanotube nanocomposite lithium ion battery anodes by sol-gel method

NASA Astrophysics Data System (ADS)

Köse, Hilal; Karaal, Şeyma; Aydın, Ali Osman; Akbulut, Hatem

2015-11-01

Free standing zinc oxide (ZnO) and multiwalled carbon nanotube (MWCNT) nanocomposite materials are prepared by a sol gel technique giving a new high capacity anode material for lithium ion batteries. Free-standing ZnO/MWCNT nanocomposite anodes with two different chelating agent additives, triethanolamine (TEA) and glycerin (GLY), yield different electrochemical performances. Field emission gun scanning electron microscopy (FEG-SEM), energy dispersive X-ray spectrometer (EDS), high resolution transmission electron microscopy (HRTEM) and X-ray diffraction (XRD) analyses reveal the produced anode electrodes exhibit a unique structure of ZnO coating on the MWCNT surfaces. Li-ion cell assembly using a ZnO/MWCNT/GLY free-standing anode and Li metal cathode possesses the best discharge capacity, remaining as high as 460 mAh g-1 after 100 cycles. This core-shell structured anode can offer increased energy storage and performance over conventional anodes in Li-ion batteries.

Influence of reaction time and synthesis temperature on the physical properties of ZnO nanoparticles synthesized by the hydrothermal method

NASA Astrophysics Data System (ADS)

Wasly, H. S.; El-Sadek, M. S. Abd; Henini, Mohamed

2018-01-01

Influence of synthesis temperature and reaction time on the structural and optical properties of ZnO nanoparticles synthesized by the hydrothermal method was investigated using X-ray diffraction (XRD), high resolution transmission electron microscopy (HR-TEM), energy-dispersive X-ray, Fourier transform infra-red spectroscopy, and UV-visible and fluorescence spectroscopy. The XRD pattern and HR-TEM images confirmed the presence of crystalline hexagonal wurtzite ZnO nanoparticles with average crystallite size in the range 30-40 nm. Their energy gap determined by fluorescence was found to depend on the synthesis temperature and reaction time with values in the range 2.90-3.78 eV. Thermal analysis, thermogravimetric and the differential scanning calorimetry were used to study the thermal reactions and weight loss with heat of the prepared ZnO nanoparticles.

Crystallization Kinetics of Calcium-magnesium Aluminosilicate (CMAS) Glass

NASA Technical Reports Server (NTRS)

Wiesner, Valerie L.; Bansal, Narottam P.

2015-01-01

The crystallization kinetics of a calcium-magnesium aluminosilicate (CMAS) glass with composition relevant for aerospace applications, like air-breathing engines, were evaluated using differential thermal analysis (DTA) in powder and bulk forms. Activation energy and frequency factor values for crystallization of the glass were evaluated. X-ray diffraction (XRD) was used to investigate the onset of crystallization and the phases that developed after heat treating bulk glass at temperatures ranging from 690 to 960 deg for various times. Samples annealed at temperatures below 900 deg remained amorphous, while specimens heat treated at and above 900 deg exhibited crystallinity originating at the surface. The crystalline phases were identified as wollastonite (CaSiO3) and aluminum diopside (Ca(Mg,Al) (Si,Al)2O6). Scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS) were employed to examine the microstructure and chemical compositions of crystalline phases formed after heat treatment.

Electrochemical characterization and electrode kinetics for antimony electrodeposition from its oxychloride solution in the presence of tartaric acid

NASA Astrophysics Data System (ADS)

Majidzade, Vusala Asim; Guliyev, Parvin Heydar; Aliyev, Akif Shikhan; Elrouby, Mahmoud; Tagiyev, Dilgam Babir

2017-05-01

This work is devoted to investigate the process of the electrochemical deposition of antimony from antimony oxychloride solution in the presence of tartaric acid in aqueous media. The kinetics and the mechanism of the electrodeposition process at the electrode surface are studied and proposed by the aid of cyclic, linear sweep voltammetric and chronoamperometric characterization methods. It is found that, the process is affected by the presence of tartaric acid and some factors during the electro-reduction process. The results also show that, the temperature, the potential sweep rate and the concentration of antimony have a great influence on the achievement of the electrodeposition process. Some important parameters are calculated such as, the activation energy of the electrochemical reaction, the diffusion coefficient and the number of saturated nucleation sites. The electrodeposited film is examined using X-ray diffraction, scanning electron microscopy and Energy Dispersive Spectroscopy.

Atomic-Scale Characterization of Oxide Interfaces and Superlattices Using Scanning Transmission Electron Microscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Spurgeon, Steven R.; Chambers, Scott A.

Scanning transmission electron microscopy (STEM) has become one of the fundamental tools to characterize oxide interfaces and superlattices. Atomic-scale structure, chemistry, and composition mapping can now be conducted on a wide variety of materials systems thanks to the development of aberration-correctors and advanced detectors. STEM imaging and diffraction, coupled with electron energy loss (EELS) and energy-dispersive X-ray (EDS) spectroscopies, offer unparalleled, high-resolution analysis of structure-property relationships. In this chapter we highlight investigations into key phenomena, including interfacial conductivity in oxide superlattices, charge screening effects in magnetoelectric heterostructures, the design of high-quality iron oxide interfaces, and the complex physics governing atomic-scalemore » chemical mapping. These studies illustrate how unique insights from STEM characterization can be integrated with other techniques and first-principles calculations to develop better models for the behavior of functional oxides.« less

Cellulose Acetate Modified Titanium Dioxide (TiO2) Nanoparticles Electrospun Composite Membranes: Fabrication and Characterization

NASA Astrophysics Data System (ADS)

Das, Chandan; Gebru, Kibrom Alebel

2017-12-01

Hybrid membranes from Cellulose Acetate (CA) and titanium oxide (TiO2) nanoparticles were fabricated using electrospinning technique. The electrospun hybrid membranes were characterized using field emission scanning electron microscopy, high energy electrons of the energy dispersive X-ray spectroscopy, X-ray diffraction patterns, atomic force microscopy, zeta potential (ζ), and thermo gravimetric analysis. The impact of TiO2 contents on the electrospun membranes matrix was studied in detail. All these characterization results indicated that TiO2 were uniformly distributed within the CA electrospun membrane's matrix. The addition of TiO2 caused formation of largely interconnected fiber networks which in turn have a positive effect on the enhancement of the membrane pore structures. As the amount of TiO2 addition was raised from 0 to 6.5 wt%, the entanglements of the fibers and the spider-net like network among fibers were increased.

Residual strain gradient determination in metal matrix composites by synchrotron X-ray energy dispersive diffraction

NASA Technical Reports Server (NTRS)

Kuntz, Todd A.; Wadley, Haydn N. G.; Black, David R.

1993-01-01

An X-ray technique for the measurement of internal residual strain gradients near the continuous reinforcements of metal matrix composites has been investigated. The technique utilizes high intensity white X-ray radiation from a synchrotron radiation source to obtain energy spectra from small (0.001 cu mm) volumes deep within composite samples. The viability of the technique was tested using a model system with 800 micron Al203 fibers and a commercial purity titanium matrix. Good agreement was observed between the measured residual radial and hoop strain gradients and those estimated from a simple elastic concentric cylinders model. The technique was then used to assess the strains near (SCS-6) silicon carbide fibers in a Ti-14Al-21Nb matrix after consolidation processing. Reasonable agreement between measured and calculated strains was seen provided the probe volume was located 50 microns or more from the fiber/matrix interface.

Probing long-range structural order in SnPc/Ag(111) by umklapp process assisted low-energy angle-resolved photoelectron spectroscopy

NASA Astrophysics Data System (ADS)

Jauernik, Stephan; Hein, Petra; Gurgel, Max; Falke, Julian; Bauer, Michael

2018-03-01

Laser-based angle-resolved photoelectron spectroscopy is performed on tin-phthalocyanine (SnPc) adsorbed on silver Ag(111). Upon adsorption of SnPc, strongly dispersing bands are observed which are identified as secondary Mahan cones formed by surface umklapp processes acting on photoelectrons from the silver substrate as they transit through the ordered adsorbate layer. We show that the photoemission data carry quantitative structural information on the adsorbate layer similar to what can be obtained from a conventional low-energy electron diffraction (LEED) study. More specifically, we compare photoemission data and LEED data probing an incommensurate-to-commensurate structural phase transition of the adsorbate layer. Based on our results we propose that Mahan-cone spectroscopy operated in a pump-probe configuration can be used in the future to probe structural dynamics at surfaces with a temporal resolution in the sub-100-fs regime.

Long-term oxidization and phase transition of InN nanotextures

PubMed Central

2011-01-01

The long-term (6 months) oxidization of hcp-InN (wurtzite, InN-w) nanostructures (crystalline/amorphous) synthesized on Si [100] substrates is analyzed. The densely packed layers of InN-w nanostructures (5-40 nm) are shown to be oxidized by atmospheric oxygen via the formation of an intermediate amorphous In-Ox-Ny (indium oxynitride) phase to a final bi-phase hcp-InN/bcc-In2O3 nanotexture. High-resolution transmission electron microscopy, energy-dispersive X-ray spectroscopy, electron energy loss spectroscopy and selected area electron diffraction are used to identify amorphous In-Ox-Ny oxynitride phase. When the oxidized area exceeds the critical size of 5 nm, the amorphous In-Ox-Ny phase eventually undergoes phase transition via a slow chemical reaction of atomic oxygen with the indium atoms, forming a single bcc In2O3 phase. PMID:21711908

Low Cost CaTiO3 Perovskite Synthesized from Scallop (Anadara granosa) Shell as Antibacterial Ceramic Material

NASA Astrophysics Data System (ADS)

Fatimah, Is; Nur Ilahi, Rico; Pratami, Rismayanti

2018-01-01

Research on perovskite CaTiO3 synthesis from scallop (Anadara granosa) shell and its test as material for antibacterial ceramic application have been conducted. The synthesis was performed by calcium extraction from the scallop shell followed by solid-solid reaction of obtained calcium with TiO2. Physicochemical character of the perovskite wasstudied by measurement of crystallinity using x-ray diffraction (XRD), diffuse-reflectance UV Visible spectrophotometry, scanning electrone microscope-energy dispersive x-ray (SEM-EDX) and Fourier-Transform InfraRed. Considering the future application of the perovskite as antibacterial agent, laboratory test of the peroskite as material in antibacterial ceramic preparation was also conducted. Result of research indicated that perovskite formation was obtained and the material demonstrated photocatalytic activity as identified by band gap energy (Eg) value. The significant activity was also reflected by the antibacterial action of formed ceramic.

Lattice strain measurements on sandstones under load using neutron diffraction

NASA Astrophysics Data System (ADS)

Frischbutter, A.; Neov, D.; Scheffzük, Ch.; Vrána, M.; Walther, K.

2000-11-01

Neutron diffraction methods (both time-of-flight- and angle-dispersive diffraction) are applied to intracrystalline strain measurements on geological samples undergoing uniaxial increasing compressional load. The experiments were carried out on Cretaceous sandstones from the Elbezone (East Germany), consisting of >95% quartz which are bedded but without crystallographic preferred orientation of quartz. From the stress-strain relation the Young's modulus for our quartz sample was determined to be (72.2±2.9) GPa using results of the neutron time-of-flight method. The influence of different kinds of bedding in sandstones (laminated and convolute bedding) could be determined. We observed differences of factor 2 (convolute bedding) and 3 (laminated bedding) for the elastic stiffness, determined with angle dispersive neutron diffraction (crystallographic strain) and with strain gauges (mechanical strain). The data indicate which geological conditions may influence the stress-strain behaviour of geological materials. The influence of bedding on the stress-strain behaviour of a laminated bedded sandstone was indicated by direct residual stress measurements using neutron time-of-flight diffraction. The measurements were carried out six days after unloading the sample. Residual strain was measured for three positions from the centre to the periphery and within two radial directions of the cylinder. We observed that residual strain changes from extension to compression in a different manner for two perpendicular directions of the bedding plane.

Method of determining dispersion dependence of refractive index of nanospheres building opals

NASA Astrophysics Data System (ADS)

Kępińska, Mirosława; Starczewska, Anna; Duka, Piotr

2017-11-01

The method of determining dispersion dependence of refractive index of nanospheres building opals is presented. In this method basing on angular dependences of the spectral positions of Bragg diffraction minima on transmission spectra for opal series of known spheres diameter, the spectrum of effective refractive index for opals and then refractive index for material building opal's spheres is determined. The described procedure is used for determination of neff(λ) for opals and nsph(λ) for material which spheres building investigated opals are made of. The obtained results are compared with literature data of nSiO2(λ) considered in the analysis and interpretation of extremes related to the light diffraction at (hkl) SiO2 opal planes.

Thermal, structural, functional, optical and magnetic studies of pure and Ba doped CdO nanoparticles.

PubMed

Sivakumar, S; Venkatesan, A; Soundhirarajan, P; Khatiwada, Chandra Prasad

2015-12-05

In this research, a chemical precipitation method was used to synthesize undoped and doped cadmium oxide nanoparticles and studied by TG-DTA, XRD, FT-IR, SEM, with EDX and antibacterial activities, respectively. The melting points, thermal stability and the kinetic parameters like entropy (ΔS), enthalpy (ΔH), Gibb's energy (ΔG), activation energy (E), frequency factor (A) were evaluated from TG-DTA measurements. X-ray diffraction analysis (XRD) brought out the information about the synthesized products exist in spherical in shape with cubic structure. The functional groups and band area of the samples were established by Fourier transform infrared (FT-IR) spectroscopy. The direct and indirect band gap energy of pure and doped samples were determined by UV-Vis-DRS. The surface morphological, elemental compositions and particles sizes were evaluated by scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDS). Finally, antibacterial activities indicated the Gram-positive and Gram-negative bacteria are more active in transporter, dehydrogenize and periplasmic enzymatic activities of pure and doped samples. Copyright © 2015 Elsevier B.V. All rights reserved.

Dispersions of TiS2 nanosheets in organic medium

NASA Astrophysics Data System (ADS)

Manjunatha, S.; Kumar, A. Sunil; Machappa, T.

2018-05-01

Here in this article, we report Li-intercalated titanium disulfide (TiS2) two-dimensional (2D) nanosheets, exfoliated in 1-methyl-2-pyrrolidinone (NMP) forming a quite stable dispersions of pale brownish color. As synthesized TiS2 nanosheets were characterized by transmission electron microscopy (TEM). Selected area electron diffraction (SAED) pattern confirmed the hexagonal lattice structure of the exfoliated nanosheets.

Polyimide Nanocomposites Prepared from High-Temperature, Reduced Charge Organoclays

NASA Technical Reports Server (NTRS)

Delozier, D. M.; Orwoll, R. A.; Cahoon, J. F.; Ladislaw, J. S.; Smith, J. G., Jr.; Connell, J. W.

2003-01-01

Montmorillonite clays modified with the dihydrochloride salt of 1,3-bis(3-aminophenoxy)benzene (APB) were used in the preparation of polyimide/organoclay hybrid films. Organoclays with varying surface charge based upon APB were prepared and examined for their dispersion behavior in the polymer matrix. High molecular weight poly(amide acid) solutions were prepared in the presence of the organoclays. Films were cast and subsequently heated to 300C to cause imidization. The resulting nanocomposite films, containing 3 wt% of organoclay, were characterized by transmission electron microscopy and X-ray diffraction. The clay's cation exchange capacity (CEC) played a key role in determining the extent of dispersion in the polyimide matrix. Considerable dispersion was observed in some of the nanocomposite films. The most effective organoclay was found to have a CEC of 0.70 meq/g. Nanocomposite films prepared with 3-8 wt% of this organoclay were characterized by transmission electron microscopy (TEM), X-ray diffraction (XRD), and thin-film tensile testing. High levels of clay dispersion could be achieved even at the higher clay loadings. Results from mechanical testing revealed that while the moduli of the nanocomposites increased with increasing clay loadings, both strength and elongation decreased.

Characterization of photoacoustic sources in tissue using time domain measurements

NASA Astrophysics Data System (ADS)

Viator, John Andrew

Photoacoustic phenomenon in tissue and tissue phantoms is investigated with the particular goal of discrimination of diseased and healthy tissue. Propagation of broadband photoacoustic sources in tissue phantoms is studied with emphasis on attenuation, dispersion, and diffraction. Attenuation of photoacoustic waves induced by a circular laser spot on an absorber/air interface is modeled by the on-axis approximation of the acoustic field of a baffled piston source. Dispersion is studied in a diffraction free situation, where the disk of irradiation was created by a 5 mm laser spot on a 200 cm -1 solution. The genesis of diffraction in an absorbing solution was displayed by showing the merging of a boundary wave with a plane wave from a circular laser spot on an absorbing solution. Depth profiling of absorbing tissue phantoms and stained tissue was shown using a photoacoustic method. Acrylamide gels with layers of different optical absorption and stained elastin biomaterials were irradiated with stress confined laser pulses. The resulting acoustic waves were detected with a lithium niobate wideband acoustic transducer and processed in an algorithm to determine absorption coefficient as a function of depth. Spherical photoacoustic sources were generated in optically clear and turbid tissue phantoms. Propagation time and acoustic pulse duration were used to determine location and size, respectively. The photoacoustic sources were imaged using a multiplicative backprojection scheme. Image sources from acoustic boundaries were detected and dipole sources were detected and imaged. Finally an endoscopic photoacoustic probe was designed, built, and tested for use in determining treatment depth after palliative photodynamic therapy of esophageal cancer. The probe was less than 2.5 mm in diameter and consisted of a side firing 600 mum optical fiber to deliver laser energy and a 890 mum diameter, side viewing piezoelectric detector. The sensitivity of the probe was determined. The probe was also tested on coagulated and non-coagulated liver, ex vivo and on normally perfused and underperfused human skin, in vivo.

Surface molecular imprinting onto fluorescein-coated magnetic nanoparticlesvia reversible addition fragmentation chain transfer polymerization: A facile three-in-one system for recognition and separation of endocrine disrupting chemicals

NASA Astrophysics Data System (ADS)

Li, Ying; Dong, Cunku; Chu, Jia; Qi, Jingyao; Li, Xin

2011-01-01

In this study, we present a general protocol for the making of surface-imprinted magnetic fluorescence beads viareversible addition-fragmentation chain transfer polymerization. The resulting composites were characterized by X-ray diffraction analysis, transmission electron microscopy, scanning electron microscopy, fluorescence spectroscopy, Fourier transform infrared spectroscopy, and energy dispersive spectroscopy. The as-synthesized beads exhibited homogeneous polymer films (thickness of about 5.7 nm), spherical shape, high fluorescence intensity and magnetic property (Magnetization (Ms) = 3.67 emu g-1). The hybrids bind the original template 17β-estradiol with an appreciable selectivity over structurally related compounds. In addition, the resulting hybrids performed without obvious deterioration after five repeated cycles. This study therefore demonstrates the potential of molecularly imprinted polymers for the recognition and separation of endocrine disrupting chemicals.In this study, we present a general protocol for the making of surface-imprinted magnetic fluorescence beads viareversible addition-fragmentation chain transfer polymerization. The resulting composites were characterized by X-ray diffraction analysis, transmission electron microscopy, scanning electron microscopy, fluorescence spectroscopy, Fourier transform infrared spectroscopy, and energy dispersive spectroscopy. The as-synthesized beads exhibited homogeneous polymer films (thickness of about 5.7 nm), spherical shape, high fluorescence intensity and magnetic property (Magnetization (Ms) = 3.67 emu g-1). The hybrids bind the original template 17β-estradiol with an appreciable selectivity over structurally related compounds. In addition, the resulting hybrids performed without obvious deterioration after five repeated cycles. This study therefore demonstrates the potential of molecularly imprinted polymers for the recognition and separation of endocrine disrupting chemicals. Electronic supplementary information (ESI) available: Supplementary figure S1. The hysteresis loop of Fe3O4 (a), Fe3O4@SiO2 (b), and Fe3O4@SiO2-Dye-SiO2 (c). See DOI: 10.1039/c0nr00614a

Structural and electrical characterisation of Li(2)O : TiO(2) : SnO(2) : P(2)O(5) electrolyte glass.

PubMed

Abrahams, Isaac; Hadzifejzovic, Emina; Dygas, Jozef R

2004-10-07

Glasses of general formula 50Li(2)O : xSnO(2) : (10 -x)TiO(2) : 40P(2)O(5)(0.0 < or = x < or = 10) were investigated by differential scanning calorimetry, X-ray diffraction and ac impedance, (31)P solid-state NMR and IR spectroscopies. Three isotropic resonances can be identified in the (31)P NMR spectra, which have been assigned to various phosphate species. Analysis of the ratios of integrated intensities in the (31)P spectra leads to models for the Ti and Sn coordination environments. Both TiO(2) and SnO(2) are found to be predominantly network forming with Ti and Sn proposed to be in five- and four-coordinate environments respectively. Analysis of ac impedance spectra collected at low temperatures reveals two forms of permittivity dispersion, viz: high frequency conductivity dispersion and Cole-Cole type relaxation of permittivity. The activation energy of the relaxation frequency of the permittivity dispersion is equal to that of the dc conductivity, which is consistent with cooperative motion of lithium ions. The results also suggest that the observed increase in conductivity with temperature appears to be mainly due to an increase in mobility rather than increase in carrier concentration.

Synthesis and characterization of supported polysugar-stabilized palladium nanoparticle catalysts for enhanced hydrodechlorination of trichloroethylene

NASA Astrophysics Data System (ADS)

Bacik, Deborah B.; Zhang, Man; Zhao, Dongye; Roberts, Christopher B.; Seehra, Mohinar S.; Singh, Vivek; Shah, Naresh

2012-07-01

Palladium (Pd) nanoparticle catalysts were successfully synthesized within an aqueous phase using sodium carboxymethyl cellulose (CMC) as a capping ligand which offers a green alternative to conventional nanoparticle synthesis techniques. The CMC-stabilized Pd nanoparticles were subsequently dispersed within support materials using the incipient wetness impregnation technique for utilization in heterogeneous catalyst systems. The unsupported and supported (both calcined and uncalcined) Pd nanoparticle catalysts were characterized using transmission electron microscopy, energy dispersive x-ray spectrometry, x-ray diffraction, and Brunauer-Emmett-Teller surface area measurement and their catalytic activity toward the hydrodechlorination of trichloroethylene (TCE) in aqueous media was examined using homogeneous and heterogeneous catalyst systems, respectively. The unsupported Pd nanoparticles showed considerable activity toward the degradation of TCE, as demonstrated by the reaction kinetics. Although the supported Pd nanoparticle catalysts had a lower catalytic activity than the unsupported particles that were homogeneously dispersed in the aqueous solutions, the supported catalysts retained sufficient activity toward the degradation of TCE. In addition, the use of the hydrophilic Al2O3 support material induced a mass transfer resistance to TCE that affected the initial hydrodechlorination rate. This paper demonstrates that supported Pd catalysts can be applied to the heterogeneous catalytic hydrodechlorination of TCE.

Electrophoretic Deposition of Cu-SiO2 Coatings by DC and Pulsed DC for Enhanced Surface-Mechanical Properties

NASA Astrophysics Data System (ADS)

Maharana, H. S.; Lakra, Suprabha; Pal, S.; Basu, A.

2016-01-01

The present study explored the possibilities of improvement in the surface-mechanical properties of electrodeposited Cu-SiO2 composite coating and its underlying mechanism. Composite coatings were developed using SiO2-dispersed acidic copper sulfate electrolyte by direct current and pulse-current electro-codeposition techniques with variation of pulse frequencies at a fixed duty cycle. X-ray diffraction analysis of the coatings revealed information regarding the presence of various phases and crystallographic orientations of the deposited Cu matrix. Scanning electron microscopy and energy dispersive x-ray spectroscopy techniques were used to investigate the surface morphology and chemical composition of the coatings, respectively, and it was observed that SiO2 particles were uniformly distributed in the composite coatings. Surface roughness was found to be reduced with the increasing pulse frequency. The Vickers microhardness and ball-on-plate wear study showed improvement in surface-mechanical properties due to the formation of fine Cu matrix, dispersion strengthening due to homogeneously distributed SiO2 particles, and the preferred orientation of the Cu matrix. Marginal decrease in electrical conductivity with the increasing SiO2 content and pulse frequency was observed from the four-probe electrical conductivity measurement technique.

Quantum diffraction and shielding effects on the low-energy electron-ion bremsstrahlung in two-component semiclassical plasmas

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lee, Myoung-Jae; Jung, Young-Dae, E-mail: ydjung@hanyang.ac.kr; Department of Physics, Applied Physics, and Astronomy, Rensselaer Polytechnic Institute, 110 8th Street, Troy, New York 12180-3590

2015-10-15

The quantum diffraction and shielding effects on the low-energy bremsstrahlung process are investigated in two-component semiclassical plasmas. The impact-parameter analysis with the micropotential taking into account the quantum diffraction and shielding effects is employed to obtain the electron-ion bremsstrahlung radiation cross section as a function of the de Broglie wavelength, density parameter, impact parameter, photon energy, and projectile energy. The result shows that the influence of quantum diffraction and shielding strongly suppresses the bremsstrahlung radiation spectrum in semiclassical plasmas. It is found that the quantum diffraction and shielding effects have broaden the photon emission domain. It is also found thatmore » the photon emission domain is almost independent of the radiation photon energy. In addition, it is found that the influence of quantum diffraction and shielding on the bremsstrahlung spectrum decreases with an increase of the projectile energy. The density effect on the electron-ion bremsstrahlung cross section is also discussed.« less

Structural and Spectral Characterization of Co2+- and Ni2+-DOPED CdO Powder Prepared From Solution at Room Temperature

NASA Astrophysics Data System (ADS)

Reddy, C. V.; Rao, L. V. Krishna; Satish, D. V.; Shim, J.; Ravikumar, R. V. S. S. N.

2015-11-01

The mild and simple solution method was used for the synthesis of Co2+- and Ni2+-doped CdO powders at room temperature. The prepared powders were characterized using powder X-ray diffraction, scanning electron microscopy (SEM) with energy dispersive spectroscopy (EDS), optical absorption, and Fourier transform infrared spectroscopy (FTIR). From the powder X-ray diffraction patterns, it has been observed that the prepared Co2+ and Ni2+ ion-doped CdO powders belong to the cubic phase, and the evaluated average crystalline sizes of the powders are 20 and 14 nm, respectively. The SEM images and the EDS spectra show that the prepared powders are distributed over different sizes in the grain boundaries. Optical absorption studies allow determination of site symmetry of the metal ion with its ligands. The crystal field (Dq) and inter-electronic repulsion (B and C) parameters have been evaluated from the optical absorption spectra. The FTIR spectra show the characteristic fundamental vibrations of the metal oxide and CdO.

Choline-amino acid ionic liquids: past and recent achievements about the structure and properties of these really "green" chemicals.

PubMed

Gontrani, Lorenzo

2018-06-01

The structure of choline-amino acid ionic liquids, atoxic task-specific solvents composed of materials originated from renewable feedstocks, is reviewed in this letter. The varied and strong interactions that these liquids are capable of establishing are largely dependent on their structure and confer them outstanding solvating properties with respect to a large number of different solutes. Among the experimental methods capable of yielding structural insight, the energy-dispersive version of X-Ray diffraction, that uses the Bremsstrahlung radiation of the X-Ray tube, is a technique very well suited to investigate these liquid systems. The diffraction spectra of five choline-amino acid ionic liquids, recently measured, are reported and discussed; in particular, the presence or absence of the medium-range order pre-peak is related to the presence of polar groups within the amino acid side chain that destroys the hydrophobic interactions between aliphatic chains. In the final section, a recent example of choline-amino acid ionic liquids as for ancient paper preservation and two other interesting results are discussed at the end.

Preparation and characterization of hydroxyapatite-coated iron oxide particles by spray-drying technique.

PubMed

Donadel, Karina; Felisberto, Marcos D V; Laranjeira, Mauro C M

2009-06-01

Magnetic particles of iron oxide have been increasingly used in medical diagnosis by magnetic resonance imaging and in cancer therapies involving targeted drug delivery and magnetic hyperthermia. In this study we report the preparation and characterization of iron oxide particles coated with bioceramic hydroxyapatite by spray-drying. The iron oxide magnetic particles (IOMP) were coated with hydroxyapatite (HAp) by spray-drying using two IOMP/HAp ratios (0.7 and 3.2). The magnetic particles were characterized by way of scanning electronic microscopy, energy dispersive X-ray, X-ray diffraction, Fourier transformed infrared spectroscopy, flame atomic absorption spectrometry,vibrating sample magnetometry and particle size distribution (laser diffraction). The surface morphology of the coated samples is different from that of the iron oxide due to formation of hydroxyapatite coating. From an EDX analysis, it was verified that the surface of the coated magnetic particles is composed only of HAp, while the interior containsiron oxide and a few layers of HAp as expected. The results showed that spray-drying technique is an efficient and relatively inexpensive method for forming spherical particles with a core/shell structure.

Atomically designed precursors in optical fiber amplifiers: The thermal stability of the heterobimetallic ErAl3(OPri)12 in a solution-coated silica soot

NASA Astrophysics Data System (ADS)

Engholm, M.; Lashgari, K.; Edvardsson, S.; Westin, G.; Norin, L.

2005-06-01

The thermal stability of the bimetallic alkoxide ErAl3(OPri)12 doped in an unsintered silica (soot) has been investigated. Samples have been heated to different temperatures (up to 1500°C and analyzed by using ultraviolet-visible-near infrared absorption spectroscopy, infrared spectroscopy, scanning electron microscopy, energy dispersive spectroscopy, thermal gravimetric analysis, and powder x-ray diffraction. It is seen that the doped samples heated up to 1000°C show broad glasslike absorption spectra, indicating an amorphous structure, while the high-temperature sample shows an ordered crystallinelike structure with sharp characteristic absorption peaks. X-ray diffraction measurements indicate the formation of an ordered structure at temperatures of 1500°C, revealing a crystal phase of silica and phases of erbium and aluminosilicate. A comparison is also made with a sample doped with aqueous ErCl3 and Al(NO3)3. It is concluded that the local structure of the ErAl3 precursor is not preserved at temperatures above 1000°C. Alternative doping procedures are discussed.

The effect of aluminum additions on the oxidation resistance of U 3Si 2

DOE PAGES

Wood, E. Sooby; White, J. T.; Nelson, A. T.

2017-04-01

The effect of aluminum additions to U 3Si 2 is investigated in this paper as a means to improve the oxidation resistance of this nuclear fuel form. Four U-Si-Al compositions have been synthesized and characterized using scanning electron microscopy, energy dispersive spectroscopy, and x-ray diffraction. The onsets of breakaway oxidation are identified in air thermal ramp tests using thermogravimetric analysis. The final oxidation products following 1000° C air exposure are identified using x-ray diffraction and compared to those of UO 2 and U metal oxidized in the same manner. Finally, thermogravimetric data acquired in this study indicates that increasing amountsmore » of Al in U 3Si 2 further delays the onset of breakaway oxidation, providing enhanced oxidation resistance in air. Al 2O 3 formation on U 3Al 2Si 3 is observed following a heat treatment performed at 500° C in air, demonstrating the potential of Al additions to improve the oxidation resistance of U 3Si 2.« less

Cellulose aerogels functionalized with polypyrrole and silver nanoparticles: In-situ synthesis, characterization and antibacterial activity.

PubMed

Wan, Caichao; Li, Jian

2016-08-01

Green porous and lightweight cellulose aerogels have been considered as promising candidates to substitute some petrochemical host materials to support various nanomaterials. In this work, waste wheat straw was collected as feedstock to fabricate cellulose hydrogels, and a green inexpensive NaOH/polyethylene glycol solution was used as cellulose solvent. Prior to freeze-drying treatment, the cellulose hydrogels were integrated with polypyrrole and silver nanoparticles by easily-operated in-situ oxidative polymerization of pyrrole using silver ions as oxidizing agent. The tri-component hybrid aerogels were characterized by scanning electron microscope, transmission electron microscope, energy dispersive X-ray spectroscopy, selected area electron diffraction, X-ray photoelectron spectroscopy, and X-ray diffraction. Moreover, the antibacterial activity of the hybrid aerogels against Escherichia coli (Gram-negative), Staphylococcus aureus (Gram-positive) and Listeria monocytogenes (intracellular bacteria) was qualitatively and quantitatively investigated by parallel streak method and determination of minimal inhibitory concentration, respectively. This work provides an example of combining cellulose aerogels with nanomaterials, and helps to develop novel forms of cellulose-based functional materials. Copyright © 2016 Elsevier Ltd. All rights reserved.

Electroless Nickel Deposition for Front Side Metallization of Silicon Solar Cells

PubMed Central

Hsieh, Shu Huei; Hsieh, Jhong Min; Chen, Wen Jauh; Chuang, Chia Chih

2017-01-01

In this work, nickel thin films were deposited on texture silicon by electroless plated deposition. The electroless-deposited Ni layers were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive x-ray spectroscopy (EDS), X-ray diffraction analysis (XRD), and sheet resistance measurement. The results indicate that the dominant phase was Ni2Si and NiSi in samples annealed at 300–800 °C. Sheet resistance values were found to correlate well with the surface morphology obtained by SEM and the results of XRD diffraction. The Cu/Ni contact system was used to fabricate solar cells by using two different activating baths. The open circuit voltage (Voc) of the Cu/Ni samples, before and after annealing, was measured under air mass (AM) 1.5 conditions to determine solar cell properties. The results show that open circuit voltage of a solar cell can be enhanced when the activation solution incorporated hydrofluoric acid (HF). This is mainly attributed to the native silicon oxide layer that can be decreased and/or removed by HF with the corresponding reduction of series resistance. PMID:28805724

Synthesis and characterization of Ce, Cu co-doped ZnS nanoparticles

NASA Astrophysics Data System (ADS)

Harish, G. S.; Sreedhara Reddy, P.

2015-09-01

Ce, Cu co-doped ZnS nanoparticles were prepared at room temperature using a chemical co-precipitation method. The prepared nanoparticles were characterized by X- ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive analysis of X-rays (EDAX), diffuse reflectance spectroscopy (DRS), photoluminescence (PL) and high resolution Raman spectroscopic techniques. Transmission electron microscopy (TEM) and X-ray diffraction studies showed that the diameter of the particles was around 2-3 nm. Broadened XRD peaks revealed the formation of nanoparticles with a face centered cubic (fcc) structure. DRS studies confirmed that the band gap increased with an increase in the dopant concentration. The Raman spectra of undoped and Ce, Cu ions co-doped ZnS nanoparticles showed longitudinal optical mode and transverse optical mode. Compared with the Raman modes (276 and 351 cm-1) of undoped ZnS nanoparticles, the Raman modes of Ce, Cu co- doped ZnS nanoparticles were slightly shifted towards lower frequency. PL spectra of the samples showed remarkable enhancement in the intensity upon doping.

The effect of aluminum additions on the oxidation resistance of U 3Si 2

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wood, E. Sooby; White, J. T.; Nelson, A. T.

The effect of aluminum additions to U 3Si 2 is investigated in this paper as a means to improve the oxidation resistance of this nuclear fuel form. Four U-Si-Al compositions have been synthesized and characterized using scanning electron microscopy, energy dispersive spectroscopy, and x-ray diffraction. The onsets of breakaway oxidation are identified in air thermal ramp tests using thermogravimetric analysis. The final oxidation products following 1000° C air exposure are identified using x-ray diffraction and compared to those of UO 2 and U metal oxidized in the same manner. Finally, thermogravimetric data acquired in this study indicates that increasing amountsmore » of Al in U 3Si 2 further delays the onset of breakaway oxidation, providing enhanced oxidation resistance in air. Al 2O 3 formation on U 3Al 2Si 3 is observed following a heat treatment performed at 500° C in air, demonstrating the potential of Al additions to improve the oxidation resistance of U 3Si 2.« less

Properties of Nitrogen-Doped Zinc Telluride Films for Back Contact to Cadmium Telluride Photovoltaics

NASA Astrophysics Data System (ADS)

Shimpi, Tushar M.; Drayton, Jennifer; Swanson, Drew E.; Sampath, Walajabad S.

2017-08-01

Zinc telluride (ZnTe) films have been deposited onto uncoated glass superstrates by reactive radiofrequency (RF) sputtering with different amounts of nitrogen introduced into the process gas, and the structural and electronic transport properties of the resulting nitrogen-doped ZnTe (ZnTe:N) films characterized. Based on transmission and x-ray diffraction measurements, it was observed that the crystalline quality of the ZnTe:N films decreased with increasing nitrogen in the deposition process. The bulk carrier concentration of the ZnTe:N films determined from Hall-effect measurements showed a slight decrease at 4% nitrogen flow rate. The effect of ZnTe:N films as back contact to cadmium telluride (CdTe) solar cells was also investigated. ZnTe:N films were deposited before or after CdCl2 passivation on CdTe/CdS samples. Small-area devices were characterized for their electronic properties. Glancing-angle x-ray diffraction measurements and energy-dispersive spectroscopy analysis confirmed substantial loss of zinc from the samples where CdCl2 passivation was carried out after ZnTe:N film deposition.

Biotransformation of hexavalent chromium into extracellular chromium(III) oxide nanoparticles using Schwanniomyces occidentalis.

PubMed

Mohite, Pallavi T; Kumar, Ameeta Ravi; Zinjarde, Smita S

2016-03-01

To demonstrate biotransformation of toxic Cr(VI) ions into Cr2O3 nanoparticles by the yeast Schwanniomyces occidentalis. Reaction mixtures containing S. occidentalis NCIM 3459 and Cr(VI) ions that were initially yellow turned green after 48 h incubation. The coloration was due to the synthesis of chromium (III) oxide nanoparticles (Cr2O3NPs). UV-Visible spectra of the reaction mixtures showed peaks at 445 and 600 nm indicating (4)A2g → (4)T1g and (4)A2g → (4)T2g transitions in Cr2O3, respectively. FTIR profiles suggested the involvement of carboxyl and amide groups in nanoparticle synthesis and stabilization. The Cr2O3NPs ranged between 10 and 60 nm. Their crystalline nature was evident from the selective area electron diffraction and X-ray diffraction patterns. Energy dispersive spectra confirmed the chemical composition of the nanoparticles. These biogenic nanoparticles could find applications in different fields. S. occidentalis mediated biotransformation of toxic Cr(VI) ions into crystalline extracellular Cr2O3NPs under benign conditions.

Interfacial characterization and electrical properties of Ni–GaSb contacts

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lin, Kun-Lin, E-mail: kllin@narlabs.org.tw; Chen, Szu-Hung, E-mail: shchen168@narlabs.org.tw

2014-10-06

The microstructural characterization of Ni–GaSb junctions in samples annealed at 300 °C, 350 °C, and 400 °C in a N{sub 2} atmosphere was elucidated using transmission electron microscopy in conjunction with energy-dispersive spectrometry, nanobeam electron diffraction, and grazing-incident X-ray diffraction. Only the NiSb(Ga) phase is formed at the interface of Ni/GaSb when the annealing temperature is below 350 °C. However, three phases—NiSb, Ni{sub 2}Ga{sub 3}, and NiSb(Ga)—are formed simultaneously at the interface between Ni/GaSb when the annealing temperature is increased to 400 °C, which causes a significant increase in the sheet resistance of the Ni–GaSb alloy. These results indicate that the annealing temperature of themore » Ni/GaSb structure should be maintained below 350 °C for the formation of low-resistance metal Ni/GaSb contacts in GaSb-based p-type metal-oxide-semiconductor field-effect transistors.« less

Synthesis and luminescence properties of cinnamide based nanohybrid materials containing Eu (II) ions

NASA Astrophysics Data System (ADS)

Kiran Kumar, A. B. V.; Jayasimhadri, M.; Cha, Hyeongrae; Chen, Kuangcai; Lim, Jae-Min; Lee, Yong-Ill

2011-07-01

In the present work, the cinnamide based organic-inorganic hybrid luminescent materials were prepared by using sol-gel technique, in which both the components are covalently linked via Si-C bonds. The organic precursor N-(3-(triethoxysilyl)propyl)cinnamide (Cn-Si) was synthesized by (3-aminopropyl) triethoxysilane being reacted with cinnamoyal chloride. Finally, novel hybrid materials were prepared successfully through hydrolysis and polycondensation processes between the alkoxide groups of precursors Cn-Si and tetraethylorthosilane (TEOS) in the presence of europium nitrate. We have characterized thoroughly the prepared samples using FT-IR, thermal analysis (TGA/DTA), X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), energy-dispersive spectroscopy (EDS) and photoluminescence (PL) spectroscopy. The results indicate that these materials exhibit the excellent thermal stability up to 350 °C. The X-ray diffraction patterns confirmed the amorphous nature of the developed materials. The rare-earth doped hybrid materials have exhibited an intense green emission at 530 nm with CIE chromaticity coordinates (0.4801, 0.4669). Whereas, the un-doped one gives some remarkable blue emission properties under UV excitation.

Crystal structure, Raman scattering and magnetic properties of CuCr2-xZrxSe4 and CuCr2-xSnxSe4 selenospinels

NASA Astrophysics Data System (ADS)

Pinto, C.; Galdámez, A.; Barahona, P.; Moris, S.; Peña, O.

2018-06-01

Selenospinels, CuCr2-xMxSe4 (M = Zr and Sn), were synthesized via conventional solid-state reactions. The crystal structure of CuCr1.5Sn0.5Se4, CuCr1.7Sn0.3Se4, CuCr1.5Zr0.5Se4, and CuCr1.8Zr0.2Se4 were determined using single-crystal X-ray diffraction. All the phases crystallized in a cubic spinel-type structure. The chemical compositions of the single-crystals were examined using energy-dispersive X-ray analysis (EDS). Powder X-ray diffraction patterns of CuCr1.3Sn0.7Se4 and CuCr1.7Sn0.3Se4 were consistent with phases belonging to the Fd 3 bar m Space group. An analysis of the vibrational properties on the single-crystals was performed using Raman scattering measurements. The magnetic properties showed a spin glass behavior with increasing Sn content and ferromagnetic order for CuCr1.7Sn0.3Se4.

Synthesis of Novel Sea-Urchin-Like CdS and Their Optical Properties.

PubMed

Kamran, Muhammad Arshad; Liu, Ruibin; Shi, Li-Jie; Bukhtiar, Arfan; Li, Jing; Zou, Bingsuo

2015-06-01

A novel morphology of CdS sea-urchin-like microstructures is synthesized by simple thermal evaporation process. Microstructures with average size of 20-50 μm are composed of single crystalline CdS nanobelts. The structural, compositional, morphological characterization of the product were examined by X-ray diffraction, energy dispersive X-ray spectroscopy, Raman spectroscopy, scanning electron microscope, transmission electron microscopy and selected area electron diffraction while optical properties are investigated by Photoluminescence spectroscopy and time-resolved Photoluminescence measurements. The tentative growth mechanism for the growth of sea-urchin-like CdS is proposed and described briefly. A strong green emission with a maximum around 517 nm was observed from the individual CdS microstructure at room temperature, which was attributed to band-edge emission of CdS. These Novel structures exhibit excellent lasing (stimulated emission) with low threshold (9.07 μJ cm(-2)) at room temperature. We analyze the physical mechanism of stimulated emission. These results are important in the design of green luminescence, low-threshold laser and display devices in the future.

Ca-P spots modified zirconia by liquid precursor infiltration and the effect on osteoblast-like cell responses.

PubMed

Li, Yongmei; Liu, Yan; Zhang, Zutai; Zhuge, Ruishen; Ding, Ning; Tian, Yueming

2018-01-26

Ca-P spots modified zirconia by liquid precursor infiltration and the cell responses were investigated. Pre-sintered zirconia specimens were immersed in Ca-P precursor solution. After dense sintering, scanning electron microscopy showed Ca-P spots were formed on the zirconia and anchored with zirconia substrates. The distribution density was increased with the extension of immersion time. Energy dispersive spectrometer confirmed the stoichiometric Ca/P ratio was about 1.67. After hydrothermal treatment, Ca-P spots turned into rod crystals where diffraction peaks of tricalcium phosphate and hydroxyapatite were detected by X-ray diffraction, and Ca 2+ and PO 4 3- release decreased slightly (p>0.05). There was no significant decrease on three-point bending strength (p>0.05). Osteoblast-like MC3T3-E1 cells attached and spread well and showed higher proliferation on Ca-P spots modified zirconia (p<0.05), though its initial alkaline phosphatase activity was not significant high (p>0.05). In conclusion, Ca-P liquid precursor infiltration is a potential method to modify the zirconia ceramics for improving bioactivity.

Structure and mechanical properties of foils made of nanocrystalline beryllium

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhigalina, O. M., E-mail: zhigal@ns.crys.ras.ru; Semenov, A. A.; Zabrodin, A. V.

2016-07-15

The phase composition and structural features of (45–90)-μm-thick foils obtained from nanocrystalline beryllium during multistep thermomechanical treatment have been established using electron microscopy, electron diffraction, electron backscattering diffraction, and energy-dispersive analysis. This treatment is shown to lead to the formation of a structure with micrometer- and submicrometer-sized grains. The minimum average size of beryllium grains is 352 nm. The inclusions of beryllium oxide (BeO) of different modifications with tetragonal (sp. gr. P4{sub 2}/mnm) and hexagonal (sp. gr. P6{sub 3}/mmc) lattices are partly ground during deformation to a size smaller than 100 nm and are located along beryllium grain boundaries inmore » their volume, significantly hindering migration during treatment. The revealed structural features of foils with submicrometer-sized crystallites provide the thermal stability of their structural state. Beryllium with this structure is a promising material for X-ray instrument engineering and for the production of ultrathin (less than 10 μm) vacuum-dense foils with very high physicomechanical characteristics.« less

X-ray diffraction, Raman, and photoacoustic studies of ZnTe nanocrystals

NASA Astrophysics Data System (ADS)

Ersching, K.; Campos, C. E. M.; de Lima, J. C.; Grandi, T. A.; Souza, S. M.; da Silva, D. L.; Pizani, P. S.

2009-06-01

Nanocrystalline ZnTe was prepared by mechanical alloying. X-ray diffraction (XRD), energy dispersive spectroscopy, Raman spectroscopy, and photoacoustic absorption spectroscopy techniques were used to study the structural, chemical, optical, and thermal properties of the as-milled powder. An annealing of the mechanical alloyed sample at 590 °C for 6 h was done to investigate the optical properties in a defect-free sample (close to bulk form). The main crystalline phase formed was the zinc-blende ZnTe, but residual trigonal tellurium and hexagonal ZnO phases were also observed for both as-milled and annealed samples. The structural parameters, phase fractions, average crystallite sizes, and microstrains of all crystalline phases were obtained from Rietveld analyses of the X-ray patterns. Raman results corroborate the XRD results, showing the longitudinal optical phonons of ZnTe (even at third order) and those modes of trigonal Te. Nonradiative surface recombination and thermal bending heat transfer mechanisms were proposed from photoacoustic analysis. An increase in effective thermal diffusivity coefficient was observed after annealing and the carrier diffusion coefficient, the surface recombination velocity, and the recombination time parameters remained the same.

Microscopic structural change in a liquid Fe-C alloy of ~5 GPa

DOE PAGES

Shibazaki, Yuki; Kono, Yoshio; Fei, Yingwei

2015-07-04

The structure of a liquid Fe-3.5 wt% C alloy is examined for up to 7.2 GPa via multiangle energy-dispersive X-ray diffraction using a Paris-Edinburgh type large-volume press. X-ray diffraction data show clear changes in the pressure-dependent peak positions of structure factor and reduced pair distribution function at 5GPa. These results suggest that the liquid Fe-3.5wt%C alloys change structurally at approximately 5GPa. This finding serves as a microscopic explanation for the alloy’s previously observed density change at the same pressure. The pressure dependencies of the nearest and second neighbor distances of the liquid Fe-3.5 wt% C alloy are similar to thosemore » of liquid Fe which exhibits a structural change near the bcc-fcc-liquid triple point (5.2GPa and 1991 K). Here, similarities between Fe-3.5wt% C and Fe suggest that a density change also occurs in liquid Fe and that this structural change extends to other Fe-light element alloys.« less

Synthesis and characterization of nano TiO2-SiO2: PVA composite - a novel route

NASA Astrophysics Data System (ADS)

Venckatesh, Rajendran; Balachandaran, Kartha; Sivaraj, Rajeshwari

2012-07-01

A novel, simple, less time consuming and cost-effective sol-gel method has been developed to synthesize nano titania-silica with polyvinyl alcohol (PVA) composite relatively at low temperature in acidic pH. Titania sol is prepared by hydrolysis of titanium tetrachloride and was mixed with silicic acid and tetrahydrofuran mixture. The reaction was carried out under vigorous stirring for 6 h and dried at room temperature with the addition of PVA solution. The resulting powders were characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, Fourier transform infrared (FT-IR), UV-visible spectroscopy and thermal techniques. The grain size of the particles was calculated by X-ray diffraction; surface morphology and chemical composition were determined from scanning electron microscopy-energy dispersive spectroscopy; metal oxide stretching was confirmed from FT-IR spectroscopy; bandgap was calculated using UV-visible spectroscopy, and thermal stability of the prepared composite was determined by thermogravimetric/differential thermal analysis. Since TiO2 got agglomerated on the surface of SiO2, effective absorptive sites increase which in turn increase the photocatalytic efficiency of the resulting composite.

Periodical energy oscillation and pulse splitting in sinusoidal volume holographic grating.

PubMed

Yan, Xiaona; Gao, Lirun; Dai, Ye; Yang, Xihua; Chen, Yuanyuan; Ma, Guohong

2014-07-28

This paper presents dynamical diffraction properties of a femtosecond pulse in a sinusoidal volume holographic grating (VHG). By the modified coupled-wave equations of Kogelnik, we show that the diffraction of a femtosecond pulse on the VHG gives rise to periodical energy oscillation and pulse splitting. In the initial stage of diffraction, one diffracted pulse and one transmitted pulse emerge, and energy of the transmitted pulse periodically transfers to the diffracted pulse and vice versa. In the latter stage, both the diffracted and transmitted pulses split into two spatially separated pulses. One pair of transmitted and diffracted pulses propagates in the same direction and forms the output diffracted dual pulses of the VHG, and the other pair of pulses forms the output transmitted dual pulses. The pulse interval between each pair of dual pulses is in linearly proportional to the refractive index modulation and grating thickness. By the interference effect and group velocity difference we give explanations on the periodical energy oscillation and pulse splitting respectively.

Adaptable Diffraction Gratings With Wavefront Transformation

NASA Technical Reports Server (NTRS)

Iazikov, Dmitri; Mossberg, Thomas W.; Greiner, Christoph M.

2010-01-01

Diffraction gratings are optical components with regular patterns of grooves, which angularly disperse incoming light by wavelength. Traditional diffraction gratings have static planar, concave, or convex surfaces. However, if they could be made so that they can change the surface curvature at will, then they would be able to focus on particular segments, self-calibrate, or perform fine adjustments. This innovation creates a diffraction grating on a deformable surface. This surface could be bent at will, resulting in a dynamic wavefront transformation. This allows for self-calibration, compensation for aberrations, enhancing image resolution in a particular area, or performing multiple scans using different wavelengths. A dynamic grating gives scientists a new ability to explore wavefronts from a variety of viewpoints.

Highly aqueous soluble CaF2:Ce/Tb nanocrystals: effect of surface functionalization on structural, optical band gap, and photoluminescence properties.

PubMed

Ansari, Anees A; Parchur, Abdul K; Kumar, Brijesh; Rai, S B

2016-12-01

The design of nanostructured materials with highly stable water-dispersion and luminescence efficiency is an important concern in nanotechnology and nanomedicine. In this paper, we described the synthesis and distinct surface modification on the morphological structure and optical (optical absorption, band gap energy, excitation, emission, decay time, etc.) properties of highly crystalline water-dispersible CaF 2 :Ce/Tb nanocrystals (core-nanocrystals). The epitaxial growth of inert CaF 2 and silica shell, respectively, on their surface forming as CaF 2 :Ce/Tb@CaF 2 (core/shell) and CaF 2 :Ce/Tb@CaF 2 @SiO 2 (core/shell/SiO 2 ) nanoarchitecture. X-ray diffraction and transmission electron microscope image shows that the nanocrystals were in irregular spherical phase, highly crystalline (~20 nm) with narrow size distribution. The core/shell nanocrystals confirm that the surface coating is responsible in the change of symmetrical nanostructure, which was determined from the band gap energy and luminescent properties. It was found that an inert inorganic shell formation effectively enhances the luminescence efficiency and silica shell makes the nanocrystals highly water-dispersible. In addition, Ce 3+ /Tb 3+ -co-doped CaF 2 nanocrystals show efficient energy transfer from Ce 3+ to Tb 3+ ion and strong green luminescence of Tb 3+ ion at 541 nm( 5 D 4 → 7 F 5 ). Luminescence decay curves of core and core/shell nanocrystals were fitted using mono and biexponential equations, and R 2 regression coefficient criteria were used to discriminate the goodness of the fitted model. The lifetime values for the core/shell nanocrystals are higher than core-nanocrystals. Considering the high stable water-dispersion and intensive luminescence emission in the visible region, these luminescent core/shell nanocrystals could be potential candidates for luminescent bio-imaging, optical bio-probe, displays, staining, and multianalyte optical sensing. A newly designed CaF 2 :Ce/Tb nanoparticles via metal complex decomposition rout shows high dispersibility in aqueous solvents with enhanced photoluminescence. The epitaxial growth of inert CaF 2 shell and further amorphous silica, respectively, enhanced their optical and luminescence properties, which is highly usable for luminescent biolabeling, and optical bioprobe etc.

Application of high-resolution linear Radon transform for Rayleigh-wave dispersive energy imaging and mode separating

USGS Publications Warehouse

Luo, Y.; Xia, J.; Miller, R.D.; Liu, J.; Xu, Y.; Liu, Q.

2008-01-01

Multichannel Analysis of Surface Waves (MASW) analysis is an efficient tool to obtain the vertical shear-wave profile. One of the key steps in the MASW method is to generate an image of dispersive energy in the frequency-velocity domain, so dispersion curves can be determined by picking peaks of dispersion energy. In this paper, we image Rayleigh-wave dispersive energy and separate multimodes from a multichannel record by high-resolution linear Radon transform (LRT). We first introduce Rayleigh-wave dispersive energy imaging by high-resolution LRT. We then show the process of Rayleigh-wave mode separation. Results of synthetic and real-world examples demonstrate that (1) compared with slant stacking algorithm, high-resolution LRT can improve the resolution of images of dispersion energy by more than 50% (2) high-resolution LRT can successfully separate multimode dispersive energy of Rayleigh waves with high resolution; and (3) multimode separation and reconstruction expand frequency ranges of higher mode dispersive energy, which not only increases the investigation depth but also provides a means to accurately determine cut-off frequencies.

Highly surface-roughened quasi-spherical silver powders in back electrode paste for silicon solar cells

NASA Astrophysics Data System (ADS)

Yin, Peng; Liu, Shouchao; Li, Qiuying; Chen, Xiaolei; Guo, Weihong; Wu, Chifei

2017-08-01

In our work, highly surface-roughened quasi-spherical silver powders with controllable size and superior dispersibility, which have narrow size distribution and relatively high tap density, were successfully prepared by reducing silver nitrate with ascorbic acid in aqueous solutions. Gum arabic (AG) was selected as dispersant to prevent the agglomeration of silver particles. Furthermore, the effects of preparation conditions on the characteristics of the powders were systematically investigated. By varying the concentration of the reactants, dosage of dispersant, the feeding modes, synthesis temperature and the pH value of the mixture solution of silver nitrate and AG, the resulted silver particles displayed controllable size, different morphologies and surface roughness. The spherical silver powder with mean particle size of 1.20 µm, tap density of 4.1 g cm-3 and specific area value of 0.46 m2 g-1 was prepared by adjusting preparation conditions. The AG absorbed on the surface preventing the silver particles from diffusion and aggregation was proved by the ultraviolet spectra. Observations of SEM images showed that the as-prepared silver powders were relatively monodisperse silver spheres with highly roughened surface and the particle size was controllable from 1 µm to 5 µm, specific surface area value from approximately 0.2 m2 g-1 to 0.8 m2 g-1. X-ray diffraction (XRD) patterns, energy dispersive spectroscopy (EDS), x-ray photoelectron spectra (XPS) and thermal gravity analysis (TGA) demonstrated high crystallinity and purity of the obtained silver powders.

Hydrogen production via reforming of biogas over nanostructured Ni/Y catalyst: Effect of ultrasound irradiation and Ni-content on catalyst properties and performance

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sharifi, Mahdi; Reactor and Catalysis Research Center; Haghighi, Mohammad, E-mail: haghighi@sut.ac.ir

2014-12-15

Highlights: • Synthesis of nanostructured Ni/Y catalyst by sonochemical and impregnation methods. • Enhancement of size distribution and active phase dispersion by employing sonochemical method. • Evaluation of biogas reforming over Ni/Y catalyst with different Ni-loadings. • Preparation of highly active and stable catalyst with low Ni content for biogas reforming. • Getting H{sub 2}/CO very close to equilibrium ratio by employing sonochemical method. - Abstract: The effect of ultrasound irradiation and various Ni-loadings on dispersion of active phase over zeolite Y were evaluated in biogas reforming for hydrogen production. X-ray diffraction, field emission scanning electron microscopy, energy dispersive X-ray,more » Brunauer–Emmett–Teller, Fourier transform infrared analysis and TEM analysis were employed to observe the characteristics of nanostructured catalysts. The characterizations implied that utilization of ultrasound irradiation enhanced catalyst physicochemical properties including high dispersion of Ni on support, smallest particles size and high catalyst surface area. The reforming reactions were carried out at GHSV = 24 l/g.h, P = 1 atm, CH{sub 4}/CO{sub 2} = 1 and temperature range of 550–850 °C. Activity test displayed that ultrasound irradiated Ni(5 wt.%)/Y had the best performance and the activity remained stable during 600 min. Furthermore, the proposed reaction mechanism showed that there are three major reaction channels in biogas reforming.« less

Core-shell Fe3O4 polydopamine nanoparticles as sorbent for magnetic dispersive solid-phase extraction of copper from food samples.

PubMed

Yavuz, Emre; Tokalıoğlu, Şerife; Patat, Şaban

2018-10-15

In the present study, core-shell Fe 3 O 4 polydopamine nanoparticles were synthesized and used for the first time as an adsorbent for the vortex assisted magnetic dispersive solid phase extraction of copper from food samples. After elution, copper in the solutions was determined by FAAS. The adsorbent was characterized using X-ray diffraction, scanning electron microscopy, energy dispersive X-ray spectroscopy, Fourier transform infrared spectroscopy, Brunauer-Emmett-Teller surface area, and zeta potential measurements. Various parameters affecting the magnetic dispersive solid-phase extraction were evaluated. The optimum pH and magnetic adsorbent amount were found to be 5 and 40 mg, respectively. Elution was made by 3 mL of 2 mol L -1 HNO 3 .The major advantage of the method is the fast equilibration during adsorption without the need for vortexing or shaking. The preconcentration factor and detection limit of the method were found to be 150 and 0.22 mg L -1 , respectively. The precision (as RSD%) and adsorption capacity of the method were 3.7% and 28 mg g -1 , respectively. The method was successfully verified by analyzing four certified reference materials (SPS-WW1 Batch 114 Wastewater, TMDA-53.3 Lake water, BCR-482 Lichen and 1573a Tomato Leaves) and by addition/recovery tests of copper standard solution in organic baby food, muesli, macaroni, honey, and milk samples. Copyright © 2018 Elsevier Ltd. All rights reserved.

Stable diffraction-management soliton in a periodic structure with alternating left-handed and right-handed media

NASA Astrophysics Data System (ADS)

Zhang, Jinggui

2017-09-01

In this paper, we first derive a modified two-dimensional non-linear Schrödinger equation including high-order diffraction (HOD) suitable for the propagation of optical beam near the low-diffraction regime in Kerr non-linear media with spatial dispersion. Then, we apply our derived physical model to a designed two-dimensional configuration filled with alternate layers of a left-handed material (LHM) and a right-handed media by employing the mean-field theory. It is found that the periodic structure including LHM may experience diminished, cancelled, and even reversed diffraction behaviours through engineering the relative thickness between both media. In particular, the variational method analytically predicts that close to the zero-diffraction regime, such periodic structure can support stable diffraction-management solitons whose beamwidth and peak amplitude evolve periodically with the help of HOD effect. Numerical simulation based on the split-step Fourier method confirms the analytical results.

Beam steering for virtual/augmented reality displays with a cycloidal diffractive waveplate.

PubMed

Chen, Haiwei; Weng, Yishi; Xu, Daming; Tabiryan, Nelson V; Wu, Shin-Tson

2016-04-04

We proposed a switchable beam steering device with cycloidal diffractive waveplate (CDW) for eye tracking in a virtual reality (VR) or augmented reality (AR) display system. Such a CDW diffracts the incident circularly polarized light to the first order with over 95% efficiency. To convert the input linearly polarized light to right-handed or left-handed circular polarization, we developed a broadband polarization switch consisting of a twisted nematic liquid crystal cell and an achromatic quarter-wave retardation film. By cascading 2-3 CDWs together, multiple diffraction angles can be achieved. To suppress the color dispersion, we proposed two approaches to obtain the same diffraction angle for red, green, and blue LEDs-based full color displays. Our device exhibits several advantages, such as high diffraction efficiency, fast response time, low power consumption, and low cost. It holds promise for the emerging VR/AR displays.

Ultraviolet acousto-optic programmable dispersive filter laser pulse shaping in KDP.

PubMed

Coudreau, Sebastien; Kaplan, Daniel; Tournois, Pierre

2006-06-15

An acousto-optic programmable dispersive filter pulse shaper has been designed using KDP material for operation in the 200-500 nm wavelength range. With an acousto-optic interaction length of 72 mm, a spectral resolution of 0.15 nm has been measured to be consistent with theoretical predictions. Theory and experiments indicate that diffraction efficiencies up to 50% are expected in practical experimental conditions.

Energy resolution of the CdTe-XPAD detector: calibration and potential for Laue diffraction measurements on protein crystals.

PubMed

Medjoubi, Kadda; Thompson, Andrew; Bérar, Jean-François; Clemens, Jean-Claude; Delpierre, Pierre; Da Silva, Paulo; Dinkespiler, Bernard; Fourme, Roger; Gourhant, Patrick; Guimaraes, Beatriz; Hustache, Stéphanie; Idir, Mourad; Itié, Jean-Paul; Legrand, Pierre; Menneglier, Claude; Mercere, Pascal; Picca, Frederic; Samama, Jean-Pierre

2012-05-01

The XPAD3S-CdTe, a CdTe photon-counting pixel array detector, has been used to measure the energy and the intensity of the white-beam diffraction from a lysozyme crystal. A method was developed to calibrate the detector in terms of energy, allowing incident photon energy measurement to high resolution (approximately 140 eV), opening up new possibilities in energy-resolved X-ray diffraction. In order to demonstrate this, Laue diffraction experiments were performed on the bending-magnet beamline METROLOGIE at Synchrotron SOLEIL. The X-ray energy spectra of diffracted spots were deduced from the indexed Laue patterns collected with an imaging-plate detector and then measured with both the XPAD3S-CdTe and the XPAD3S-Si, a silicon photon-counting pixel array detector. The predicted and measured energy of selected diffraction spots are in good agreement, demonstrating the reliability of the calibration method. These results open up the way to direct unit-cell parameter determination and the measurement of high-quality Laue data even at low resolution. Based on the success of these measurements, potential applications in X-ray diffraction opened up by this type of technology are discussed.

Dispersion-compensated fresnel lens

DOEpatents

Johnson, Kenneth C.

1992-01-01

A transmission grating is used to reduce chromatic aberration in a Fresnel lens, wherein the lens chromatic dispersion is offset and substantially canceled by the grating's diffraction-induced dispersion. The grating comprises a Fresnel-type pattern of microscopic facets molded directly into the lens surface. The facets would typically have a profile height of around 4.multidot.10.sup.-5 inch and a profile width of at least 10.sup.-3 inch. In its primary intended application, the invention would function to improve the optical performance of a Fresnel lens used to concentrate direct sunlight.

Dispersion-compensated Fresnel lens

DOEpatents

Johnson, K.C.

1992-11-03

A transmission grating is used to reduce chromatic aberration in a Fresnel lens, wherein the lens chromatic dispersion is offset and substantially canceled by the grating's diffraction-induced dispersion. The grating comprises a Fresnel-type pattern of microscopic facets molded directly into the lens surface. The facets would typically have a profile height of around 4[times]10[sup [minus]5] inch and a profile width of at least 10[sup [minus]3] inch. In its primary intended application, the invention would function to improve the optical performance of a Fresnel lens used to concentrate direct sunlight. 10 figs.

Position sensitive and energy dispersive x-ray detector based on silicon strip detector technology

NASA Astrophysics Data System (ADS)

Wiącek, P.; Dąbrowski, W.; Fink, J.; Fiutowski, T.; Krane, H.-G.; Loyer, F.; Schwamberger, A.; Świentek, K.; Venanzi, C.

2015-04-01

A new position sensitive detector with a global energy resolution for the entire detector of about 380 eV FWHM for 8.04 keV line at ambient temperature is presented. The measured global energy resolution is defined by the energy spectra summed over all strips of the detector, and thus it includes electronic noise of the front-end electronics, charge sharing effects, matching of parameters across the channels and other system noise sources. The target energy resolution has been achieved by segmentation of the strips to reduce their capacitance and by careful optimization of the front-end electronics. The key design aspects and parameters of the detector are discussed briefly in the paper. Excellent noise and matching performance of the readout ASIC and negligible system noise allow us to operate the detector with a discrimination threshold as low as 1 keV and to measure fluorescence radiation lines of light elements, down to Al Kα of 1.49 keV, simultaneously with measurements of the diffraction patterns. The measurement results that demonstrate the spectrometric and count rate performance of the developed detector are presented and discussed in the paper.

Color separation gratings

NASA Technical Reports Server (NTRS)

Farn, Michael W.; Knowlden, Robert E.

1993-01-01

In this paper, we describe the theory, fabrication and test of a binary optics 'echelon'. The echelon is a grating structure which separates electromagnetic radiation of different wavelengths, but it does so according to diffraction order rather than by dispersion within one diffraction order, as is the case with conventional gratings. A prototype echelon, designed for the visible spectrum, is fabricated using the binary optics process. Tests of the prototype show good agreement with theoretical predictions.

X-ray and neutron diffraction anomalies preceding martensitic phase transformation in AuCuZn2 alloys

NASA Astrophysics Data System (ADS)

Nagasawa, A.; Makita, T.; Nakanishi, N.; Iizumi, M.; Morii, Y.

1988-04-01

The present paper gives the results obtained by the X-ray and neutron diffraction studies on the single crystals of the beta-1 AuCuZn2 alloys. As precursor phenomena, the dispersion relation of the [110] TA1 phonon exhibits significant dip near 2/3 [110] q max position and anomalous peaks appear around 1/3 and 2/3 [110] q max positions. Characteristics of the interplanar force constants, obtained by the analysis of the dispersion relation, and the positions of the anomalous peaks predict the martensite structures to be formed in the beta phase alloys. In the present case, both the 6R and 18R martensites will be formed by cooling and/or under the stress field.

Variable magnification variable dispersion glancing incidence imaging x-ray spectroscopic telescope

NASA Technical Reports Server (NTRS)

Hoover, Richard B. (Inventor)

1991-01-01

A variable magnification variable dispersion glancing incidence x-ray spectroscopic telescope capable of multiple high spatial revolution imaging at precise spectral lines of solar and stellar x-ray and extreme ultraviolet radiation sources includes a pirmary optical system which focuses the incoming radiation to a primary focus. Two or more rotatable carries each providing a different magnification are positioned behind the primary focus at an inclination to the optical axis, each carrier carrying a series of ellipsoidal diffraction grating mirrors each having a concave surface on which the gratings are ruled and coated with a mutlilayer coating to reflect by diffraction a different desired wavelength. The diffraction grating mirrors of both carriers are segments of ellipsoids having a common first focus coincident with the primary focus. A contoured detector such as an x-ray sensitive photogrpahic film is positioned at the second respective focus of each diffraction grating so that each grating may reflect the image at the first focus to the detector at the second focus. The carriers are selectively rotated to position a selected mirror for receiving radiation from the primary optical system, and at least the first carrier may be withdrawn from the path of the radiation to permit a selected grating on the second carrier to receive radiation.

Variable magnification variable dispersion glancing incidence imaging x ray spectroscopic telescope

NASA Technical Reports Server (NTRS)

Hoover, Richard (Inventor)

1990-01-01

A variable magnification variable dispersion glancing incidence x ray spectroscopic telescope capable of multiple high spatial revolution imaging at precise spectral lines of solar and stellar x ray and extreme ultraviolet radiation sources includes a primary optical system which focuses the incoming radiation to a primary focus. Two or more rotatable carriers each providing a different magnification are positioned behind the primary focus at an inclination to the optical axis, each carrier carrying a series of ellipsoidal diffraction grating mirrors each having a concave surface on which the gratings are ruled and coated with a multilayer coating to reflect by diffraction a different desired wavelength. The diffraction grating mirrors of both carriers are segments of ellipsoids having a common first focus coincident with the primary focus. A contoured detector such as an x ray sensitive photographic film is positioned at the second respective focus of each diffraction grating so that each grating may reflect the image at the first focus to the detector at the second focus. The carriers are selectively rotated to position a selected mirror for receiving radiation from the primary optical system, and at least the first carrier may be withdrawn from the path of the radiation to permit a selected grating on the second carrier to receive radiation.

Synthesis of highly stable silver nanoparticles through a novel green method using Mirabillis jalapa for antibacterial, nonlinear optical applications

NASA Astrophysics Data System (ADS)

Pugazhendhi, S.; Palanisamy, P. K.; Jayavel, R.

2018-05-01

Green synthesis techniques are developing as more simplistic and eco-friendly approach for the synthesis of metal nanoparticles compared to chemical reduction methods. Herein we report Synthesis of highly stable silver nanoparticles using Mirabillis jalapa seed extract as a reducing and capping agent. The as-prepared silver nanoparticles were characterized by UV-vis spectroscopy (UV-vis) to confirm the formation of silver nanoparticles by its characteristic surface plasmon resonance peak observed at 420 nm. The Powder X-ray diffraction (P-XRD) revealed the structure and crystalline nature of synthesized silver nanoparticles, The Fourier transform infra-red spectroscopic (FT-IR) revealed the presence of the biomolecules in the extract that acted as reducing as well stabilizing agent. The high resolution transmission electron microscopic (HRTEM) images divulged that the synthesized silver nanoparticles were spherical in shape and poly dispersed. The energy dispersive X-ray diffraction (EDX) profile revealed the elements present in the as-synthesized colloidal silver nanoparticles and its percentages. The Zeta potential measured for silver nanoparticles evidenced that the prepared silver nanoparticles owned high stability in room temperature itself. The as-synthesized silver nanoparticles (AgNPs) in colloidal form were showed good antimicrobial effects and it's were found to exhibit third order optical nonlinearity as studied by Z-scan technique using 532 nm Nd:YAG (SHG) CW laser beam (COHERENT-Compass 215 M-50 diode pumped) output as source. The negative nonlinearity observed was well utilized for the study of optical limiting behavior of the silver nanoparticles.

Characterizing the residual glass in a MgO/Al2O3/SiO2/ZrO2/Y2O3 glass-ceramic

PubMed Central

Seidel, Sabrina; Patzig, Christian; Wisniewski, Wolfgang; Gawronski, Antje; Hu, Yongfeng; Höche, Thomas; Rüssel, Christian

2016-01-01

The non-isochemical crystallization of glasses leads to glass-ceramics in which the chemical composition of the amorphous matrix differs from that of the parent glass. It is challenging to solely analyse the properties of these residual glassy phases because they frequently contain finely dispersed crystals. In this study, the composition of the residual glass matrix after the crystallization of a glass with the mol% composition 50.6 SiO2 · 20.7 MgO · 20.7 Al2O3 · 5.6 ZrO2 · 2.4 Y2O3 is analysed by scanning transmission electron microscopy (STEM) including energy dispersive X-ray analysis (EDXS). A batch of the residual glass with the determined composition is subsequently melted and selected properties are analysed. Furthermore, the crystallization behaviour of this residual glass is studied by X-ray diffraction, scanning electron microscopy including electron backscatter diffraction and STEM-EDXS analyses. The residual glass shows sole surface crystallization of indialite and multiple yttrium silicates while bulk nucleation does not occur. This is in contrast to the crystallization behaviour of the parent glass, in which a predominant bulk nucleation of spinel and ZrO2 is observed. The crystallization of the residual glass probably leads to different crystalline phases when it is in contact to air, rather than when it is enclosed within the microstructure of the parent glass-ceramics. PMID:27734918

Electron paramagnetic resonance, scanning electron microscopy with energy dispersion X-ray spectrometry, X-ray powder diffraction, and NMR characterization of iron-rich fired clays.

PubMed

Presciutti, Federica; Capitani, Donatella; Sgamellotti, Antonio; Brunetti, Brunetto Giovanni; Costantino, Ferdinando; Viel, Stéphane; Segre, Annalaura

2005-12-01

The aim of this study is to clarify the structure of an iron-rich clay and the structural changes involved in the firing process as a preliminary step to get information on ancient ceramic technology. To this purpose, illite-rich clay samples fired at different temperatures were characterized using a multitechnique approach, i.e., by electron paramagnetic resonance, scanning electron microscopy with electron dispersion X-ray spectrometry, X-ray powder diffraction, magic angle spinning and multiple quantum magic angle spinning NMR. During firing, four main reaction processes occur: dehydration, dehydroxylation, structural breakdown, and recrystallization. When the results are combined from all characterization methods, the following conclusions could be obtained. Interlayer H2O is located close to aluminum in octahedral sites and is driven off at temperatures lower than 600 degrees C. Between 600 and 700 degrees C dehydroxylation occurs whereas, between 800 and 900 degrees C, the aluminum in octahedral sites disappears, due to the breakdown of the illite structure, and all iron present is oxidized to Fe3+. In samples fired at 1000 and 1100 degrees C iron clustering was observed as well as large single crystals of iron with the occurrence of ferro- or ferrimagnetic effects. Below 900 degrees C the aluminum in octahedral sites presents a continuous distribution of chemical shift, suggesting the presence of slightly distorted sites. Finally, over the whole temperature range, the presence of at least two tetrahedral aluminum sites was revealed, characterized by different values of the quadrupolar coupling constant.

Asymmetric transmission in prisms using structures and materials with isotropic-type dispersion.

PubMed

Gundogdu, Funda Tamara; Serebryannikov, Andriy E; Cakmak, A Ozgur; Ozbay, Ekmel

2015-09-21

It is demonstrated that strong asymmetry in transmission can be obtained at the Gaussian beam illumination for a single prism based on a photonic crystal (PhC) with isotropic-type dispersion, as well as for its analog made of a homogeneous material. Asymmetric transmission can be realized with the aid of refraction at a proper orientation of the interfaces and wedges of the prism, whereas neither contribution of higher diffraction orders nor anisotropic-type dispersion is required. Furthermore, incidence toward a prism wedge can be used for one of two opposite directions in order to obtain asymmetry. Thus, asymmetric transmission is a general property of the prism configurations, which can be obtained by using simple geometries and quite conventional materials. The obtained results show that strong asymmetry can be achieved in PhC prisms with (nearly) circular shape of equifrequency dispersion contours, in both cases associated with the index of refraction 01. For the comparison purposes, results are also presented for solid uniform non-magnetic prisms made of a material with the same value of n. It is shown in zero-loss approximation that the PhC prism and the ultralow-index material prism (01. Possible contributions of scattering on the individual rods and diffraction on the wedge to the resulting mechanism are discussed. Analogs of unidirectional splitting and unidirectional deflection regimes, which are known from the studies of PhC gratings, are obtained in PhC prisms and solid uniform prisms, i.e. without higher diffraction orders.

Multi-element germanium detectors for synchrotron applications

DOE PAGES

Rumaiz, A. K.; Kuczewski, A. J.; Mead, J.; ...

2018-04-27

In this paper, we have developed a series of monolithic multi-element germanium detectors, based on sensor arrays produced by the Forschungzentrum Julich, and on Application-specific integrated circuits (ASICs) developed at Brookhaven. Devices have been made with element counts ranging from 64 to 384. These detectors are being used at NSLS-II and APS for a range of diffraction experiments, both monochromatic and energy-dispersive. Compact and powerful readout systems have been developed, based on the new generation of FPGA system-on-chip devices, which provide closely coupled multi-core processors embedded in large gate arrays. Finally, we will discuss the technical details of the systems,more » and present some of the results from them.« less

Characterization of the NEXT Hollow Cathode Inserts After Long-Duration Testing

NASA Technical Reports Server (NTRS)

Mackey, J.; Shastry, R.; Soulas, G.

2017-01-01

Hollow dispenser cathode inserts are a critical element of electric propulsion systems, and should therefore be well understood during long term operation to ensure reliable system performance. This work destructively investigated cathode inserts from the NEXT long-duration test which demonstrated 51,184 hours of high-voltage operation, 918 kg of propellant throughput, and 35.5 MN-s of total impulse. The characterization methods used include scanning electron microscopy with energy dispersive spectroscopy and X-ray diffraction. Microscopy analysis has been performed on fractured surfaces, emission surfaces, and metallographically polished cross-sections of post-test inserts and unused inserts. Impregnate distribution, etch region thickness, impregnate chemical content, emission surface topography, and emission surface phase identification are the primary factors investigated.

Study of the structural organization of cyclodextrin-DNA complex loaded anionic and pH-sensitive liposomes

NASA Astrophysics Data System (ADS)

Silva, Sônia M. L.; Coelho, Letícia N.; Malachias, Ângelo; Perez, Carlos A.; Pesquero, Jorge L.; Magalhães-Paniago, Rogério; de Oliveira, Mônica C.

2011-04-01

The present study investigated the effect of the 6-monodeoxy-6-monoamine-β-cyclodextrin(Am-β-CD)/DNA (Am-β-CD/DNA) complex, as well as of culture medium components and proteins, at pH 7.4 and 5.0, on membranes of anionic and pH-sensitive liposomes comprised of DOPE-CHEMS, using energy dispersive X-ray diffraction (EDXD). At pH 7.4, the Am-β-CD/DNA complex induced the appearance of lamellar and hexagonal phases of DOPE. However, at pH 5.0, only non-lamellar phases could be observed. The presence of biological components led to a disruption of lipid order, but the pH-sensitivity of liposomes was maintained.

Conducting oxide formation and mechanical endurance of potential solid-oxide fuel cell interconnects in coal syngas environment

NASA Astrophysics Data System (ADS)

Liu, Kejia; Luo, Junhang; Johnson, Chris; Liu, Xingbo; Yang, J.; Mao, Scott X.

The oxidation properties of potential SOFCs materials Crofer 22 APU, Ebrite and Haynes 230 exposed in coal syngas at 800 °C for 100 h were studied. The phases and surface morphology of the oxide scales were characterized by X-ray diffraction, scanning electron microscopy and energy-dispersive X-ray analysis (EDX). The mechanical endurance and electrical resistance of the conducting oxides were characterized by indentation and electrical impedance, respectively. It was found that the syngas exposure caused the alloys to form porous oxide scales, which increased the electrical resistant and decreased the mechanical stability. As for short-term exposure in syngas, neither carbide nor metal dusting was found in the scales of all samples.

Mirrorlike pulsed laser deposited tungsten thin film.

PubMed

Mostako, A T T; Rao, C V S; Khare, Alika

2011-01-01

Mirrorlike tungsten thin films on stainless steel substrate deposited via pulsed laser deposition technique in vacuum (10(-5) Torr) is reported, which may find direct application as first mirror in fusion devices. The crystal structure of tungsten film is analyzed using x-ray diffraction pattern, surface morphology of the tungsten films is studied with scanning electron microscope and atomic force microscope. The film composition is identified using energy dispersive x-ray. The specular and diffuse reflectivities with respect to stainless steel substrate of the tungsten films are recorded with FTIR spectra. The thickness and the optical quality of pulsed laser deposition deposited films are tested via interferometric technique. The reflectivity is approaching about that of the bulk for the tungsten film of thickness ∼782 nm.

Effect of annealing temperature on titania nanoparticles

DOE Office of Scientific and Technical Information (OSTI.GOV)

Manikandan, K., E-mail: sanjaymani367@gmail.com; Arumugam, S., E-mail: sanjaymani367@gmail.com; Chandrasekaran, G.

2014-04-24

Titania polycrystalline samples are prepared by using sol-gel route hydrolyzing a alkoxide titanium precursor under acidic conditions. The as prepared samples are treated with different calcination temperatures. The anatase phase of titania forms when treated below 600°C, above that temperature the anatase phase tends to transform into the rutile phase of titania. The experimental determination of average grain size, phase formation, lattice parameters and the crystal structures of titania samples at different calcinations is done using X-ray diffraction (XRD). Fourier Transform Infra-red Spectroscopy (FTIR), UV-vis-NIR spectroscopy and Scanning Electron Microscopy (SEM) and Energy Dispersive Analysis X-ray are used to characterizemore » the samples to bring impact on the respective properties.« less

Electrochemical Study of Cobalt in Urea and Choline Chloride

NASA Astrophysics Data System (ADS)

Li, Min; Shi, Zhongning; Wang, Zhaowen; Reddy, Ramana G.

The nucleation mechanism of Co(II) in urea-choline chloride-CoCl2 melt at 373 K was studied using chronoamperometry. Chronoamperometry experiments confirm that the electrodeposition of cobalt on tungsten electrode is governed by three-dimensional (3D) progressive nucleation and diffusion-controlled growth mechanisms. The average diffusion coefficient of Co(II) in the melt at 373 K is 1.1 × 10-6 cm2 s-1, which is in good agreement with the estimated value obtained from cyclic voltammetry data. Characterization of the Co electrodeposit using scanning electron microscope (SEM), energy-dispersive spectroscopy (EDS), and X-ray diffraction (XRD) techniques indicate that the electrodeposit obtained at -0.75 V and 373 K contain dense and compact surface formed from pure cobalt metal.

Impact of physical and chemical parameters on the hydroxyapatite nanopowder synthesized by chemical precipitation method

NASA Astrophysics Data System (ADS)

Thu Trang Pham, Thi; Phuong Nguyen, Thu; Pham, Thi Nam; Phuong Vu, Thi; Tran, Dai Lam; Thai, Hoang; Thanh Dinh, Thi Mai

2013-09-01

In this paper, the synthesis of hydroxyapatite (HAp) nanopowder was studied by chemical precipitation method at different values of reaction temperature, settling time, Ca/P ratio, calcination temperature, (NH4)2HPO4 addition rate, initial concentration of Ca(NO3)2 and (NH4)2HPO4. Analysis results of properties, morphology, structure of HAp powder from infrared (IR) spectra, x-ray diffraction (XRD), energy dispersive x-ray (EDX) spectra and scanning electron microscopy (SEM) indicated that the synthesized HAp powder had cylinder crystal shape with size less than 100 nm, single-phase structure. The variation of the synthesis conditions did not affect the morphology but affected the size of HAp crystals.

Superhydrophobic coatings on wood substrate for self-cleaning and EMI shielding

NASA Astrophysics Data System (ADS)

Xing, Yingjie; Xue, Yaping; Song, Jinlong; Sun, Yankui; Huang, Liu; Liu, Xin; Sun, Jing

2018-04-01

A layer of superhydrophobic coating having good electromagnetic shielding and self-cleaning performance was fabricated on a wood surface through an electroless copper plated process. The superhydrophobic property of the wood surface was measured by contact angle (CA) and roll-off angle (RA) measurements. The microstructure and chemical composition of the superhydrophobic coating were analyzed by scanning electron microscopy (SEM), energy dispersive spectrometer (EDS) and X-ray diffraction (XRD). The analysis revealed that the microscale particles were uniformly distributed on the wood surface and the main component of the coating is metallic copper. The as-prepared Cu coatings on wood substrate exhibit a good superhydrophobicity with water contact angle about 160° and rolling angle less than 5°.

National Synchrotron Light Source annual report 1991. Volume 1, October 1, 1990--September 30, 1991

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hulbert, S.L.; Lazarz, N.M.

1992-04-01

This report discusses the following research conducted at NSLS: atomic and molecular science; energy dispersive diffraction; lithography, microscopy and tomography; nuclear physics; UV photoemission and surface science; x-ray absorption spectroscopy; x-ray scattering and crystallography; x-ray topography; workshop on surface structure; workshop on electronic and chemical phenomena at surfaces; workshop on imaging; UV FEL machine reviews; VUV machine operations; VUV beamline operations; VUV storage ring parameters; x-ray machine operations; x-ray beamline operations; x-ray storage ring parameters; superconducting x-ray lithography source; SXLS storage ring parameters; the accelerator test facility; proposed UV-FEL user facility at the NSLS; global orbit feedback systems; and NSLSmore » computer system.« less

Core-pumped mode-locked ytterbium-doped fiber laser operating around 980 nm

NASA Astrophysics Data System (ADS)

Zhou, Yue; Dai, Yitang; Li, Jianqiang; Yin, Feifei; Dai, Jian; Zhang, Tian; Xu, Kun

2018-07-01

In this letter, we first demonstrate a core-pumped passively mode-locked all-normal-dispersion ytterbium-doped fiber oscillator based on nonlinear polarization evolution operating around 980 nm. The dissipative soliton fiber laser pulse can be compressed down to 250 fs with 1 nJ pulse energy, and the slope efficiency of the oscillator can be as high as 19%. To improve the dissipative soliton laser output spectrum smoothness, we replace the birefringent plate based intracavity filter with a diffraction-grating based filter. The output pulse duration can then be further compressed down to 180 fs with improved spectral-smoothness. These schemes have potential applications in seeding cryogenic Yb:YLF amplifiers and underwater exploration of marine resources.

An ultrahigh pressure homogenization technique for easily exfoliating few-layer phosphorene from bulk black phosphorus

NASA Astrophysics Data System (ADS)

Guan, Qing-Qing; Zhou, Hua-Jing; Ning, Ping; Lian, Pei-Chao; Wang, Bo; He, Liang; Chai, Xin-Sheng

2018-05-01

We have developed an easy and efficient method for exfoliating few-layer sheets of black phosphorus (BP) in N-methyl-2-pyrrolidone, using ultra-high pressure homogenization (UPH). The BP was first exfoliated into sheets that were a few atomic layers thick, using a homogenizer for only 30 min. Next, a double centrifugation procedure was used to separate the material into few-layer nanosheets that were examined by X-ray diffraction, atomic force microscopy (AFM), transmission electron microscopy (TEM), high-angle annular dark field scanning transmission electron microscopy (HAADF-STEM), and energy-dispersive X-ray (EDX) spectroscopy. The results show that the products are specimens of phosphorene that are only a few-layer thick.

Optical properties of ZnO powder prepared by using a proteic sol-gel process

NASA Astrophysics Data System (ADS)

Kwon, Bong-Joon; Woo, Hyun-Joo; Park, Ji-Yeon; Jang, Kiwan; Lim, Seung-Hyuk; Cho, Yong-Hoon

2013-03-01

We have studied the optical properties of ZnO powder synthesized by using a proteic sol-gel process with coconut water as the precursor. The energy dispersive X-ray spectrometer and X-ray diffraction results show high purity of the synthesized ZnO powder. From the low-temperature (12 K) and power-dependent PL spectra, the donor-bound exciton, the acceptor-bound exciton, the donor-to-acceptor pair (DAP), and the phonon-replica of the DAP transition have been observed at 3.38, 3.34, 3.26, and 3.19 eV, respectively. The free exciton emission (˜3.3 eV) is also observed at 300 K in the temperature-dependent PL spectra.

Cobalt coated substrate for matrix-free analysis of small molecules by laser desorption/ionization mass spectrometry

NASA Astrophysics Data System (ADS)

Yalcin, Talat; Li, Liang

2009-12-01

Small molecule analysis is one of the most challenging issues in matrix-assisted laser desorption/ionization (MALDI) mass spectrometry. We have developed a cobalt coated substrate as a target for matrix-free analysis of small molecules in laser desorption/ionization mass spectrometry. Cobalt coating of 60-70 nm thickness has been characterized by scanning electron microscopy, energy dispersive X-ray analysis, X-ray diffraction, and laser induced breakdown spectroscopy. This target facilitates hundreds of samples to be spotted and analyzed without mixing any matrices, in a very short time. This can save a lot of time and money and can be a very practical approach for the analysis of small molecules by laser desorption/ionization mass spectrometry.

Nanocrystalline hydroxyapatite doped with selenium oxyanions: a new material for potential biomedical applications.

PubMed

Kolmas, Joanna; Oledzka, Ewa; Sobczak, Marcin; Nałęcz-Jawecki, Grzegorz

2014-06-01

Selenium-substituted hydroxyapatites containing selenate SeO4(2-) or selenite SeO3(2-) ions were synthesized using a wet precipitation method. The selenium content was determined by atomic absorbance spectrometry. The raw, unsintered powders were also characterized using powder X-ray diffraction, middle-range FT-IR spectroscopy and transmission electron microscopy with energy-dispersive X-ray spectroscopic microanalysis. The synthesized apatites were found to be pure and nanocrystalline with a crystal size similar to that in bone mineral. The incorporation of selenium oxyanions into the crystal lattice was confirmed. The toxicity of hydroxyapatites containing selenite or selenate ions was evaluated with a protozoan assay and bacterial luminescence test. Copyright © 2014 Elsevier B.V. All rights reserved.

Multi-element germanium detectors for synchrotron applications

DOE Office of Scientific and Technical Information (OSTI.GOV)

Rumaiz, A. K.; Kuczewski, A. J.; Mead, J.

In this paper, we have developed a series of monolithic multi-element germanium detectors, based on sensor arrays produced by the Forschungzentrum Julich, and on Application-specific integrated circuits (ASICs) developed at Brookhaven. Devices have been made with element counts ranging from 64 to 384. These detectors are being used at NSLS-II and APS for a range of diffraction experiments, both monochromatic and energy-dispersive. Compact and powerful readout systems have been developed, based on the new generation of FPGA system-on-chip devices, which provide closely coupled multi-core processors embedded in large gate arrays. Finally, we will discuss the technical details of the systems,more » and present some of the results from them.« less

Structural, electrical and photovoltaic properties of CoS/Si heterojunction prepared by spray pyrolysis

NASA Astrophysics Data System (ADS)

El Radaf, I. M.; Nasr, Mahmoud; Mansour, A. M.

2018-01-01

Au/p-CoS/n-Si/Al heterojunction device was fabricated by spray pyrolysis technique. The structural and morphological features were examined by x-ray diffraction, scanning electron microscope and energy dispersive x-ray analysis. The capacitance-voltage characteristics of the prepared heterojunction were analyzed at room temperature in the dark. The current-voltage characteristics were examined under dark and different incident light intensities 20-100 mW cm-2. The rectification ratio, series resistance, shunt resistance, diode ideality factor and the effective barrier height were determined at dark and illumination conditions. The photovoltaic parameters such as short circuit current density, open circuit voltage, fill factor and power conversion efficiency were calculated at different incident light intensities.

Structural characterization of a new lipid/DNA complex showing a selective transfection efficiency in ovarian cancer cells

NASA Astrophysics Data System (ADS)

Caracciolo, G.; Pozzi, D.; Caminiti, R.; Congiu Castellano, A.

2003-04-01

We investigated, for the first time, by using Energy Dispersive X-ray Diffraction, the structure of a new ternary cationic liposome formulated with dioleoyl trimethylammonium propane (DOTAP), 1,2-dioleoyl-3-phosphatidylethanolamine (DOPE) and cholesterol (Chol) (DDC) which has been recently found to have a selective high gene transfer ability in ovarian cancer cells. Our structural results provide a further experimental support to the widely accepted statement that there is not a simple and direct correlation between structure and transfection efficiency and that the factors controlling cationic lipid/DNA (CL-DNA) complexes-mediated gene transfer depend not only on the formulations of the cationic liposomes and their thermodynamic phase, but also significantly on the cell properties.

High pressure high temperature devitrification of Fe78B13Si9 metallic glass with simultaneous x-ray structural characterization

NASA Astrophysics Data System (ADS)

Stemshorn, Andrew K.; Vohra, Yogesh K.; Smith, Spencer J.

2018-06-01

Changes in bulk crystallization behavior following devitrification at high pressure are investigated for a Fe78B13Si9 composition metallic glass using in-situ energy dispersive x-ray powder diffraction. Crystallization with time was evaluated for a series of measurements to a maximum pressure of 5.63 ± 0.15 GPa for the Fe78B13Si9 glass. Pressure was found to strongly affect onset bulk crystallization temperature Tx. Crystallization at each pressure was found to progress in two stages. In the first stage, α-Fe precipitates and in the second Fe2B forms while α-Fe continues to crystallize. Complementary high pressure room temperature studies were conducted.

Properties of magnetic iron oxides used as materials for wastewater treatment

NASA Astrophysics Data System (ADS)

Matei, E.; Predescu, A.; Vasile, E.; Predescu, A.

2011-07-01

The paper describes the properties of some nanopowders obtained by coprecipitation and used as adsorbent for wastewater treatment. The Fe3O4 and γ-Fe2O3 nanopowders were obtained using iron salts and NaOH as precipitation agents. D-sorbitol was used to prevent the agglomeration between the nanoparticles. The particle size and distribution were detected using a transmission electron microscopy (TEM) and a scanning electron microscope (SEM) equipped with dispersive analyze system in X radiation energy (EDS). The structure of the iron oxide nanoparticles was characterized by X-ray powder diffraction. Thus, the nanoparticles were characterized and compare in terms of particle size and chemical composition and used for adsorption studies in order to removal hexavalent chromium from waste waters.

A novel ultrasonication method in the preparation of zirconium impregnated cellulose for effective fluoride adsorption.

PubMed

Barathi, M; Kumar, A Santhana Krishna; Rajesh, N

2014-05-01

In the present work, we propose for the first time a novel ultrasound assisted methodology involving the impregnation of zirconium in a cellulose matrix. Fluoride from aqueous solution interacts with the cellulose hydroxyl groups and the cationic zirconium hydroxide. Ultrasonication ensures a green and quick alternative to the conventional time intensive method of preparation. The effectiveness of this process was confirmed by comprehensive characterization of zirconium impregnated cellulose (ZrIC) adsorbent using Fourier transform infrared spectroscopy (FT-IR), energy dispersive X-ray spectrometry (EDX) and X-ray diffraction (XRD) studies. The study of various adsorption isotherm models, kinetics and thermodynamics of the interaction validated the method. Copyright © 2013 Elsevier B.V. All rights reserved.

Crystallography and Morphology of MC Carbides in Niobium-Titanium Modified As-Cast HP Alloys

NASA Astrophysics Data System (ADS)

Buchanan, Karl G.; Kral, Milo V.; Bishop, Catherine M.

2014-07-01

The microstructures of two as-cast heats of HP alloy stainless steels modified with niobium and titanium were examined with particular attention paid to the interdendritic niobium-titanium-rich carbides formed during solidification of these alloys. Generally, these precipitates obtain a blocky morphology in the as-cast condition. However, the (NbTi)C precipitates may obtain a nodular morphology. To provide further insight to the origin of the two different morphologies obtained by the (NbTi)C precipitates in the HP-NbTi alloy, the microstructure and crystallography of each have been studied in detail using scanning electron microscopy, transmission electron microscopy, various electron diffraction methods (EBSD, SAD, and CBED), and energy-dispersive X-ray spectroscopy.