Analysis of synthetic diamond single crystals by X-ray topography and double-crystal diffractometry

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

Prokhorov, I. A., E-mail: igor.prokhorov@mail.ru; Ralchenko, V. G.; Bolshakov, A. P.

2013-12-15

Structural features of diamond single crystals synthesized under high pressure and homoepitaxial films grown by chemical vapor deposition (CVD) have been analyzed by double-crystal X-ray diffractometry and topography. The conditions of a diffraction analysis of diamond crystals using Ge monochromators have been optimized. The main structural defects (dislocations, stacking faults, growth striations, second-phase inclusions, etc.) formed during crystal growth have been revealed. The nitrogen concentration in high-pressure/high-temperature (HPHT) diamond substrates is estimated based on X-ray diffraction data. The formation of dislocation bundles at the film-substrate interface in the epitaxial structures has been revealed by plane-wave topography; these dislocations are likelymore » due to the relaxation of elastic macroscopic stresses caused by the lattice mismatch between the substrate and film. The critical thicknesses of plastic relaxation onset in CVD diamond films are calculated. The experimental techniques for studying the real diamond structure in optimizing crystal-growth technology are proven to be highly efficient.« less

p-type zinc-blende GaN on GaAs substrates

NASA Astrophysics Data System (ADS)

Lin, M. E.; Xue, G.; Zhou, G. L.; Greene, J. E.; Morkoç, H.

1993-08-01

We report p-type cubic GaN. The Mg-doped layers were grown on vicinal (100) GaAs substrates by plasma-enhanced molecular beam epitaxy. Thermally sublimed Mg was, with N2 carrier gas, fed into an electron-cyclotron resonance source. p-type zinc-blende-structure GaN films were achieved with hole mobilities as high as 39 cm2/V s at room temperature. The cubic nature of the films were confirmed by x-ray diffractometry. The depth profile of Mg was investigated by secondary ions mass spectroscopy.

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

Petrova, V. A.; Orekhov, A. S.; Chernyakov, D. D.

A method for preparing multilayer film composites based on chitosan has been developed by the example of polymer pairs: chitosan–hyaluronic acid, chitosan–alginic acid, and chitosan–carrageenan. The structure of the composite films is characterized by X-ray diffractometry and scanning electron microscopy. It is shown that the deposition of a solution of hyaluronic acid, alginic acid, or carrageenan on a chitosan gel film leads to the formation of a polyelectrolyte complex layer at the interface, which is accompanied by the ordering of chitosan chains in the surface region; the microstructure of this layer depends on the nature of contacting polymer pairs.

Purification Procedures for Single-Wall Carbon Nanotubes

NASA Technical Reports Server (NTRS)

Gorelik, Olga P.; Nikolaev, Pavel; Arepalli, Sivaram

2001-01-01

This report summarizes the comparison of a variety of procedures used to purify carbon nanotubes. Carbon nanotube material is produced by the arc process and laser oven process. Most of the procedures are tested using laser-grown, single-wall nanotube (SWNT) material. The material is characterized at each step of the purification procedures by using different techniques including scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), transmission electron microscopy (TEM), Raman, X-ray diffractometry (XRD), thermogravimetric analysis (TGA), nuclear magnetic resonance (NMR), and high-performance liquid chromatography (HPLC). The identified impurities are amorphous and graphitic carbon, catalyst particle aggregates, fullerenes, and hydrocarbons. Solvent extraction and low-temperature annealing are used to reduce the amount of volatile hydrocarbons and dissolve fullerenes. Metal catalysts and amorphous as well as graphitic carbon are oxidized by reflux in acids including HCl, HNO3 and HF and other oxidizers such as H2O2. High-temperature annealing in vacuum and in inert atmosphere helps to improve the quality of SWNTs by increasing crystallinity and reducing intercalation.

RF sputtered silicon and hafnium nitrides as applied to 440C steel

NASA Technical Reports Server (NTRS)

Grill, A.; Aron, P. R.

1984-01-01

Silicon nitride and hafnium nitride coatings were deposited on oxidized and unoxidized 440C stainless steel substrates. Sputtering was done in mixtures of argon and nitrogen gases from pressed powder silicon nitride and from hafnium metal targets. The coatings and the interface between the coating and substrate were investigated by X-ray diffractometry, scanning electron microscopy, energy dispersive X-ray analysis and Auger electron spectroscopy. Oxide was found at all interfaces with an interface width of at least 600 A for the oxidized substrates and at least 300 A for the unoxidized substrates. Scratch test results demonstrate that the adhesion of hafnium nitride to both oxidized and unoxidized 440C is superior to that of silicon nitride. Oxidized 440C is found to have increased adhesion, to both nitrides, over that of unoxidized 440C. Coatings of both nitrides deposited at 8 mtorr were found to have increased adhesion to both oxidized and unoxidized 440C over those deposited at 20 mtorr.

Enhancement of valve metal osteoconductivity by one-step hydrothermal treatment.

PubMed

Zuldesmi, Mansjur; Waki, Atsushi; Kuroda, Kensuke; Okido, Masazumi

2014-09-01

In this study, we produced super-hydrophilic surfaces of valve metals (Ti, Nb, Ta and Zr) by one-step hydrothermal treatment. Their surface characteristics and osteoconductivity using an in vivo test were then assessed. These data were compared with that of as-polished, as-anodized and both anodized+hydrothermally treated samples. Changes in surface chemistry, surface morphology and structure were investigated by X-ray photoelectron spectroscopy, scanning electron microscopy, and X-ray diffractometry. The results revealed that the water contact angles of valve metals were decreased by hydrothermal treatment and continued to reduce dramatically until lower than 10° after being immersed in phosphate buffered solution. By producing super-hydrophilic surfaces, the osteoconductivity of these hydrothermally treated valve metals was enhanced by up to 55%. Copyright © 2014 Elsevier B.V. All rights reserved.

Delaminating and restacking MgAl-layered double hydroxide monitored and characterized by a range of instrumental methods

NASA Astrophysics Data System (ADS)

Muráth, Szabolcs; Somosi, Zoltán; Tóth, Ildikó Y.; Tombácz, Etelka; Sipos, Pál; Pálinkó, István

2017-07-01

The delamination-restacking properties of MgAl-layered double hydroxide (MgAl-LDH) were studied in various solvents. The LDH samples were successfully delaminated in polar amides (formamide, N-methylformamide, N-methylacetamide). Usually, delamination was finalized by ultrasonic treatment. As rehydrating solutions, numerous Na-salts with single-, double- and triple-charged anions were used. Reconstruction was accomplished with anions of one or two negative charges, but triple-charged ones generally disrupted the rebuilding process, likely, because their salts with the metals of the LDH are very stable, and the thin layers can more readily transform to salts than the ordered materials. Samples and delamination-restacking processes were characterized by X-ray diffractometry (XRD), infrared spectroscopy (IR), dynamic light scattering (DLS), scanning electron microscopy (SEM) and energy-dispersive X-ray analysis (EDX).

Laser formation of titanium nitride films as a result of Ti coating modification in a nitrogen atmosphere

NASA Astrophysics Data System (ADS)

Eskin, Sergei

1998-12-01

Laser treatment of the 303 and 416 stainless steels with Ti precoating was studied. CW CO2 and UV ArF excimer lasers were used. The TiN films were formed at a treatment velocity of 0.5 to 3 - 5 cm/sec and a power density of CO2 laser at (3 - 5) 104 W/cm2. X-ray diffractometry, x-ray mapping and Auger electron spectroscopy techniques indicated a TiN phase on the surface with oxygen content 12 - 25 at%. The thickness of the TiN film was 0.3 - 0.4 micrometers after treatment of the 5 micrometers Ti coating and about 900 angstroms for the 0.3 micrometers coating. Some characteristics of TiN films were examined and features of the nitriding process are discussed.

New insight into the promoting role of process on the CeO₂-WO₃/TiO₂ catalyst for NO reduction with NH₃ at low-temperature.

PubMed

Zhang, Shule; Zhong, Qin; Shen, Yuge; Zhu, Li; Ding, Jie

2015-06-15

This study aimed at investigating the reason of high catalytic activity for CeO2-WO3/TiO2 catalyst from the aspects of WO3 interaction with other species and the NO oxidation process. Analysis by X-ray diffractometry, photoluminescence spectra, diffuse reflectance UV-visible, X-ray photoelectron spectroscopy, density functional theory calculations, electron paramagnetic resonance spectroscopy, temperature-programmed-desorption of NO and in situ diffuse reflectance infrared transform spectroscopy showed that WO3 could interact with CeO2 to improve the electron gaining capability of CeO2 species. In addition, WO3 species acted as electron donating groups to transfer the electrons to CeO2 species. The two aspects enhanced the formation of reduced CeO2 species to improve the formation of superoxide ions. Furthermore, the Ce species were the active sites for the NO adsorption and the superoxide ions over the catalyst needed oxidizing the adsorbed NO to improve the NO oxidation. This process was responsible for the high catalytic activity of CeO2-WO3/TiO2 catalyst. Copyright © 2015 Elsevier Inc. All rights reserved.

High Resolution X-Ray Diffraction of Macromolecules with Synchrotron Radiation

NASA Technical Reports Server (NTRS)

Stojanoff, Vivian; Boggon, Titus; Helliwell, John R.; Judge, Russell; Olczak, Alex; Snell, Edward H.; Siddons, D. Peter; Rose, M. Franklin (Technical Monitor)

2000-01-01

We recently combined synchrotron-based monochromatic X-ray diffraction topography methods with triple axis diffractometry and rocking curve measurements: high resolution X-ray diffraction imaging techniques, to better understand the quality of protein crystals. We discuss these methods in the light of results obtained on crystals grown under different conditions. These non destructive techniques are powerful tools in the characterization of the protein crystals and ultimately will allow to improve, develop, and understand protein crystal growth. High resolution X-ray diffraction imaging methods will be discussed in detail in light of recent results obtained on Hen Egg White Lysozyme crystals and other proteins.

Nonlinear refraction properties of nickel oxide thin films at 800 nm

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

Melo, Ronaldo P. Jr. de; Silva, Blenio J. P. da; Santos, Francisco Eroni P. dos

2009-11-01

Measurements of the nonlinear refractive index, n{sub 2}, of nickel oxide films prepared by controlled oxidation of nickel films deposited on substrates of soda-lime glass are reported. The structure and morphology of the samples were characterized by scanning electron microscopy, atomic force microscopy, and x-ray diffractometry. Samples of excellent optical quality were prepared. The nonlinear measurements were performed using the thermally managed eclipse Z-scan technique at 800 nm. A large value of n{sub 2}approx =10{sup -12} cm{sup 2}/W and negligible nonlinear absorption were obtained.

Synthesis and characterization of Ru-Ti[sub 4]O[sub 7] microelectrode arrays

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

He, L.; Franzen, H.F.; Vitt, J.E.

1994-04-01

A synthesis is described for Ru microelectrode arrays within a conductive Ti[sub 4]O[sub 7] ceramic matrix. Data obtained by X-ray diffractometry and scanning electron microscopy are consistent with the existence of heterogeneous mixtures of Ru particles (ca. 0.8 [mu]m diam) within the Ti[sub 4]O[sub 7] matrices. No mixed metal oxides or other new compounds are detected. Rotated disk electrodes (RDEs) constructed from the Ru-Ti[sub 4]O[sub 7] materials are compared on the basis of their voltammetric response for the oxidations of I[sup [minus

Functionalization of 2D macroporous silicon under the high-pressure oxidation

NASA Astrophysics Data System (ADS)

Karachevtseva, L.; Kartel, M.; Kladko, V.; Gudymenko, O.; Bo, Wang; Bratus, V.; Lytvynenko, O.; Onyshchenko, V.; Stronska, O.

2018-03-01

Addition functionalization after high-pressure oxidation of 2D macroporous silicon structures is evaluated. X-ray diffractometry indicates formation of orthorhombic SiO2 phase on macroporous silicon at oxide thickness of 800-1200 nm due to cylindrical symmetry of macropores and high thermal expansion coefficient of SiO2. Pb center concentration grows with the splitting energy of LO- and TO-phonons and SiO2 thickness in oxidized macroporous silicon structures. This increase EPR signal amplitude and GHz radiation absorption and is promising for development of high-frequency devices and electronically controlled elements.

Study on different characteristics of doped tri calcium phosphate at different sintering temperatures

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

Samanta, Sujan Krishna, E-mail: itssujan@rediffmail.com; Chanda, Abhijit, E-mail: abhijitchanda.biomed@gmail.com

2016-04-13

Pure β-tricalcium phosphate (β-TCP), Zn-doped (3wt %) β-TCP and Mg- doped (3wt %) β-TCP samples were prepared by using a wet chemical precipitation synthesis technique, followed by calcination at 800 °C in air. The developed materials were subjected to sintering at different temperatures. Density and porosity were compared. The X-ray diffractometry (XRD) and Fourier-transformed infrared (FTIR) spectrometer were used to examine the changes in crystalline phases and presence of functional groups of TCP ceramics. The scanning electron microscopy (SEM) was used to study the pore formation, pore size, grain size.

Structure of chitosan gels mineralized by sorption

NASA Astrophysics Data System (ADS)

Modrzejewska, Z.; Skwarczyńska, A.; Douglas, T. E. L.; Biniaś, D.; Maniukiewicz, W.; Sielski, J.

2015-10-01

The paper presents the structural studies of mineralized chitosan hydrogels. Hydrogels produced by using sodium beta-glycerophosphate (Na-β-GP) as a neutralizing agent. Mineralization was performed method "post loading", which consisted in sorption to the gels structure Ca ions. In order to obtain - in the structure of gels - compounds similar to the hydroxyapatites present naturally in bone tissue, gels after sorption were modified in: pH 7 buffer and sodium hydrogen phosphate. In order to determine the structural properties of the gels, the following methods were used: infrared spectroscopy with Fourier transformation, FTIR, X-ray diffractometry, XRD, scanning electron microscopy, SEM.

Effects of fines content on hydraulic conductivity and morphology of laterite soil as hydraulic barrier

NASA Astrophysics Data System (ADS)

Bello Yamusa, Yamusa; Yunus, Nor Zurairahetty Mohd; Ahmad, Kamarudin; Rahman, Norhan Abd; Sa'ari, Radzuan

2018-03-01

Laterite soil was investigated to find out the effects of fines content and to identify the micro-structural and molecular characteristics to evaluate its potentiality as a compacted soil landfill liner material. Tests were carried out on natural soil and reconstituted soil by dry weight of soil samples to determine the physical and engineering properties of the soil. All tests were carried out on the samples by adopting the British Standard 1377:1990. The possible mechanisms that contributed to the clay mineralogy were analyzed using spectroscopic and microscopic techniques such as field emission scanning electron microscopy (FESEM), energy-dispersive X-ray (EDX) and X-ray diffractometry (XRD). The laterite soil was found to contain kaolinite as the major clay minerals. A minimum of 50% fines content of laterite soil met the required result for hydraulic barriers in waste containment facilities.

Observing Graphene Grow: Catalyst–Graphene Interactions during Scalable Graphene Growth on Polycrystalline Copper

PubMed Central

2013-01-01

Complementary in situ X-ray photoelectron spectroscopy (XPS), X-ray diffractometry, and environmental scanning electron microscopy are used to fingerprint the entire graphene chemical vapor deposition process on technologically important polycrystalline Cu catalysts to address the current lack of understanding of the underlying fundamental growth mechanisms and catalyst interactions. Graphene forms directly on metallic Cu during the high-temperature hydrocarbon exposure, whereby an upshift in the binding energies of the corresponding C1s XPS core level signatures is indicative of coupling between the Cu catalyst and the growing graphene. Minor carbon uptake into Cu can under certain conditions manifest itself as carbon precipitation upon cooling. Postgrowth, ambient air exposure even at room temperature decouples the graphene from Cu by (reversible) oxygen intercalation. The importance of these dynamic interactions is discussed for graphene growth, processing, and device integration. PMID:24041311

The ceramics of Malpaís of Zacapu, Michoacán, Mexico, during the Early and Middle Postclassic periods (900-1450 AD): Micro-chemical characterization of surface paintings

NASA Astrophysics Data System (ADS)

Jadot, E.; Schiavon, N.; Manso, M.

2016-05-01

Tarascan ceramic sherds from two Postclassical archaeological sites (900-1450 AD) at the Malpaís of Zacapu, Michoacán, Mexico, were investigated by combining Back-Scattered Scanning Electron Microscopy and Energy Dispersive Spectroscopy (BSEM-EDS), μ-X-Ray Diffractometry (μ-XRD), μ-X-ray Fluorescence Spectroscopy (μ-XRF) and μ-Raman Spectroscopy. These sherds are famous for their forms and decorations although the composition of its raw materials remains so far unknown and focused only on the composition of the ceramic paste. For the purpose of surface decoration characterization, the pigments used in slips and paintings were identified as hematite, magnetite, amorphous carbon, graphite and lignite. Furthermore chemical and molecular structure determination allowed the identification of technological aspects such as the firing temperatures and atmospheres used in ceramics production.

Atomic Layer Deposition of Rhenium Disulfide.

PubMed

Hämäläinen, Jani; Mattinen, Miika; Mizohata, Kenichiro; Meinander, Kristoffer; Vehkamäki, Marko; Räisänen, Jyrki; Ritala, Mikko; Leskelä, Markku

2018-06-01

2D materials research is advancing rapidly as various new "beyond graphene" materials are fabricated, their properties studied, and materials tested in various applications. Rhenium disulfide is one of the 2D transition metal dichalcogenides that has recently shown to possess extraordinary properties such as that it is not limited by the strict monolayer thickness requirements. The unique inherent decoupling of monolayers in ReS 2 combined with a direct bandgap and highly anisotropic properties makes ReS 2 one of the most interesting 2D materials for a plethora of applications. Here, a highly controllable and precise atomic layer deposition (ALD) technique is applied to deposit ReS 2 thin films. Film growth is demonstrated on large area (5 cm × 5 cm) substrates at moderate deposition temperatures between 120 and 500 °C, and the films are extensively characterized using field emission scanning electron microscopy/energy-dispersive X-ray spectroscopy, X-ray diffractometry using grazing incidence, atomic force microscopy, focused ion beam/transmission electron microscopy, X-ray photoelectron spectroscopy, and time-of-flight elastic recoil detection analysis techniques. The developed ReS 2 ALD process highlights the potential of the material for applications beyond planar structure architectures. The ALD process also offers a route to an upgrade to an industrial scale. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Structural, Optical and Electrical Properties of ITO Thin Films

NASA Astrophysics Data System (ADS)

Sofi, A. H.; Shah, M. A.; Asokan, K.

2018-02-01

Transparent and conductive thin films of indium tin oxide were fabricated on glass substrates by the thermal evaporation technique. Tin doped indium ingots with low tin content were evaporated in vacuum (1.33 × 10-7 kpa) followed by an oxidation for 15 min in the atmosphere in the temperature range of 600-700°C. The structure and phase purity, surface morphology, optical and electrical properties of thin films were studied by x-ray diffractometry and Raman spectroscopy, scanning electron microcopy and atomic force microscopy, UV-visible spectrometry and Hall measurements in the van der Pauw configuration. The x-ray diffraction study showed the formation of the cubical phase of polycrystalline thin films. The morphological analysis showed the formation of ginger like structures and the energy dispersive x-ray spectrum confirmed the presence of indium (In), tin (Sn) and oxygen (O) elements. Hall measurements confirmed n-type conductivity of films with low electrical resistivity ( ρ) ˜ 10-3 Ω cm and high carrier concentration ( n) ˜ 1020 cm-3. For prevalent scattering mechanisms in the films, experimental data was analyzed by calculating a mean free path ( L) using a highly degenerate electron gas model. Furthermore, to investigate the performance of the deposited films as a transparent conductive material, the optical figure of merit was obtained for all the samples.

Synthesis and Characterization of Cobalt Substituted Zinc Ferrite Nanoparticles by Microwave Combustion Method.

PubMed

Sundararajan, M; Kennedy, L John; Vijaya, J Judith

2015-09-01

Pure and cobalt doped zinc ferrites were prepared by microwave combustion method using L-arginine as a fuel. The prepared samples were characterized by various instrumental techniques such as X-ray powder diffractometry, high resolution scanning electron microscopy (HR-SEM), energy dispersive X-ray analysis, Fourier transformed infrared (FT-IR) spectroscopy, photoluminescence spectroscopy and UV-Visible diffuse reflectance spectroscopy. Vibrating sample magnetometry at room temperature was recorded to study the magnetic behavior of the samples. X-ray analysis confirmed the formation of zinc ferrites normal spinel-type structure with an average crystallite sizes in the range, 25.69 nm to 35.68 nm. The lattice parameters decreased as cobalt fraction was increased. The HR-SEM images showed nanoparticles are agglomerated. The estimated band gap energy value was found to decrease with an increase in cobalt content (1.87 to 1.62 eV). Broad visible emissions are observed in the photoluminescence spectra. A gradual increase in the coercivity and saturation magnetization (M(s)) were noted at relatively higher cobalt doping fractions.

From nicotinate-containing layered double hydroxides (LDHs) to NAD coenzyme-LDH nanocomposites - Syntheses and structural characterization by various spectroscopic methods

NASA Astrophysics Data System (ADS)

Muráth, Szabolcs; Dudás, Csilla; Kukovecz, Ákos; Kónya, Zoltán; Sipos, Pál; Pálinkó, István

2017-07-01

The syntheses of nicotinate anion- and NAD coenzyme-layered double hydroxide (LDH) composites were performed with the aim of having the organic component among the layers. In-house prepared CaAl-LDHs were the host materials. Intercalation was attempted by direct ion exchange or by the dehydration-rehydration method applying aqueous solvent mixtures (containing ethanol, propanol, acetone, N,N-dimethylformamide). For structural characterization, beside X-ray diffractometry, X-ray photoelectron and IR spectroscopies, transmission and scanning electron microscopies as well as energy-dispersive X-ray analysis were used. Molecular modelling served for the visualization of the arrangements of the intercalated ions among the layers of the LDH samples. Although not all the intercalation methods and solvent mixtures led to intercalated composite materials, successful ones could be identified. The combination of spectroscopic methods helped in proposing sensible spatial arrangements for the intercalated anions. The NAD-CaAl-LDH composite proved to be an active catalyst in the oxidation of hydroquinone to 1,4-bezoquinoe in the presence of H2O2.

Effect of intrinsic electronic defect states on the morphology and optoelectronic properties of Sn-rich SnS particles

NASA Astrophysics Data System (ADS)

Singh, Chetan C.; Panda, Emila

2018-05-01

A small variation in the elemental composition of a chemical compound can cause the formation of additional electronic defect states in the material, thereby altering the overall microstructure and thus induced properties. In this work, we observed chemical constitution-induced modification in the morphology and optoelectronic properties of SnS. To this end, SnS particles were prepared using the solution chemical route and were characterized using a wide range of experimental techniques, such as x-ray diffractometry, field emission scanning electron microscopy, high resolution transmission electron microscopy, energy dispersive spectroscopy (EDS), x-ray photoelectron spectroscopy (XPS), UV-Vis spectrophotometry, and scanning tunneling spectroscopy (STS). All these SnS particles are found to be Sn-rich and p-type. However, distinctly different morphologies (i.e., flower-like and aggregated ones) are observed. These are then correlated with the electronic defect states, which are induced because of the presence of Sn vacancies, Sn antisites, and/or Sn interstitials. A combination of EDS, XPS, and STS data confirmed the presence of a higher concentration of Sn vacancies along with lower quantities of Sn interstitials and/or antisites in the SnS particles with flower-like morphologies giving rise to higher hole concentration, which subsequently leads to reduced transport, optical band gaps, and barrier heights.

Energy dispersive X-ray fluorescence spectroscopy/Monte Carlo simulation approach for the non-destructive analysis of corrosion patina-bearing alloys in archaeological bronzes: The case of the bowl from the Fareleira 3 site (Vidigueira, South Portugal)

NASA Astrophysics Data System (ADS)

Bottaini, C.; Mirão, J.; Figuereido, M.; Candeias, A.; Brunetti, A.; Schiavon, N.

2015-01-01

Energy dispersive X-ray fluorescence (EDXRF) is a well-known technique for non-destructive and in situ analysis of archaeological artifacts both in terms of the qualitative and quantitative elemental composition because of its rapidity and non-destructiveness. In this study EDXRF and realistic Monte Carlo simulation using the X-ray Monte Carlo (XRMC) code package have been combined to characterize a Cu-based bowl from the Iron Age burial from Fareleira 3 (Southern Portugal). The artifact displays a multilayered structure made up of three distinct layers: a) alloy substrate; b) green oxidized corrosion patina; and c) brownish carbonate soil-derived crust. To assess the reliability of Monte Carlo simulation in reproducing the composition of the bulk metal of the objects without recurring to potentially damaging patina's and crust's removal, portable EDXRF analysis was performed on cleaned and patina/crust coated areas of the artifact. Patina has been characterized by micro X-ray Diffractometry (μXRD) and Back-Scattered Scanning Electron Microscopy + Energy Dispersive Spectroscopy (BSEM + EDS). Results indicate that the EDXRF/Monte Carlo protocol is well suited when a two-layered model is considered, whereas in areas where the patina + crust surface coating is too thick, X-rays from the alloy substrate are not able to exit the sample.

Synthesis of Single Crystalline ZnO Nanoparticles by Salt-Assisted Spray Pyrolysis

NASA Astrophysics Data System (ADS)

Panatarani, Camellia; Lenggoro, I. Wuled; Okuyama, Kikuo

2003-04-01

LiNO3 was used as a shield in the preparation of single crystalline ZnO particles by a spray pyrolysis process in order to prevent agglomeration and enhance the crystallinity of the ZnO. LiNO3 was added to a precursor solution of zinc acetate dihydrate prior to its atomization by means of an ultrasonic transducer. Agglomerate-free particles having a mean particle size of 26 nm were successfully obtained after washing the product. X-ray diffractometry, field-emission scanning electron micrograph and transmission electron micrograph data indicate that the size and morphology of ZnO were strongly influenced by the operating temperature used and the residence time of the particle in the reactor.

Thickness dependence of the exchange bias in epitaxial manganite bilayers

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

Kobrinskii, A. L.; Goldman, A. M.; Varela del Arco, Maria

Exchange bias has been studied in a series of La{sub 2/3}Ca{sub 1/3}MnO{sub 3}/La{sub 1/3}Ca{sub 2/3}MnO{sub 3} bilayers grown on (001) SrTiO{sub 3} substrates by ozone-assisted molecular-beam epitaxy. The high crystalline quality of the samples and interfaces has been verified using high-resolution x-ray diffractometry and Z-contrast scanning transmission electron microscopy with electron-energy-loss spectroscopy. The dependence of exchange bias on the thickness of the antiferromagnetic layer has been investigated. A critical value for the onset of the hysteresis loop shift has been determined. An antiferromagnetic anisotropy constant has been obtained by fitting the results to the generalized Meiklejohn-Bean model.

Electric property measurement of free-standing SrTiO3 nanoparticles assembled by dielectrophoresis

NASA Astrophysics Data System (ADS)

Budiman, Faisal; Kotooka, Takumi; Horibe, Yoichi; Eguchi, Masanori; Tanaka, Hirofumi

2018-06-01

Free-standing strontium titanate (SrTiO3/STO) nanoparticles (NPs) were synthesized by the sol–gel method. X-ray diffractometry revealed that the required minimum annealing temperature to synthesize pure and highly crystalline STO NPs was 500 °C. Moreover, morphological observation by field emission scanning electron microscopy showed that the STO NPs have a spherical structure and their size depended on annealing condition. Electrical properties were measured using a low-temperature probing system. Here, an electrode was fabricated by electron beam lithography and the synthesized STO NPs were aligned at the electrodes by dielectrophoresis. The conductance of a sample was proportional to temperature. Two conduction mechanisms originating from hopping and tunneling appeared in the Arrhenius plot.

Ultrastructure of selected struvite-containing urinary calculi from cats.

PubMed

Neumann, R D; Ruby, A L; Ling, G V; Schiffman, P S; Johnson, D L

1996-01-01

To elucidate the ultrastructural details of struvite-containing urinary calculi from cats. Specimens studied were inclusive of the range of textures visible during preliminary analysis by use of a stereoscopic dissecting microscope. Textural types, which were used to infer crystal growth conditions, were differentiated with regard to crystal habit, crystal size, growth orientation, and primary porosity. Thirty specimens were selected from a collection of approximately 1,600 feline urinary calculi: 20 of these were composed entirely of struvite, and 10 consisted of struvite and calcium phosphate (apatite). Qualitative and quantitative analyses of specimens included use of plain and polarized light microscopy, x-ray diffractometry, scanning electron microscopy with backscattered electron imagery, x-ray fluorescence scans, and electron probe microanalysis. Four textural types were recognized among struvite calculi, whereas 2 textural types of struvite-apatite calculi were described. The presence of minute, well interconnected primary pores in struvite-containing urinary calculi from cats is an important feature, which may promote possible interaction of calculi with changes in urine composition. Primary porosity, which can facilitate interaction between the calculus and changing urine composition, may explain the efficacy of dietary or medicinal manipulations to promote the dissolution of struvite-containing uroliths from this species.

Capacity fading of LiAlyNi1-x-yCoxO2 cathode for lithium-ion batteries during accelerated calendar and cycle life tests (effect of depth of discharge in charge-discharge cycling on the suppression of the micro-crack generation of LiAlyNi1-x-yCoxO2 particle)

NASA Astrophysics Data System (ADS)

Watanabe, Shoichiro; Kinoshita, Masahiro; Hosokawa, Takashi; Morigaki, Kenichi; Nakura, Kensuke

2014-08-01

Cycle performance of a LiAl0.10Ni0.76Co0.14O2 (NCA) cathode/graphite cell closely depended on the range of depth of discharge in charge-discharge processes (ΔDOD). When ΔDOD was 10-70%, cycle performance at 25 °C was maintained even at 60 °C. Deterioration phenomena were analyzed by electrochemical method, X-ray photoelectron spectroscopy (XPS), X-ray diffractometry (XRD), and micro-cracks in NCA particles were analyzed with cross-sectional views by scanning electron microscopy (SEM). Many micro-cracks were observed only after a 0-100% DOD region cycle test. Cycle tests in several restricted ΔDOD conditions showed that the deterioration was closely related to not the upper and lower limits of DOD or operation voltage but the width of ΔDOD.

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

Pratapa, S.; Susanti, L.; Insany, Y. A. S.

Simple coprecipitation method has been used to produce nanoparticles of MgO (magnesia), MgO{center_dot}Al{sub 2}O{sub 3}(spinel), Y{sub 2}O{sub 3}(yttria) and Fe{sub 3}O{sub 4}(ferrite). The raw materials were, in respective, magnesium powder, magnesium and aluminium powders, ytrria powder, and natural sand. The coprecipitation included the use of suitable acid and base to dissolve the powders or sand and to produce precipitates, as well as the use of water to wash and purify the precipitates, and drying at relatively low temperatures, namely lower than 100 deg. C, followed by heating at 450 deg. C, 750 deg. C, 600 deg. C and 200 deg.more » C to produce magnesia, spinel, yttria and ferrite nanopowders, respectively. X-ray diffractometry was used to characterise the purity and nanocrystallinity of the final powders. It was found qualitatively that the powders were of high purity. Further line-broadening analysis using single-line and Rietveld-based softwares was performed to reveal the nanocrystallinity of the powders. Different line breadth values were found for the powders, indicating different crystallite sizes. It was also found that, particularly for spinel and yttria, the diffraction peaks exhibited 'longer' tails, indicating broader crystallite size distribution. The average crystallite size for the powders ranged from 3 to 70 nm. The results could then be used as 'fingerprints' for nanocrystallinity using x-ray diffractometry. The XRD crystallite sizes for yttria and ferrite nanocrystals are in fair agreement with their counterparts from electron microscopy observation.« less

Preparation and analysis of multilayer composites based on polyelectrolyte complexes

NASA Astrophysics Data System (ADS)

Petrova, V. A.; Orekhov, A. S.; Chernyakov, D. D.; Baklagina, Yu. G.; Romanov, D. P.; Kononova, S. V.; Volod'ko, A. V.; Ermak, I. M.; Klechkovskaya, V. V.; Skorik, Yu. A.

2016-11-01

A method for preparing multilayer film composites based on chitosan has been developed by the example of polymer pairs: chitosan-hyaluronic acid, chitosan-alginic acid, and chitosan-carrageenan. The structure of the composite films is characterized by X-ray diffractometry and scanning electron microscopy. It is shown that the deposition of a solution of hyaluronic acid, alginic acid, or carrageenan on a chitosan gel film leads to the formation of a polyelectrolyte complex layer at the interface, which is accompanied by the ordering of chitosan chains in the surface region; the microstructure of this layer depends on the nature of contacting polymer pairs.

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.

Growth of single crystals of mercuric iodide (HgI/sub 2/) in spacelab III

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

Van Den Berg, L.; Schnepple, W.F.

1981-01-01

Continued development of a system designed to grow crystals by physical vapor transport in the environment of Spacelab III will be described, with special emphasis on simulation of expected space conditions, adjustment of crystal growth parameters, and on board observation and control of the experiment by crew members and ground personnel. A critical factor in the use of mercuric iodide for semiconductor detectors of x-rays and gamma-rays is the crystalline quality of the material. The twofold purpose of the Spacelab III experiment is therefore to grow single crystals with superior electronic properties as an indirect result of the greatly reducedmore » gravity field during the growth, and to obtain data which will lead to improved understanding of the vapor transport mechanism. The experiments planned to evaluate the space crystals, including gamma-ray diffractometry and measurements of stoichiometry, lattice dimensions, mechanical strength, luminescense, and detector performance are discussed.« less

Synthesis and characterization of zeolites prepared from industrial fly ash.

PubMed

Franus, Wojciech; Wdowin, Magdalena; Franus, Małgorzata

2014-09-01

In this paper, we present the possibility of using fly ash to produce synthetic zeolites. The synthesis class F fly ash from the Stalowa Wola SA heat and power plant was subjected to 24 h hydrothermal reaction with sodium hydroxide. Depending on the reaction conditions, three types of synthetic zeolites were formed: Na-X (20 g fly ash, 0.5 dm(3) of 3 mol · dm(-3) NaOH, 75 °C), Na-P1 (20 g fly ash, 0.5 dm(3) of 3 mol · dm(-3) NaOH, 95 °C), and sodalite (20 g fly ash, 0.8 dm(3) of 5 mol · dm(-3) NaOH + 0.4 dm(3) of 3 mol · dm(-3) NaCl, 95 °C). As synthesized materials were characterized to obtain mineral composition (X-ray diffractometry, Scanning electron microscopy-energy dispersive spectrometry), adsorption properties (Brunauer-Emmett-Teller surface area, N2 isotherm adsorption/desorption), and ion exchange capacity. The most effective reaction for zeolite preparation was when sodalite was formed and the quantitative content of zeolite from X-ray diffractometry was 90 wt%, compared with 70 wt% for the Na-X and 75 wt% for the Na-P1. Residues from each synthesis reaction were the following: mullite, quartz, and the remains of amorphous aluminosilicate glass. The best zeolitic material as characterized by highest specific surface area was Na-X at almost 166 m(2) · g(-1), while for the Na-P1 and sodalite it was 71 and 33 m(2) · g(-1), respectively. The ion exchange capacity decreased in the following order: Na-X at 1.8 meq · g(-1), Na-P1 at 0.72 meq · g(-1), and sodalite at 0.56 meq · g(-1). The resulting zeolites are competitive for commercially available materials and are used as ion exchangers in industrial wastewater and soil decontamination.

Photoluminescent properties of complex metal oxide nanopowders for gas sensing

NASA Astrophysics Data System (ADS)

Bovhyra, R. V.; Mudry, S. I.; Popovych, D. I.; Savka, S. S.; Serednytski, A. S.; Venhryn, Yu. I.

2018-03-01

This work carried out research on the features of photoluminescence of the mixed and complex metal oxide nanopowders (ZnO/TiO2, ZnO/SnO2, Zn2SiO4) in vacuum and gaseous ambient. The nanopowders were obtained using pulsed laser reactive technology. The synthesized nanoparticles were characterized by X-ray diffractometry, energy-dispersive X-ray analysis, and scanning and transmission electron microscopy analysis for their sizes, shapes and collocation. The influence of gas environment on the photoluminescence intensity was investigated. A change of ambient gas composition leads to a rather significant change in the intensity of the photoluminescence spectrum and its deformation. The most significant changes in the photoluminescent spectrum were observed for mixed ZnO/TiO2 nanopowders. This obviously is the result of a redistribution of existing centers of luminescence and the appearance of new adsorption centers of luminescence on the surface of nanopowders. The investigated nanopowders can be effectively used as sensing materials for the construction of the multi-component photoluminescent sensing matrix.

Magnetic force microscopy study of domain walls in Co{sub 2}Z ferrite

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

Qin, Lang; Verweij, Henk, E-mail: verweij.1@osu.edu

2014-03-01

Graphical abstract: - Highlights: • Hexaferrite Co{sub 2}Z is synthesized through the modified Pechini method. • Magnetic domains are observed in anisotropic Co{sub 2}Z single grain using MFM. • Observed single grain domain thickness is in good agreement with Dotsh model. - Abstract: Hexaferrite Co{sub 2}Z was synthesized through the modified Pechini method. Partially oriented samples were obtained after consolidation with uniaxial pressing and calcination/sintering at 1300 °C/1330 °C. The sample composition and morphology was identified with X-ray diffractometry (XRD) and scanning electron microscopy (SEM) with energy-dispersive X-ray spectrometry (EDS). MFM studies of the single grains revealed a domain structuremore » with 0.7 μm wide. The Co{sub 2}Z static magnetization was measured with a vibrating sample magnetometer (VSM), and was used to calculate a single grain domain with a thickness of 4.8 μm. This result is in good agreement with SEM observations of the single grain thickness.« less

Mechanochemical synthesis and intercalation of Ca(II)Fe(III)-layered double hydroxides

NASA Astrophysics Data System (ADS)

Ferencz, Zs.; Szabados, M.; Varga, G.; Csendes, Z.; Kukovecz, Á.; Kónya, Z.; Carlson, S.; Sipos, P.; Pálinkó, I.

2016-01-01

A mechanochemical method (grinding the components without added water - dry grinding, followed by further grinding in the presence of minute amount of water or NaOH solution - wet grinding) was used in this work for the preparation and intercalation of CaFe-layered double hydroxides (LDHs). Both the pristine LDHs and the amino acid anion (cystinate and tyrosinate) intercalated varieties were prepared by the two-step grinding procedure in a mixer mill. By systematically changing the conditions of the preparation method, a set of parameters could be determined, which led to the formation of close to phase-pure LDH. The optimisation procedure was also applied for the intercalation processes of the amino acid anions. The resulting materials were structurally characterised by a range of methods (X-ray diffractometry, scanning electron microscopy, energy dispersive analysis, thermogravimetry, X-ray absorption and infra-red spectroscopies). It was proven that this simple mechanochemical procedure was able to produce complex organic-inorganic nanocomposites: LDHs intercalated with amino acid anions.

Enhanced photocatalytic activity of Fe-doped TiO2 coated on N-doped activated carbon composites for photocatalytic degradation of dyeing wastewater

NASA Astrophysics Data System (ADS)

Zhou, Jie; Zhu, Beibei; Wang, Lu; Li, Ya; Qiao, Qichen

2017-10-01

Fe-doped TiO2 coated on N-doped activated carbon (Fe-TiO2/N-AC, FTNA) composites were synthesized simply by a straightforward two-step procedure. The obtained materials were characterized by X-ray diffractometry (XRD), N2 adsorption-desorption, scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS) and FT-IR spectroscopies. Through the degradation of dyeing wastewater, the photocatalytic activity of FTNA was investigated under ultraviolet light irradiation. The results showed that containing N functional groups were successfully introduced onto the surface of the activated carbon. Compared with Fe-TiO2/AC (FTA), FTNA with average particle size of TiO2 13.6 nm and surface area 1007.89 m2/g showed a higher photoactivity. Additionally, for the photocatalytic degradation of dyeing wastewater, the optimum N content and catalyst content were 0.8% and 5g/L, respectively. Moreover, the photoactivity and photo stability of the catalyst after many runs was also evaluated.

In situ removal of arsenic from groundwater by using permeable reactive barriers of organic matter/limestone/zero-valent iron mixtures.

PubMed

Gibert, O; de Pablo, J; Cortina, J-L; Ayora, C

2010-08-01

In this study, two mixtures of municipal compost, limestone and, optionally, zero-valent iron were assessed in two column experiments on acid mine treatment. The effluent solution was systematically analysed throughout the experiment and precipitates from both columns were withdrawn for scanning electron microscopy, energy-dispersive X-ray spectroscopy, X-ray diffractometry analysis and, from the column containing zero-valent iron, solid digestion and sequential extraction analysis. The results showed that waters were cleaned of arsenic, metals and acidity, but chemical and morphological analysis suggested that metal removal was not due predominantly to biogenic sulphide generation but to pH increase, i.e. metal (oxy)hydroxide and carbonate precipitation. Retained arsenic and metal removal were clearly associated to co-precipitation with and/or sorption on iron and aluminum (oxy)hydroxides. An improvement on the arsenic removal efficiency was achieved when the filling mixture contained zero-valent iron. Values of arsenic concentrations were then always below 10 microg/L.

The Formation Mechanism and Corrosion Resistance of a Composite Phosphate Conversion Film on AM60 Alloy.

PubMed

Chen, Jun; Lan, Xiangna; Wang, Chao; Zhang, Qinyong

2018-03-08

Magnesium alloy AM60 has high duc and toughness, which is expected to increase in demand for automotive applications. However, it is too active, and coatings have been extensively studied to prevent corrosion. In this work, a Ba-containing composite phosphate film has been prepared on the surface of AM60. The composition and formation mechanism of the film have been investigated using a scanning electronic microscope equipped with energy dispersive X-ray spectroscopy, Fourier transform infrared, X-ray photoelectron spectroscopy, and X-ray diffractometry tests. The corrosion resistance of the film has been measured by electrochemical and immersion tests. The results show that the deposition film has fully covered the substrate but there are some micro-cracks. The structure of the film is complex, and consists of MgHPO₄·3H₂O, MnHPO₄·2.25H₂O, BaHPO₄·3H₂O, BaMg₂(PO₄)₂, Mg₃(PO₄)₂·22H₂O, Ca₃(PO₄)₂·xH₂O, and some amorphous phases. The composite phosphate film has better anticorrosion performance than the AM60 and can protect the bare alloy from corrosion for more than 12 h in 0.6 M NaCl.

Reversible Li storage for nanosize cation/anion-disordered rocksalt-type oxyfluorides: LiMoO2 - x LiF (0 ≤ x ≤ 2) binary system

NASA Astrophysics Data System (ADS)

Takeda, Nanami; Hoshino, Satoshi; Xie, Lixin; Chen, Shuo; Ikeuchi, Issei; Natsui, Ryuichi; Nakura, Kensuke; Yabuuchi, Naoaki

2017-11-01

A binary system of LiMoO2 - x LiF (0 ≤ x ≤ 2), Li1+xMoO2Fx, is systematically studied as potential positive electrode materials for rechargeable Li batteries. Single phase and nanosized samples on this binary system are successfully prepared by using a mechanical milling route. Crystal structures and Li storage properties on the binary system are also examined. Li2MoO2F (x = 1), which is classified as a cation-/anion-disordered rocksalt-type structure and is a thermodynamically metastable phase, delivers a large reversible capacity of over 300 mAh g-1 in Li cells with good reversibility. Highly reversible Li storage is realized for Li2MoO2F consisting of nanosized particles based on Mo3+/Mo5+ two-electron redox as evidenced by ex-situ X-ray absorption spectroscopy coupled with ex-situ X-ray diffractometry. Moreover, the presence of the most electronegative element in the framework structure effectively increases the electrode potential of Mo redox through an inductive effect. From these results, potential of nanosized lithium molybdenum oxyfluorides for high-capacity positive electrode materials of rechargeable Li batteries are discussed.

Passivation of hematite nanorod photoanodes with a phosphorus overlayer for enhanced photoelectrochemical water oxidation

NASA Astrophysics Data System (ADS)

Xiong, Dehua; Li, Wei; Wang, Xiaoguang; Liu, Lifeng

2016-09-01

Hematite (i.e., α-Fe2O3) nanorod photoanodes passivated with a phosphorus overlayer have been fabricated by decomposing sodium hypophosphite (NaH2PO2) at a low temperature over the hematite nanorod surface. Extensive scanning electron microscopy, transmission electron microscopy, x-ray diffractometry and UV-vis spectroscopy characterizations confirm that conformal deposition of an amorphous phosphorus overlayer does not change the crystal structure, morphology, and optical absorption properties of hematite photoanodes. X-ray photoelectron spectroscopy reveals that phosphorus in the deposited overlayer exists in an oxidized state. Comprehensive steady-state polarization, transient photocurrent response, and impedance spectroscopy measurements as well as Mott-Schottky analysis manifest that the phosphorus overlayer is able to effectively passivate surface states and suppress electron-hole recombination, substantially enhancing the photocurrent for water oxidation. Combining the phosphorization treatment with two-step thermal activation, a photocurrent density of 1.1 mA cm-2 is achieved at 1.23 V versus reversible hydrogen electrode under illumination of 100 mW cm-2, ca 55 times higher than that of the non-activated pristine hematite photoanode measured under the same conditions. The simple and fast phosphorization strategy we present here can be readily applied to passivate surfaces of other semiconductor photoelectrodes to improve their photoelectrochemical performance.

Ion-induced crystal damage during plasma-assisted MBE growth of GaN layers

NASA Astrophysics Data System (ADS)

Kirchner, V.; Heinke, H.; Birkle, U.; Einfeldt, S.; Hommel, D.; Selke, H.; Ryder, P. L.

1998-12-01

Gallium nitride layers were grown by plasma-assisted molecular-beam epitaxy on (0001)-oriented sapphire substrates using an electron cyclotron resonance (ECR) and a radio frequency (rf) plasma source. An applied substrate bias was varied from -200 to +250 V, resulting in a change of the density and energy of nitrogen ions impinging the growth surface. The layers were investigated by high-resolution x-ray diffractometry and high-resolution transmission electron microscopy (HRTEM). Applying a negative bias during growth has a marked detrimental effect on the crystal perfection of the layers grown with an ECR plasma source. This is indicated by a change in shape and width of (0002) and (202¯5) reciprocal lattice points as monitored by triple axis x-ray measurements. In HRTEM images, isolated basal plane stacking faults were found, which probably result from precipitation of interstitial atoms. The crystal damage in layers grown with a highly negative substrate bias is comparable to that observed for ion implantation processes at orders of magnitude larger ion energies. This is attributed to the impact of ions on the growing surface. None of the described phenomena was observed for the samples grown with the rf plasma source.

Structural properties of H-implanted InP crystals

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

Bocchi, C.; Franzosi, P.; Lazzarini, L.

1993-07-01

H has been implanted in InP crystals at the energy E [equals] 100 keV and at different doses ranging from [sigma] [equals] 1 x 10[sup 13] to [sigma] [equals] 5 x 10[sup 16] cm[sup [minus]2]. The depth dependence of the elastic lattice strain has been investigated by high resolution X-ray diffractometry. The implantation produces a lattice dilation. The strain increases with increasing depth, reaches the maximum at about 0.75 [mu]m, and then decreases rapidly; moreover the maximum strain is proportional to the dose. No extended crystal defects have been detected by transmission electron microscopy up to [sigma] <1 x 10[supmore » 16] cm[sup [minus]2] a buried amorphous layer 28 nm in thickness has been observed at the same depth where the strain is maximum. The thickness of the amorphous layer increases by further increasing the dose and reaches a value of about 0.18 [mu]m for [sigma] [equals] 5 x 10[sup 16] cm[sup [minus]2].« less

X-ray diffraction characterization of epitaxial CVD diamond films with natural and isotopically modified compositions

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

Prokhorov, I. A., E-mail: igor.prokhorov@mail.ru; Voloshin, A. E.; Ralchenko, V. G.

2016-11-15

Comparative investigations of homoepitaxial diamond films with natural and modified isotopic compositions, grown by chemical vapor deposition (CVD) on type-Ib diamond substrates, are carried out using double-crystal X-ray diffractometry and topography. The lattice mismatch between the substrate and film is precisely measured. A decrease in the lattice constant on the order of (Δa/a){sub relax} ∼ (1.1–1.2) × 10{sup –4} is recorded in isotopically modified {sup 13}C (99.96%) films. The critical thicknesses of pseudomorphic diamond films is calculated. A significant increase in the dislocation density due to the elastic stress relaxation is revealed by X-ray topography.

Mesoporous silica templated zirconia nanoparticles

NASA Astrophysics Data System (ADS)

Ballem, Mohamed A.; Córdoba, José M.; Odén, Magnus

2011-07-01

Nanoparticles of zirconium oxide (ZrO2) were synthesized by infiltration of a zirconia precursor (ZrOCl2·8H2O) into a SBA-15 mesoporous silica mold using a wet-impregnation technique. X-ray diffractometry and high-resolution transmission electron microscopy show formation of stable ZrO2 nanoparticles inside the silica pores after a thermal treatment at 550 °C. Subsequent leaching out of the silica template by NaOH resulted in well-dispersed ZrO2 nanoparticles with an average diameter of 4 nm. The formed single crystal nanoparticles are faceted with 110 surfaces termination suggesting it to be the preferred growth orientation. A growth model of these nanoparticles is also suggested.

Corrosion products of carbonation induced corrosion in existing reinforced concrete facades

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

Köliö, Arto; Honkanen, Mari; Lahdensivu, Jukka

Active corrosion in reinforced concrete structures is controlled by environmental conditions and material properties. These factors determine the corrosion rate and type of corrosion products which govern the total achieved service life. The type and critical amount of corrosion products were studied by electron microscopy and X-ray diffractometry on concrete and reinforcement samples from existing concrete facades on visually damaged locations. The corrosion products in outdoor environment exposed concrete facades are mostly hydroxides (Feroxyhite, Goethite and Lepidocrocite) with a volume ratio to Fe of approximately 3. The results can be used to calibrate calculation of the critical corrosion penetration ofmore » concrete facade panels.« 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.

Strength Characteristics of Resorbable Osteoconductive Ceramics Based on Diphosphates of Calcium and Alkali Metals

NASA Astrophysics Data System (ADS)

Putlayev, V. I.; Evdokimov, P. V.; Garshev, A. V.; Prosvirin, D. V.; Klimashina, E. S.; Safronova, T. V.; Ivanov, V. K.

2014-02-01

An investigation into the strength characteristics of ceramics based on diphosphates Ca(3- x)М2 x (PO4)2 ( x = 0-1 and М = Na, K) provides evidence of composition strengthening in the range х = 0.6-0.8 containing the greatest amount of the supercooled high-temperature modification α-СаМРО4. The method of high-temperature x-ray diffractometry is used to examine thermal expansion of rhenanite phases of СаМРО4.

Various types of semiconductor photocatalysts modified by CdTe QDs and Pt NPs for toluene photooxidation in the gas phase under visible light

NASA Astrophysics Data System (ADS)

Marchelek, M.; Grabowska, E.; Klimczuk, T.; Lisowski, W.; Zaleska-Medynska, A.

2017-01-01

A novel synthesis process was used to prepare TiO2 microspheres, TiO2 P-25, SrTiO3 and KTaO3 decorated by CdTe QDs and/or Pt NPs. The effect of semiconductor matrix, presence of CdTe QDs and/or Pt NPs on the semiconductor surface as well as deposition technique of Pt NPs (photodeposition or radiolysis) on the photocatalytic activity were investigated. The as-prepared samples were characterized by X-ray powder diffractometry (XRD), X-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM) with energy-dispersive X-ray (EDX) spectroscopy, scanning electron microscopy (SEM), photoluminescence spectrometry (PL), Fourier transform infrared (FT-IR) and Raman spectra, diffuse reflectance spectroscopy (DRS) and BET surface area analysis. The photocatalytic decomposition of toluene in gas phase, activated by light-emitting diodes (LEDs), with the CdTe/Pt nanoparticles-modified TiO2 microspheres, P25, SrTiO3 and KTaO3 semiconductors was investigated under UV-vis and visible irradiation.The results showed that the photoactivity depends on semiconductor matrix. The highest photoactivity under Vis light was observed for KTaO3/CdTe-Pt(R) sample (56% of toluene was decompose after 30 min of irradiation). The efficiency of the most active sample was 3 times higher than result for P25 and two times higher than for unmodified KTaO3.

Spatial Distribution of Trehalose Dihydrate Crystallization in Tablets by X-ray Diffractometry.

PubMed

Thakral, Naveen K; Yamada, Hiroyuki; Stephenson, Gregory A; Suryanarayanan, Raj

2015-10-05

Crystallization of trehalose dihydrate (C12H22O11·2H2O) was induced by storing tablets of amorphous anhydrous trehalose (C12H22O11) at 65% RH (RT). Our goal was to evaluate the advantages and limitations of two approaches of profiling spatial distribution of drug crystallization in tablets. The extent of crystallization, as a function of depth, was determined in tablets stored for different time-periods. The first approach was glancing angle X-ray diffractometry, where the penetration depth of X-rays was modulated by the incident angle. Based on the mass attenuation coefficient of the matrix, the depth of X-ray penetration was calculated as a function of incident angle, which in turn enabled us to "calculate" the extent of crystallization to different depths. In the second approach, the tablets were split into halves and the split surfaces were analyzed directly. Starting from the tablet surface and moving toward the midplane, XRD patterns were collected in 36 "regions", in increments of 0.05 mm. The results obtained by the two approaches were, in general, in good agreement. Additionally, the results obtained were validated by determining the "average" crystallization in the entire tablet by using synchrotron radiation in the transmission mode. The glancing angle method could detect crystallization up to ∼650 μm and had a "surface bias". Being a nondestructive technique, this method will permit repeated analyses of the same tablet at different time points, for example, during a stability study. However, split tablet analyses, while a "destructive" technique, provided comprehensive and unbiased depth profiling information.

Characterization and evaluation of miconazole salts and cocrystals for improved physicochemical properties.

PubMed

Tsutsumi, Shunichirou; Iida, Motoo; Tada, Norio; Kojima, Takashi; Ikeda, Yukihiro; Moriwaki, Toshiya; Higashi, Kenjirou; Moribe, Kunikazu; Yamamoto, Keiji

2011-12-15

Miconazole salts and cocrystals were studied to improve the physicochemical properties of miconazole. Maleate, hemifumarate, and hemisuccinate were prepared and characterized by powder X-ray diffractometry, differential scanning calorimetry, and single crystal X-ray diffractometry. The intrinsic dissolution rate and stability of each miconazole crystal form were compared to those of freebase and nitrate to evaluate the optimal crystal form. Crystal structure analysis indicated that maleate was a salt formed by proton transfer from the acid to the imidazole group of miconazole. Hemifumarate and hemisuccinate were determined to be cocrystals formed by hydrogen bonding between the acids and the base in their crystal lattices. Intrinsic dissolution tests showed that the formation of salts and cocrystals improved the dissolution rate of miconazole. Stability tests of preliminary formulations prepared with each crystal form indicated that maleate and hemifumarate were unstable at 80°C and generated a specific degraded product, i.e., a Michael adduct, between miconazole and the acids. Hemisuccinate had a superior intrinsic dissolution rate and stability, and is thus considered a promising crystal form of miconazole. Copyright © 2011 Elsevier B.V. All rights reserved.

Structure-substitution limit correlation study on Cr{sup 3+} substituted polycrystalline yttrium iron garnet

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

Modi, K. B.; Saija, K. G.; Sharma, P. U.

2016-05-06

Polycrystalline samples of Cr{sup 3+} - substituted yttrium iron garnet (Y{sub 3}Fe{sub 5}O{sub 12}) system with general chemical formula, Y{sub 3}Fe{sub 5-x}Cr{sub x}O{sub 12}, x = 0.0, 0.2, 0.4 and 0.6 were synthesized by double sintering ceramic technique and characterized by X-ray powder diffractometry. The Rietveld fitted X-ray diffraction patterns analysis revealed mono phase formation for x = 0.0 - 0.4 compositions while x = 0.6 composition possesses mixed phase character. The observed substitution limit has been discussed in the light of ionic size of substituent, electrostatic energy, electronic configuration and synthesis parameters. These observations strongly suggest that the electronicmore » configuration of Cr{sup 3+}, which is favorable to the formation of d2sp3 (octahedral) type bonds, must be important. In the case of Cr{sup 3+}, the substitution does not appear to proceed well for x much greater than 0.5, this limitation probably is a consequence of the strong preference of a smaller ion Cr{sup 3+}, for a larger octahedral site which quickly leads to a condition not comparable with the requirement of the structure. The distribution of cations, mean ionic radii and theoretical lattice constant values have been determined.« less

The Formation Mechanism and Corrosion Resistance of a Composite Phosphate Conversion Film on AM60 Alloy

PubMed Central

Lan, Xiangna; Wang, Chao; Zhang, Qinyong

2018-01-01

Magnesium alloy AM60 has high duc and toughness, which is expected to increase in demand for automotive applications. However, it is too active, and coatings have been extensively studied to prevent corrosion. In this work, a Ba-containing composite phosphate film has been prepared on the surface of AM60. The composition and formation mechanism of the film have been investigated using a scanning electronic microscope equipped with energy dispersive X-ray spectroscopy, Fourier transform infrared, X-ray photoelectron spectroscopy, and X-ray diffractometry tests. The corrosion resistance of the film has been measured by electrochemical and immersion tests. The results show that the deposition film has fully covered the substrate but there are some micro-cracks. The structure of the film is complex, and consists of MgHPO4·3H2O, MnHPO4·2.25H2O, BaHPO4·3H2O, BaMg2(PO4)2, Mg3(PO4)2·22H2O, Ca3(PO4)2·xH2O, and some amorphous phases. The composite phosphate film has better anticorrosion performance than the AM60 and can protect the bare alloy from corrosion for more than 12 h in 0.6 M NaCl. PMID:29518038

Self-propagating high-temperature synthesis and luminescent properties of ytterbium doped rare earth (Y, Sc, Lu) oxides nanopowders

NASA Astrophysics Data System (ADS)

Permin, D. A.; Novikova, A. V.; Balabanov, S. S.; Gavrishchuk, E. M.; Kurashkin, S. V.; Savikin, A. P.

2018-04-01

This paper describes a comparative study of structural and luminescent properties of 5%Yb-doped yttrium, scandium, and lutetium oxides (Yb:RE2O3) powders and ceramics fabricated by self-propagating high-temperature synthesis. According to X-ray diffractometry and electron microscopy the chosen method ensures preparation of low-agglomerated cubic Ctype crystal structured powders at one step. No crucial differences in luminescence spectra were found the Yb:RE2O3 powders and ceramics. It was shown that the emission lifetimes of the Yb:RE2O3 powders are lowered by crystal structure defects, while its values for ceramics samples are compared to that of monocrystals and more influenced by rare earth impurities.

Selective laser sintering of single-phase powder Cr-V tool steel

NASA Astrophysics Data System (ADS)

Kovalev, A. I.; Mishina, V. P.; Wainstein, D. L.; Titov, V. I.; Moiseev, V. F.; Tolochko, N. K.

2002-10-01

Presented is positive experience from selective laser sintering (SLS) of cylindrical steel specimens (3.0% C, 3.0% Cr, 1.0% Si, 12.0% V, Fe balance) 30 mm long and 5 mm in diameter by rapid prototyping. It was demonstrated that monolithic steel material could be successfully fabricated by this technology. Differential thermal analysis (DTA), scanning electron microscopy (SEM), and x-ray diffractometry (XRD) were used to study the microstructure, phase, and chemical composition of the source material and obtained specimens. Low-melting cementite-based eutectic was found to provide the liquid phase sintering of powder tool steel. The porosity of the green sintered specimens did not exceed 5%. The mean hardness value of sintered specimens was 825 HV.

Clay-mineraloid weathering products in Antarctic meteorites

NASA Technical Reports Server (NTRS)

Gooding, James L.

1986-01-01

The production of clay mineraloids (CMs) in the weathering of stony meteorites recovered in the Allan Hills and Elephant Moraine areas of Antarctica is investigated, applying electron microbeam analysis, pyrolysis/mass spectroscopy, X-ray diffractometry, and differential scanning calorimetry to whole-rock chips from two eucrites, two diogenites, and an H5 chondrite. The data are presented in tables, graphs, and photomicrographs and characterized in detail. Massive to incipient-vermicular CM formations with smectitelike or micalike compositions and indications of poor crystallization are observed and attributed to hydrocryogenic diagenesis (with little or no liquid water) on time scales of 10-1000 kyr. The need to take the compositional effects of weathering into account before attempting to reconstruct the preterrestrial histories of meteorites is stressed.

Ultrastructure of selected struvite-containing urinary calculi from dogs.

PubMed

Domingo-Neumann, R A; Ruby, A L; Ling, G V; Schiffman, P S; Johnson, D L

1996-09-01

To elucidate the ultrastructural details of struvite-containing urinary calculi from dogs. 38 specimens were selected from a collection of approximately 13,000 canine urinary calculi: 18 of these were composed entirely of struvite, and 20 consisted of struvite and calcium phosphate (apatite). Qualitative and quantitative analyses of specimens included use of plain and polarized light microscopy, x-ray diffractometry, scanning electron microscopy with backscattered electron imagery, x-ray fluorescence scans, and electron microprobe analysis. 4 textural types were recognized among struvite calculi, and 4 textural types of struvite-apatite calculi were described. Evidences of calculus dissolution were described from 4 calculi studied. The presence of small, well interconnected primary pores in struvite-containing urinary calculi from dogs appears to be a significant factor in determining the possible interaction of calculi with changes in the urine composition. The progress of dissolution from the calculus surface to the calculus interior appears to be largely affected by the primary porosity originally present between crystals forming the calculus framework. Apatite was observed to be more resistant to dissolution than struvite. The prevalence of fine concentric laminations having low porosity, and the common occurrence of apatite among struvite-containing urinary calculi from dogs may be 2 reasons why the efficacy of dietary and medicinal manipulations in dissolving urinary calculi is greater among cats than it is among dogs.

Growth, structural, optical, thermal and mechanical properties of ammonium pentaborate single crystal.

PubMed

Balakrishnan, T; Bhagavannarayana, G; Ramamurthi, K

2008-11-15

Nonlinear optical single crystals of ammonium pentaborate (APB) were grown by the slow cooling method from aqueous solution. Grown crystal was characterized by powder X-ray diffraction (PXRD) and FT-IR spectral analysis. Perfection of the grown crystal was evaluated by high-resolution X-ray diffractometry (HRXRD). The effect of nylon threading on the perfection of the grown bigger crystal was also studied by HRXRD. The range and percentage of optical transmission was ascertained by recording UV-vis-NIR spectrum. Thermal properties were investigated by TG-DTA and DSC analyses. Its mechanical hardness was estimated by Vickers microhardness tester.

Synthesis of AlFeCuCrMg{sub x} (x = 0, 0.5, 1, 1.7) alloy powders by mechanical alloying

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

Maulik, Ornov; Kumar, Vinod, E-mail: vkt.meta@mnit.ac.in; Adjunct Faculty, Materials Research Centre, Malaviya National Institute of Technology, Jaipur 302017

2015-12-15

Novel AlFeCuCrMg{sub x} (x = 0, 0.5, 1, 1.7 mol) high-entropy alloys (HEAs) were synthesized by mechanical alloying. The effect of Mg content on the phase evolution of HEAs was investigated using X-Ray diffractometry (XRD), transmission electron microscopy (TEM) and selected area electron diffraction (SAED) pattern analysis. The particle morphology and composition of HEAs were investigated by scanning electron microscopy (SEM). Thermodynamic parameters were calculated and analyzed to explain the formation of a solid solution. XRD analysis revealed BCC as major phase and FCC as a minor phase in as-milled AlFeCuCr and AlFeCuCrMg{sub 0.5} HEAs. Also, XRD analysis of as-milledmore » AlFeCuCrMg, AlFeCuCrMg{sub 1.7} confirmed the formation of two BCC phases (BCC 1 and BCC 2). TEM–SAED analysis of AlFeCuCrMg{sub x} HEAs concurred with XRD results. Microstructural features and mechanism for solid solution formation have been conferred in detail. Phase formation of the present HEAs has been correlated with calculated thermodynamic parameters. Differential thermal analysis (TGA-DTA) of these alloys confirmed that there is no substantial phase change up to 500 °C. - Highlights: • Novel AlFeCuCrMg{sub x} (x = 0, 0.5, 1, 1.7) HEAs were prepared by mechanical alloying. • Phase evolution and lattice parameter were studied by X-Ray Diffraction. • Crystallite size and lattice microstrain calculated failed to obey the Williamson–Hall method. • Criterions for formation of simple solid solution were compared to the thermodynamic parameters of the present HEAs. • Increase in the Mg concentration in AlMg{sub x}FeCuCr (x = 0, 0.5, 1, 1.7) HEAs supports the formation of BCC phase.« less

Synthesis and characterization of polyethylenimine-based iron oxide composites as novel contrast agents for MRI.

PubMed

Masotti, A; Pitta, A; Ortaggi, G; Corti, M; Innocenti, C; Lascialfari, A; Marinone, M; Marzola, P; Daducci, A; Sbarbati, A; Micotti, E; Orsini, F; Poletti, G; Sangregorio, C

2009-04-01

Use of polyethylenimines (PEIs) of different molecular weight and selected carboxylated-PEI derivatives (PEI-COOH) in the synthesis and stabilization of iron oxide nanoparticles, to obtain possible multifunctional contrast agents. Oxidation of Fe(II) at slightly elevated pH and temperature resulted in the formation of highly soluble and stable nanocomposites of iron oxides and polymer. Composites were characterized and studied by atomic force microscopy (AFM), transmission electron microscopy (TEM), X-ray diffractometry, AC and DC magnetometry, NMR relaxometry and magnetic resonance imaging (MRI). From AFM the dimensions of the aggregates were found to be in the ~150-250 nm size region; the mean diameter of the magnetic core of the compounds named PEI-25, PEI-500 and PEI-COOH60 resulted d approximately 20 +/- 5 nm for PEI-25, d approximately 9.5 +/- 1.0 nm for PEI-500 and d approximately 6.8 +/- 1.0 nm for PEI-COOH60. In PEI-COOH60 TEM and X-ray diffractometry revealed small assemblies of mineral magnetic cores with clear indications that the main constituents are maghemite and/or magnetite as confirmed by AC and DC SQUID magnetometry. For PEI-COOH60, the study of NMR-dispersion profiles revealed r (1) and r (2) relaxivities comparable to superparamagnetic iron-oxide commercial compounds in the whole investigated frequency range 7 < or = nu < or = 212 MHz. PEI-25 was studied as possible MRI contrast agent (CA) to map the cerebral blood volume (CBV) and cerebral blood flow (CBF) in an animal model obtaining promising results. The reported compounds may be further functionalized to afford novel multifunctional systems for biomedical applications.

Effect of hydrodynamics and surface roughness on the electrochemical behaviour of carbon steel in CSG produced water

NASA Astrophysics Data System (ADS)

Eyu, Gaius Debi; Will, Geoffrey; Dekkers, Willem; MacLeod, Jennifer

2015-12-01

The influence of fluid flow, surface roughness and immersion time on the electrochemical behaviour of carbon steel in coal seam gas produced water under static and hydrodynamic conditions has been studied. The disc electrode surface morphology before and after the corrosion test was characterized using scanning electron microscopy (SEM). The corrosion product was examined using X-ray photoelectron spectroscopy (XPS) and X-ray diffractometry (XRD).The results show that the anodic current density increased with increasing surface roughness and consequently a decrease in corrosion surface resistance. Under dynamic flow conditions, the corrosion rate increased with increasing rotating speed due to the high mass transfer coefficient and formation of non-protective akaganeite β-FeO(OH) and goethite α-FeO(OH) corrosion scale at the electrode surface. The corrosion rate was lowest at 0 rpm. The corrosion rate decreased in both static and dynamic conditions with increasing immersion time. The decrease in corrosion rate is attributed to the deposition of corrosion products on the electrode surface. SEM results revealed that the rougher surface exhibited a great tendency toward pitting corrosion.

RADIOACTIVITY DOSAGE OF ORNAMENTAL GRANITIC ROCKS BASED ON CHEMICAL, MINERALOGICAL AND LITHOLOGICAL DATA

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

Salas, H.T.; Nalini, H.A. Jr.; Mendes, J.C.

2004-10-03

One hundred samples of granitic rock were collected from granite traders in Belo Horizonte. Autoradiography, optical microscopy, diffractometry, and chemical analysis (X-ray spectrometry, X-ray fluorescence, neutron activation, gravimetry and electron probe microanalysis) were used to determine the mineral assemblages and lithotypes. Autoradiographic results for several samples showed the presence of monazite, allanite and zircon. Chemical analysis revealed concentrations of uranium of {le} 30ppm, and thorium {le} 130ppm. Higher concentrations generally correlated with high concentrations of light rare earths in silica-rich rocks of granitic composition. Calculations were made of radioactive doses for floor tiles in a standard room for samples withmore » total concentration of uranium and thorium greater than 60ppm. On the basis of calculations of {sup 232}Th, {sup 40}K and {sup 226}Ra from Th, K and U analysis, the doses calculated were between 0.11 and 0.34 mSv/year, which are much lower than the acceptable international exposure standard of 1.0 mSv/year.« less

Low Temperature Synthesis of Cobalt-Chromium Carbide Nanoparticles-Doped Carbon Nanofibers.

PubMed

Yousef, Ayman; Brooks, Robert M; Abutaleb, Ahmed; Al-Deyab, Salem S; El-Newehy, Mohamed H

2018-04-01

Electrospinning has been used to synthesize cobalt-chromium carbide nanoparticles (NPs)-doped carbon nanofibers (CNFs) (Composite). Electrospun mat comprising of cobalt acetate, chromium acetate and poly(vinyl alcohol) (PVA) has been carbonized at low temperature (850 °C) for 3 h under argon atmosphere to produce the introduced composite. The process was achieved at low temperature due to the presence of cobalt as an activator. Field emission scanning electron microscope (FE-SEM), X-ray diffractometry (XRD), and transmission electron microscopy (TEM) equipped with EDX techniques were used to determine the products characteristics. The results indicated the formation of pure cobalt (Co), Cr7C3 NPs and crystalline CNFs. The Co and Cr7C3 NPs were covered with CNFs. Overall, the proposed NFs open new avenue to prepare different metals-metal carbides-carbon NFs at low temperature and short reaction time.

Self-assembled biomimetic superhydrophobic CaCO3 coating inspired from fouling mineralization in geothermal water.

PubMed

Wang, Gong G; Zhu, Li Q; Liu, Hui C; Li, Wei P

2011-10-18

Inspired from fouling self-mineralization in geothermal water, a novel biomimetic cactuslike CaCO(3) coating with superhydrophobic features is reported in this letter. The structure, morphologies, and phases of the CaCO(3) coating were characterized by X-ray diffractometry, scanning electron microscopy, transmission electron microscopy, and infrared spectrophotometry. After prenucleation treatment, a continuous cactuslike CaCO(3) coating with hierarchical nano- and microstructures was self-assembled on stainless steel surfaces after immersion in simulated geothermal water at 50 °C for 48 h. After being modified with a low-surface-energy monolayer of sodium stearate, the as-prepared coating exhibited superhydrophobic properties with a water contact angle of 158.9° and a sliding angle of 2°. Therefore, this work might open up a new application field of geothermal resources and provide insight into designing multidimensional structures with functional applications, including superhydrophobic surfaces. © 2011 American Chemical Society

Manganese porphyrin immobilized on magnetic MCM-41 nanoparticles as an efficient and reusable catalyst for alkene oxidations with sodium periodate

NASA Astrophysics Data System (ADS)

Hajian, Robabeh; Ehsanikhah, Amin

2018-01-01

This study describes the immobilization of tetraphenylporphyrinatomanganese(III) chloride, (MnPor), onto imidazole functionalized MCM-41 with magnetite nanoparticle core (Fe3O4@MCM-41-Im). The resultant material (Fe3O4@MCM-41-Im@MnPor) was characterized by X-ray diffractometry (XRD), Fourier transform infra-red (FT-IR), diffuse reflectance UV-Vis spectrophotometry (DR UV-Vis), field emission scanning electron microscopy (FESEM), Inductively coupled plasma (ICP), analyzer transmission electron microscopy (TEM) and Brunauer-Emmett-Teller (BET) surface area. This new heterogenized catalyst was applied as an efficient catalyst for the epoxidation of a variety of cyclic and linear olefins with NaIO4 under mild conditions. The prepared catalyst can be easily recovered through the application of an external magnet, and reused several times without any significant decrease in activity and magnetic properties.

Enhanced UV-visible response of bismuth subcarbonate nanowires for degradation of xanthate and photocatalytic reaction mechanism.

PubMed

Cui, Kuixin; He, Yuehui; Jin, Shengming

2016-04-01

(BiO)2CO3 nanowires were prepared by simple hydrothermal treatment of commercial Bi2O3 powders and characterized by X-ray diffractometry, scanning electron microscopy, transmission electron microscopy (TEM), high-resolution TEM, and X-ray photoelectron spectroscopy (XPS). The photocatalytic activity of (BiO)2CO3 nanowires was studied through degradation of sodium isopropyl xanthate. Photocatalytic experimental results indicated that the as-prepared (BiO)2CO3 nanowires show high photocatalytic efficiency. Photocatalytic activity increased after two cycles. Time-dependent UV-vis spectra demonstrated that the final degradation products included isopropyl alcohol and carbon disulfide. UV-vis diffuse reflection spectra showed that the band gap of the as-prepared (BiO)2CO3 nanowires and recycled (BiO)2CO3 nanowires were 2.75 eV and 1.15 eV, respectively. XPS results indicated that formation of Bi2S3@(BiO)2CO3 core-shell nanowires occurred after recycled photodegradation of isopropyl xanthate owing to existence of two types of Bi configurations in the recycled (BiO)2CO3 nanowires. A probable degradation mechanism of isopropyl xanthate was also proposed. Copyright © 2016 Elsevier Ltd. All rights reserved.

Microstructures and Mechanical Properties of Co-Cr Dental Alloys Fabricated by Three CAD/CAM-Based Processing Techniques

PubMed Central

Kim, Hae Ri; Jang, Seong-Ho; Kim, Young Kyung; Son, Jun Sik; Min, Bong Ki; Kim, Kyo-Han; Kwon, Tae-Yub

2016-01-01

The microstructures and mechanical properties of cobalt-chromium (Co-Cr) alloys produced by three CAD/CAM-based processing techniques were investigated in comparison with those produced by the traditional casting technique. Four groups of disc- (microstructures) or dumbbell- (mechanical properties) specimens made of Co-Cr alloys were prepared using casting (CS), milling (ML), selective laser melting (SLM), and milling/post-sintering (ML/PS). For each technique, the corresponding commercial alloy material was used. The microstructures of the specimens were evaluated via X-ray diffractometry, optical and scanning electron microscopy with energy-dispersive X-ray spectroscopy, and electron backscattered diffraction pattern analysis. The mechanical properties were evaluated using a tensile test according to ISO 22674 (n = 6). The microstructure of the alloys was strongly influenced by the manufacturing processes. Overall, the SLM group showed superior mechanical properties, the ML/PS group being nearly comparable. The mechanical properties of the ML group were inferior to those of the CS group. The microstructures and mechanical properties of Co-Cr alloys were greatly dependent on the manufacturing technique as well as the chemical composition. The SLM and ML/PS techniques may be considered promising alternatives to the Co-Cr alloy casting process. PMID:28773718

Iron-antimony-based hybrid oxides as high-performance anodes for lithium-ion storage

NASA Astrophysics Data System (ADS)

Nguyen, Tuan Loi; Kim, Doo Soo; Hur, Jaehyun; Park, Min Sang; Yoon, Sukeun; Kim, Il Tae

2018-06-01

We report a facile approach to synthesize Fe-Sb-based hybrid oxides nanocomposites consisting of Sb, Sb2O3, and Fe3O4 for use as new anode materials for lithium-ion batteries. The composites are synthesized via galvanic replacement between Fe3+ and Sb at high temperature in triethylene glycol medium. The phase, morphology, and composition changes of the composites involved in the various stages of the replacement reaction are characterized using X-ray diffractometry, high-resolution transmission electron microscopy, and energy dispersive X-ray spectroscopy. The as-prepared composites have different compositions with very small particle sizes (<< 10 nm). The FexSbyOz-18 h composite, for instance, exhibits high capacity, better cyclic stability, and rate performance than other composites, with a highly stable specific capacity of 434 mAh g-1 at 500 cycles. The excellent electrochemical performance can be ascribed to the high interfacial contact area between the nanocomposite and electrolyte, stable structure of the composites owing to a mixture of inactive phases generated by the conversion reaction between Li+ and oxide metal-whose structure serves as an electron conductor, inhibits agglomeration of Sb particles, and acts as an effective buffer against volume change of Sb during cycling-and high Li+ diffusion ability.

Microwave combustion synthesis of Co1-xZnxFe2O4 (0⩽x⩽0.5): Structural, magnetic, optical and vibrational spectroscopic studies.

PubMed

Sundararajan, M; Kennedy, L John; Vijaya, J Judith; Aruldoss, Udaya

2015-04-05

Nanostructured pure and zinc doped cobalt ferrites (Co1-xZnxFe2O4 where x fraction ranging from 0 to 0.5) were prepared by microwave combustion method employing urea as a fuel. The nanostructured samples were characterized by using various instrumental techniques such as X-ray powder diffractometry, high resolution scanning electron microscopy, energy dispersive X-ray analysis, UV-visible diffuse reflectance spectroscopy, photoluminescence spectroscopy and Fourier transformed infrared (FT-IR) spectroscopy. Vibrating sample magnetometry at room temperature was recorded to study the magnetic behavior of the samples. X-ray analysis and the FT-IR spectroscopy revealed the formation of cobalt ferrite cubic spinel-type structure. The average crystallite sizes for the samples were in the range of 3.07-11.30 nm. The direct band gap (Eg) was estimated using Kubelka-Munk method and is obtained from the UV-vis spectra. The band gap value decreased with an increase in zinc fraction (2.56-2.17 eV). The violet and green emission observed in the photoluminescence spectra revealed that cobalt ferrites are governed by defect controlled processes. The elemental analysis of zinc doped cobalt ferrites were obtained from energy dispersive X-ray (EDX) analysis. From the magnetic measurements, it is observed that cobalt ferrite and zinc doped cobalt ferrite systems fall under the soft ferrite category. The saturation magnetization (Ms) value of undoped cobalt ferrite is 14.26 emu/g, and it has reached a maximum of 29.61 emu/g for Co0.7Zn0.3Fe2O4. Copyright © 2014 Elsevier B.V. All rights reserved.

The effect of X-ray exposure on Ba2SiO4:Eu3+

NASA Astrophysics Data System (ADS)

Volhard, Max-Fabian; Jüstel, Thomas

2018-03-01

The ortho-silicates Ba2SiO4:Eu3+ and Ba2SiO4:Eu2+ are well-established materials for fluorescent light sources, e.g., phosphor converted LEDs. Samples containing Eu2+or Eu3+were synthesised by the solid-state-method, and the phase purity was determined by X-ray powder diffractometry. The photoluminescence of both phosphors was examined as a function of the pre-treatment. Upon irradiation of Ba2SiO4:Eu3+ with X-rays (tungsten target source), the reduction of Eu3+ towards Eu2+ was observed. This reduction behaviour was thoroughly recorded, and the linearity of the process was determined. Furthermore, the relationship between the acceleration voltage and the reduction process is discussed.

Single-crystal sapphire microstructure for high-resolution synchrotron X-ray monochromators

DOE PAGES

Asadchikov, Victor E.; Butashin, Andrey V.; Buzmakov, Alexey V.; ...

2016-03-22

We report on the growth and characterization of several sapphire single crystals for the purpose of x-ray optics applications. Structural defects were studied by means of laboratory double-crystal X-ray diffractometry and white beam synchrotron-radiation topography. The investigations confirmed that the main defect types are dislocations. The best quality crystal was grown using the Kyropoulos technique with a dislocation density of 10 2-10 3 cm -2 and a small area with approximately 2*2 mm 2 did not show dislocation contrast in many reflections and has suitable quality for application as a backscattering monochromator. As a result, a clear correlation between growthmore » rate and dislocation density is observed, though growth rate is not the only parameter impacting the quality.« less

A mixed valence zinc dithiolene system with spectator metal and reactor ligands.

PubMed

Ratvasky, Stephen C; Mogesa, Benjamin; van Stipdonk, Michael J; Basu, Partha

2016-08-16

Neutral complexes of zinc with N,N'-diisopropylpiperazine-2,3-dithione ( i Pr 2 Dt 0 ) and N,N'-dimethylpiperazine-2,3-dithione (Me 2 Dt 0 ) with chloride or maleonitriledithiolate (mnt 2- ) as coligands have been synthesized and characterized. The molecular structures of these zinc complexes have been determined using single crystal X-ray diffractometry. Complexes recrystallize in monoclinic P type systems with zinc adopting a distorted tetrahedral geometry. Two zinc complexes with mixed-valent dithiolene ligands exhibit ligand-to-ligand charge transfer bands. Optimized geometries, molecular vibrations and electronic structures of charge-transfer complexes were calculated using density functional theory (B3LYP/6-311G+(d,p) level). Redox orbitals are shown to be almost exclusively ligand in nature, with a HOMO based heavily on the electron-rich maleonitriledithiolate ligand, and a LUMO comprised mostly of the electron-deficient dithione ligand. Charge transfer is thus believed to proceed from dithiolate HOMO to dithione LUMO, showing ligand-to-ligand redox interplay across a d 10 metal.

Enhanced Photocatalytic Activity toward Organic Pollutants Degradation and Mechanism Insight of Novel CQDs/Bi₂O₂CO₃ Composite.

PubMed

Zhang, Zisheng; Lin, Shuanglong; Li, Xingang; Li, Hong; Zhang, Tong; Cui, Wenquan

2018-05-15

Novel carbon quantum dots (CQDs) modified with Bi₂O₂CO₃ (CQDs/Bi₂O₂CO₃) were prepared using a simple dynamic-adsorption precipitation method. X-ray diffractometry (XRD), transmission electron microscopy (TEM), energy dispersive X-ray spectroscopy (EDX), and scanning electron microscopy (SEM) were used to test the material composition, structure, and band structures of the as-prepared samples. Methylene blue (MB) and colorless phenol, as target organic pollutants, were used to evaluate the photocatalytic performance of the CQDs/Bi₂O₂CO₃ hybrid materials under visible light irradiation. Experimental investigation shows that 2⁻5 nm CQDs were uniformly decorated on the surface of Bi₂O₂CO₃; CQDs/Bi₂O₂CO₃ possess an efficient photocatalytic performance, and the organic matter removal rate of methylene blue and phenol can reach up to 94.45% and 61.46% respectively, within 2 h. In addition, the degradation analysis of phenol by high performance liquid chromatography (HPLC) proved that there are no other impurities in the degradation process. Photoelectrochemical testing proved that the introduction of CQDs (electron acceptor) effectively suppresses the recombination of e - -h⁺, and promotes charge transfer. Quenching experiments and electron spin resonance (ESR) suggested that ·OH, h⁺, and ·O₂ - were involved in the photocatalytic degradation process. These results suggested that the up-conversion function of CQDs could improve the electron transfer and light absorption ability of photocatalysts and ·O₂ - formation. Furthermore, the up-conversion function of CQDs would help maintain photocatalytic stability. Finally, the photocatalytic degradation mechanism was proposed according to the above experimental result.

Heats of immersion of titania powders in primer solutions

NASA Technical Reports Server (NTRS)

Siriwardane, R.; Wightman, J. P.

1983-01-01

The oxide layer present on titanium alloys can play an important role in determining the strength and durability of adhesive bonds. Here, three titania powders in different crystalline phases, rutile-R1, anatase-A1, and anatase-A2, are characterized by several techniques. These include microelectrophoresis, X-ray diffractometry, surface area pore volume analysis, X-ray photoelectron spectroscopy, and measurements of the heats of immersion. Of the three powders, R1 has the highest heat of immersion in water, while the interaction between water and A1 powder is low. Experimental data also suggest a specific preferential interaction of polyphenylquinoxaline with anatase.

Marble protection: An inorganic electrokinetic approach

NASA Astrophysics Data System (ADS)

Meloni, Paola; Manca, Francesco; Carcangiu, Gianfranco

2013-05-01

The influence of an electric potential difference in an aqueous solution was studied as a method for depositing a calcium oxalate coating over a weathered carbonatic stone. Samples of weathered Carrara white marble were treated at 15 and 50 °C for 5 h in an electrokinetic cell, specifically conceived for this study, containing a solution of ammonium oxalate (4% by weight), and were subsequently characterised by scanning electron microscopy, X-ray diffractometry, thermogravimetric analysis and mercury intrusion porosimetry. The electrokinetic treatment proved to be a cost effective and time saving process, able to produce a thick and homogeneous calcium oxalate coating over the stone surface that improves its chemical and physical resistance in low pH environments, and is able to protect the stone from the by-products of urban pollution.

A facile and efficient strategy for the fabrication of porous linseed gum/cellulose superabsorbent hydrogels for water conservation.

PubMed

Zhang, Hao; Luan, Qian; Huang, Qingde; Tang, Hu; Huang, Fenghong; Li, Wenlin; Wan, Chuyun; Liu, Changsheng; Xu, Jiqu; Guo, Pingmei; Zhou, Qi

2017-02-10

The linseed gum/cellulose composite hydrogels were successfully fabricated by mixing cellulose and linseed gum solutions dissolved in the NaOH/urea aqueous system and cross-linked with epichlorohydrin. The morphology and structure of the composite hydrogels were investigated by scanning electron microscopy (SEM), Fourier transform infrared (FTIR) spectroscopy, X-ray diffractometry (XRD) and thermogravimetric analysis (TGA). The swelling ratio and water retention properties were investigated. The results revealed that linseed gum mainly contributed to water adsorption, whereas the cellulose acted as a backbone to strengthen the porous structure. This work provided a simple way to prepare cellulose-based superabsorbent hydrogels, which could be potentially applied as an effective water conservation material in agriculture. Copyright © 2016 Elsevier Ltd. All rights reserved.

Geology and geochemistry of the Arctic prospect, Ambler District, Alaska

NASA Astrophysics Data System (ADS)

Schmidt, J. M.

The Arctic volcanogenic massive sulfide prospect is the largest known (40 million ton) deposit hosted by the low greenschist grade, latest Devonian Ambler Sequence of bimodal, basaltic and rhyolitic volcanic and volcanoclastic rocks, pelitic, graphitic and calcareous metasediments. Detailed field mapping, core logging, petrography, X-ray diffractometry, electron microprobe analyses and whole-rock major element analyses of hydrothermally altered rocks were used to determine the emplacement history and setting of sulfide deposition. Low greenschist grade metamorphism was essentially isochemical on a macroscopic scale, and preserved volcanic compositions, the major element chemistry of alteration and the compositions of individual metamorphic, alteration and relict igneous minerals. Mineralization at Arctic was formed along a synvolcanic fault in a tectonically and volcanically active basin within a rifted continental margin, possibly related to an actively spreading oceanic rift.

Characterization of calcium phosphate coatings deposited by Nd:YAG laser ablation at 355 nm: influence of thickness.

PubMed

Fernández-Pradas, J M; Clèries, L; Sardin, G; Morenza, J L

2002-05-01

Calcium phosphate coatings were deposited by pulsed laser ablation with a radiation of 355 nm from a Nd:YAG laser. All the coatings were obtained at the same conditions, but deposition was stopped after different number of pulses to get coatings with different thickness. The influence of thickness in the structural and mechanical properties of the coatings was investigated. Coatings structure was characterised by scanning electron microscopy, grazing incidence X-ray diffractometry and Raman spectroscopy. The mechanical properties were evaluated by scratch test. The morphology of the coatings is dominated by the presence of droplets. The coatings are composed mainly of hydroxyapatite, alpha tricalcium phosphate and amorphous calcium phosphate. Thinner coatings withstand higher loads of failure in the scratch test.

Chemical compositions, infrared spectroscopy, and X-ray diffractometry study on brown-rotted woods

Treesearch

Gai-Yun Li; Luo-Hua Huang; Chung Hse; Te-Fu Qin

2011-01-01

The effect of brown-rot decay on the chemical composition and crystallinity of Masson pine was studied by exposing it to Wolfiporia cocos (Schwein.) Ryvarden and Gilbn. for durations of up to 15 weeks in the field. The holocellulose content, α-cellulose content, and wood crystallinity decreased slowly in the initial stage, followed by a significant reduction...

Nitriding of titanium and titanium: 8 percent aluminum, 1 percent molybdenum, 1 percent vanadium alloy with an ion-beam source

NASA Technical Reports Server (NTRS)

Gill, A.

1983-01-01

Titanium and Ti-8Al-1Mo-1V alloy were nitrided with an ion-beam source of nitrogen or argon and nitrogen at a total pressure of 2 x 10 to the minus 4th power to 10 x 10 to the minus 4th power torr. The treated surface was characterized by surface profilometry, X-ray diffractometry, Auger electron spectroscopy and microhardness measurements. The tetragonal Ti2N phase formed in pure titanium and Ti-8Al-1Mo-1V alloy with traces of AlN in the alloy. Two opposite processes competed during the ion-beam-nitriding process: (1) formation of nitrides in the surface layer and (2) sputtering of the nitrided layers by the ion beam. The highest surface hardnesses, about 500 kg/sq mm in titanium and 800 kg/sq mm in Ti-8Al-1Mo-1V, were obtained by ion nitriding with an ion beam of pure nitrogen at 4.2 x 10 to the minus 4th power torr at a beam voltage of 1000 V.

Synthesis of LiFePO4/C composites based on natural iron stone using a sol gel method

NASA Astrophysics Data System (ADS)

Angela, Riyan; Islam, Humaatul; Sari, Vamellia; Latif, Chaironi; Zainuri, Mochamad; Pratapa, Suminar

2017-01-01

Synthesis of LiFePO4/C composites has been carried out using a sol gel method. The Fe precursor was made from a natural iron stone of Tanah Laut, South Kalimantan, while the other raw materials were commercial Li2CO3 powder and NH4H2PO4 powder with HCl and water as solvents. Citric acid was used as the carbon source in the synthesis. This study used a molar ratio of 1:1:2 for Li:Fe:P with variation of added citric acid of 1.5 and 2.5 g. The solutions were dried in air at 100°C. The dried powders were characterized using DSC-TGA and then calcined at 600 and 700°C under argon environment for 10 hours. The calcined powders were characterized by X-ray diffractometry (XRD), scanning electron microscopy-energy dispersive x-ray (SEM-EDX), and LCR meter. It was found that the samples contained LiFePO4 as the dominant phase and LiFeP2O7 and Fe2O3 as secondary phases. The analysis showed that the addition of citric acid influenced the electronic conductivity of the composites. A Rietveld relative weight fraction of up to 94.7% was achieved in the synthesis at temperature 600°C. The LFP/C sample exhibited electronic conductivity of 4.56×10-3 Scm-1 which was six times of that of the pure LFP.

LiFePO4 Nanostructures Fabricated from Iron(III) Phosphate (FePO4 x 2H2O) by Hydrothermal Method.

PubMed

Saji, Viswanathan S; Song, Hyun-Kon

2015-01-01

Electrode materials having nanometer scale dimensions are expected to have property enhancements due to enhanced surface area and mass/charge transport kinetics. This is particularly relevant to intrinsically low electronically conductive materials such as lithium iron phosphate (LiFePO4), which is of recent research interest as a high performance intercalation electrode material for Li-ion batteries. Many of the reported works on LiFePO4 synthesis are unattractive either due to the high cost of raw materials or due to the complex synthesis technique. In this direction, synthesis of LiFePO4 directly from inexpensive FePO4 shows promise.The present study reports LiFePO4 nanostructures prepared from iron (III) phosphate (FePO4 x 2H2O) by precipitation-hydrothermal method. The sintered powder was characterized by X-ray diffractometry (XRD), X-ray photoelectron spectroscopy (XPS), Inductive coupled plasma-optical emission spectroscopy (ICP-OES), and Electron microscopy (SEM and TEM). Two synthesis methods, viz. bulk synthesis and anodized aluminum oxide (AAO) template-assisted synthesis are reported. By bulk synthesis, micro-sized particles having peculiar surface nanostructuring were formed at precipitation pH of 6.0 to 7.5 whereas typical nanosized LiFePO4 resulted at pH ≥ 8.0. An in-situ precipitation strategy inside the pores of AAO utilizing the spin coating was utilized for the AAO-template-assisted synthesis. The template with pores filled with the precipitate was subsequently subjected to hydrothermal process and high temperature sintering to fabricate compact rod-like structures.

Characterization of home-made silver sulphide based iodide selective electrode.

PubMed

Rajbhandari Nyachhyon, A; Yadav, A P; Manandhar, K; Pradhananga, R R

2010-09-15

Polycrystalline silver sulphide/silver iodide ion selective electrodes (ISEs) with four different compositions, 9:1, 2:1, 1:1, 1:9 Ag(2)S-AgI mole ratios, have been fabricated in the laboratory and characterized by X-ray diffractometry (XRD), scanning electron microscopy (SEM), and electrochemical impedance spectroscopy (EIS). X-ray diffraction studies show the presence of Ag(3)SI, Ag(2)S and AgI crystalline phases in the electrode material. The electrode surfaces have been found to become smoother and lustrous with increasing percentage of silver sulphide in silver iodide. ISE 1:1, ISE 2:1 and ISE 9:1 all responded in Nernstian manner with slopes of about 60 mV/decade change in iodide ion concentration in the linear range of 1 x 10(-1) to 1 x 10(-6)M while ISE 1:9 showed sub-Nernstian behavior with slope of about 45 mV up to the concentration 1 x 10(-5)M. Two capacitive loops, one corresponding to the charge transfer process at metal electrode and the back contact and a second loop corresponding to the charge transfer process at membrane-electrolyte interface have been observed at high and low frequency ranges, respectively. Mott-Schottky analysis shows that the materials are n-type semiconductors with donor defect concentrations in the range of 5.1 x 10(14) to 2.4 x 10(19)/cm(3). Copyright (c) 2010 Elsevier B.V. All rights reserved.

Synthesis of core-shell structured FAU/SBA-15 composite molecular sieves and their performance in catalytic cracking of polystyrene

NASA Astrophysics Data System (ADS)

Du, Jinlong; Shi, Chunwei; Wu, Wenyuan; Bian, Xue; Chen, Ping; Cui, Qingzhu; Cui, Zhixuan

2017-12-01

Composite molecular sieves, FAU/SBA-15, having core-shell structure were synthesized. The synthesized composite sieves were characterized by X-ray diffractometry (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive X-ray spectroscopy (EDS), pyrolysis fourier transform infrared (Py-FTIR) spectroscopy, temperature programmed desorption spectra (NH3-TPD), UV Raman spectroscopy, nuclear magnetic resonance (NMR) and other techniques. XRD, SEM, TEM, N2 adsorption-desorption, mass spectrometry, NMR and EDS results showed that the composite molecular sieve contained two pore channels. Py-FTIR results showed that the addition of HY molecular sieves improved the acidity of the composite zeolite. The crystallization mechanism during the growth of FAU/SBA-15 shell was deduced from the influence of crystallization time on the synthesis of FAU/SBA-15 core-shell structured composite molecular sieve. HY dissociated partially in H2SO4 solution, and consisted of secondary structural units. This framework structure was more stable than its presence in the isolated form on the same ring or in the absence of Al. Thus it played a guiding role and connected with SBA-15 closely through the Si-O bond. This resulted in the gradual covering of the exterior surface of FAU phase by SBA-15 molecular sieves. The presence of SBA-15 restricted the formation of the other high mass components and increased the selectivity towards ethylbenzene.

Lattice damage and Al-metal precipitation in 2.5 MeV-electron-irradiated AlH3

NASA Astrophysics Data System (ADS)

Zogal, O. J.; Vajda, P.; Beuneu, F.; Pietraszko, A.

1998-04-01

AlH3 powder was bombarded with energetic electrons at 20 K and at room temperature and investigated by EPR, NMR, X-ray diffractometry, and microwave dielectric-constant measurements. The EPR spectra of the irradiated powder and of a selected single crystal cuboid of ˜ {10^{ - 1}} mm edge show a complex asymmetric line centered at g = 2.009, with a Curie-like temperature dependence, attributed to radiation-induced color centers and/or their agglomerates. At the same time, the grains, which have become shiny black after irradiation, exhibit an increase of both the real and the imaginary part of ɛ. 27Al-NMR spectra of the irradiated powder present a Knight-shifted line at 1600(50) ppm, close to the position of bulk metallic Al, and corresponding to a concentration of c(Al) ˜ {10^{ - 1}}. In addition, the main hydride line differs from that before irradiation, demonstrating an alteration of environmental symmetry. The irradiation induces also a change in shape and width of the 1H-NMR line, another indication of symmetry change in the lattice. Finally, a refined X-ray single-crystal structure analysis of the irradiated cuboid indicates a change of structure from trigonal R -3 c to R -3, with a loss of mirror symmetry for the two Al sites caused by the introduction of Al-defects in the vicinity of one of them.

Soft chemistry routes for synthesis of rare earth oxide nanoparticles with well defined morphological and structural characteristics

NASA Astrophysics Data System (ADS)

Mancic, L.; Marinkovic, B. A.; Marinkovic, K.; Dramicanin, M.; Milosevic, O.

2011-11-01

Phosphors of (Y0.75Gd0.25)2O3:Eu3+ (5 at.%) have been prepared through soft chemistry routes. Conversion of the starting nitrates mixture into oxide is performed through two approaches: (a) hydrothermal treatment (HT) at 200 °C/3 h of an ammonium hydrogen carbonate precipitated mixture and (b) by thermally decomposition of pure nitrate precursor solution at 900 °C in dispersed phase (aerosol) within a tubular flow reactor by spray pyrolysis process (SP). The powders are additionally thermally treated at different temperatures: 600, 1000, and 1100 °C for either 3 or 12 h. HT—derived particles present exclusively one-dimensional morphology (nanorods) up to the temperatures of 600 °C, while the leaf-like particles start to grow afterward. SP—derived particles maintain their spherical shape up to the temperatures of 1100 °C. These submicron sized spheres were actually composed of randomly aggregated nanoparticles. All powders exhibits cubic Ia- 3 structure (Y0.75Gd0.25)2O3:Eu and have improved optical characteristics due to their nanocrystalline nature. The detailed study of the influence of structural and morphological powder characteristics on their emission properties is performed based on the results of X-ray powder diffractometry, scanning electron microscopy, X-ray energy dispersive spectroscopy, transmission electron microscopy, and photoluminescence measurements.

Morphology and structure features of ZnAl{sub 2}O{sub 4} spinel nanoparticles prepared by matrix-isolation-assisted calcination

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

Du, Xuelian, E-mail: xueliandu@126.com; Li, Liqiang; Zhang, Wenxing

2015-01-15

Graphical abstract: The substrate ZnO as the isolation medium is effective in preventing the sintering and agglomeration of ZnAl{sub 2}O{sub 4} nanoparticles, and it also prevents their contamination. High purity, well-dispersed, and single-crystal ZnAl{sub 2}O{sub 4} nanoparticles with 3.72 eV band gap were obtained. - Abstract: Well-dispersed ZnAl{sub 2}O{sub 4} spinel nanoparticles with an average crystalline size of 25.7 nm were synthesized successfully and easily by polymer-network and matrix-isolation-assisted calcination. The product microstructure and features were investigated by X-ray diffractometry, thermogravimetric and differential thermal analysis, Fourier transform-infrared spectroscopy, N{sub 2} adsorption–desorption isotherms, and energy dispersive X-ray spectra. The morphology andmore » optical performance of the as-prepared ZnAl{sub 2}O{sub 4} nanoparticles were characterized by scanning electron microscope, transmission electron microscopy, and photoluminescence spectrometer. Experimental results indicate that excess ZnO acted as the isolation medium is effective in preventing the sintering and agglomeration of ZnAl{sub 2}O{sub 4} nanoparticles, and it also prevents their contamination. Then, high purity and well-dispersed ZnAl{sub 2}O{sub 4} nanoparticles with single-crystal structure were obtained.« less

Correlation Between the Extent of Catalytic Activity and Charge Density of Montmorillonites

PubMed Central

Steudel, Annett; Emmerich, Katja; Lagaly, Gerhard; Schuhmann, Rainer

2010-01-01

Abstract The clay mineral montmorillonite is a member of the phyllosilicate group of minerals, which has been detected on martian soil. Montmorillonite catalyzes the condensation of activated monomers to form RNA-like oligomers. Extent of catalysis, that is, the yield of oligomers, and the length of the longest oligomer formed in these reactions widely varies with the source of montmorillonite (i.e., the locality where the mineral is mined). This study was undertaken to establish whether there exists a correlation between the extent of catalytic property and the charge density of montmorillonites. Charge density was determined by saturating the montmorillonites with alkyl ammonium cations that contained increasing lengths of alkyl chains, [CH3-(CH2)n-NH3]+, where n = 3–16 and 18, and then measuring d(001), interlayer spacing of the resulting montmorillonite-alkyl ammonium-montmorillonite complex by X-ray diffractometry (XRD). Results demonstrate that catalytic activity of montmorillonites with lower charge density is superior to that of higher charge density montmorillonite. They produce longer oligomers that contain 9 to 10 monomer units, while montmorillonite with high charge density catalyzes the formation of oligomers that contain only 4 monomer units. The charge density of montmorillonites can also be calculated from the chemical composition if elemental analysis data of the pure mineral are available. In the next mission to Mars, CheMin (Chemistry and Mineralogy), a combined X-ray diffraction/X-ray fluorescence instrument, will provide information on the mineralogical and elemental analysis of the samples. Possible significance of these results for planning the future missions to Mars for the search of organic compounds and extinct or extant life is discussed. Key Words: Mars—Origin of life—Montmorillonite—Mineral catalysis—Layer charge density—X–ray diffractometry. Astrobiology 10, 743–749. PMID:20854214

Biocompatibility of the micro-patterned NiTi surface produced by femtosecond laser

NASA Astrophysics Data System (ADS)

Liang, Chunyong; Wang, Hongshui; Yang, Jianjun; Li, Baoe; Yang, Yang; Li, Haipeng

2012-11-01

Biocompatibility of the micro-patterned NiTi surface produced by femtosecond laser (FSL) was studied in this work. The surface characteristics of the laser treated NiTi alloys were investigated by scanning electron microscopy (SEM), atom force microscopy (AFM), X-ray diffractometry (XRD) and X-ray photoelectron spectrum (XPS). The biocompatibility was evaluated by in vitro cell culture test. The results showed that, grooves, ripples, which covered by nanoparticles were formed on the sample surfaces, and the Ni/Ti ratio on the alloy surface increased with increasing laser energy. The crystal structure was not changed by laser treatment. However, the cell culture test proved that the micro-patterns induced by FSL were beneficial to improve the biocompatibility of NiTi alloys: the growth of osteoblasts oriented along the grooves, a large amount of synapses and filopodias were formed due to the ripples, holes and nanoparticles on the alloy surface, and the proliferation rate and alkaline phosphatase (ALP) content of cells were increased after FSL treatment. However, due to the toxicity of Ni ions on cell growth, the NiTi alloy surface should not be treated by laser fluence of more than 3.82 J/cm2 to obtain the ideal biocompatibility.

Investigation on microstructure and mechanical properties of Mo2FeB2 based cermets with and without PVA

NASA Astrophysics Data System (ADS)

Shen, Yupeng; Huang, Zhifu; Jian, Yongxin; Yang, Ming; Li, Kemin

2018-03-01

Mo2FeB2 based cermets with and without PVA have been investigated by x-ray diffractometry (XRD), x-ray photoelectron spectroscope (XPS) and scanning electron microscopy (SEM). The density and transverse rupture strength (TRS) of green compact, relative density, hardness (HRA), fracture toughness (KIC) and TRS of Mo2FeB2 based cermets were also measured. The results indicate that, compared with the Mo2FeB2 based cermets without PVA, the density of green compact with PVA can be improved slightly at the same pressure. However, the much higher TRS is obtained for the green compact without PVA. Meanwhile, Mo2FeB2 particles exhibit the finer and less congruity feature for Mo2FeB2 based cermets without PVA. In addition, the higher relative density, hardness, fracture toughness and TRS can be acquired for the cermets without PVA. Obviously, considering the mechanical properties and preparation period of Mo2FeB2 based cermets, no adding PVA is the optimized process of powder molding in the manufacture of Mo2FeB2 based cermets.

Preparation of MWCNT-Fe3O4 Nanocomposites from Iron Sand Using Sonochemical Route

NASA Astrophysics Data System (ADS)

Rahmawati, R.; Melati, A.; Taufiq, A.; Sunaryono; Diantoro, M.; Yuliarto, B.; Suyatman, S.; Nugraha, N.; Kurniadi, D.

2017-05-01

The composites of multi-walled carbon nanotube (MWCNT) and magnetite (Fe3O4) nanoparticles from iron sand were successfully prepared via the sonochemical route. In this experiment, the MWCNT-Fe3O4 nanocomposites were prepared with different compositions of MWCNT (0.01%, 0.02%, and 0.04%) with the constant composition of Fe3O4 particles. The characterizations were performed by means of X-Ray Diffractometry (XRD), Fourier Transform Infra-Red (FTIR) Spectrometer and Scanning Electron Microscopy (SEM) integrated with Energy Dispersive X-Ray (EDX). The XRD data analysis showed that the Fe3O4 crystallize in spinel structure in nanometric size. Furthermore, the crystallinity of the samples tended to reduce by increasing the MWCNT compositions. The SEM images showed that Fe3O4 tend to agglomerate in nanometric size. The FTIR spectra detected the functional groups of Fe-O bonding that showed the existence of Fe2+ and Fe3+. In the composites, the Fe3O4 nanoparticles were physically mixed with the MWCNTs constructing a unique structure. The as prepared MWCNT-Fe3O4 nanocomposites have the potential for bio-applications.

Improving the tribocorrosion resistance of Ti6Al4V surface by laser surface cladding with TiNiZrO2 composite coating

NASA Astrophysics Data System (ADS)

Obadele, Babatunde Abiodun; Andrews, Anthony; Mathew, Mathew T.; Olubambi, Peter Apata; Pityana, Sisa

2015-08-01

Ti6Al4V alloy was laser cladded with titanium, nickel and zirconia powders in different ratio using a 2 kW CW ytterbium laser system (YLS). The microstructures of the cladded layers were examined using field emission scanning electron microscopy (FESEM) equipped with energy dispersive X-ray spectroscopy (EDS) and X-ray diffractometry (XRD). Corrosion and tribocorrosion tests were performed on the cladded surface in 1 M H2SO4 solution. The microstructure revealed the transformation from a dense dendritic structure in TiNi coating to a flower-like structure observed in TiNiZrO2 cladded layers. There was a significant increase in surface microindentation hardness values of the cladded layers due to the present of hard phase ZrO2 particles. The results obtained show that addition of ZrO2 improves the corrosion resistance property of TiNi coating but decrease the tribocorrosion resistance property. The surface hardening effect induced by ZrO2 addition, combination of high hardness of Ti2Ni phase could be responsible for the mechanical degradation and chemical wear under sliding conditions.

Pulse electrodeposition of self-lubricating Ni-W/PTFE nanocomposite coatings on mild steel surface

NASA Astrophysics Data System (ADS)

Sangeetha, S.; Kalaignan, G. Paruthimal; Anthuvan, J. Tennis

2015-12-01

Ni-W/PTFE nanocomposite coatings with various contents of PTFE (polytetafluoroethylene) particles were prepared by pulse current (PC) electrodeposition from the Ni-W plating bath containing self lubricant PTFE particles to be co-deposited. Co-deposited PTFE particulates were uniformly distributed in the Ni-W alloy matrix. The coatings were characterized by Scanning Electron Microscopy (SEM), Energy Dispersive X-Ray Analysis (EDAX), X-ray Diffractometry (XRD) and Vicker's micro hardness tester. Tafel Polarization and electrochemical Impedance methods were used to evaluate the corrosion resistance behaviour of the nanocomposite coatings in 3.5% NaCl solution. It was found that, the Ni-W/PTFE nanocomposite coating has better corrosion resistance than the Ni-W alloy coating. Surface roughness and friction coefficient of the coated samples were assessed by Mitutoyo Surftest SJ-310 (ISO1997) and Scratch tester TR-101-M4 respectively. The contact angle (CA) of a water droplet on the surface of nanocomposite coating was measured by Optical Contact Goniometry (OCA 35). These results indicated that, the addition of PTFE in the Ni-W alloy matrix has resulted moderate microhardness, smooth surface, less friction coefficient, excellent water repellency and enhanced corrosion resistance of the nanocomposite coatings.

Capillary optics for radiation focusing

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

Peurrung, A.J.; Reeder, P.L.; Bliss, M.

Capillary lens technology may ultimately bring benefits to neutron and x-ray-based science like conventional lenses with visible light. Although the technology is not yet 10 years old, these lenses have already had a significant impact in engineering, science, and medicine. Capillary lenses are advantageous when it is desirable to increase the radiation flux at a location without regard to its angular divergence. PNNL has worked to improve the technology in several ways. A single, optimally tapered capillary was manufactured, which allows intensity gains of a factor of 270 for an initially parallel, incident x-ray beam. Feasibility of constructing neutron lensesmore » using {sup 58}Ni (particularly effective at reflecting neutrons) has been explored. Three applications for capillary optics have been identified and studied: neutron telescope, Gandolphi x-ray diffractometry, and neutron radiotherapy. A brief guide is given for determining which potential applications are likely to be helped by capillary optics.« less

A Compact X-Ray System for Support of High Throughput Crystallography

NASA Technical Reports Server (NTRS)

Ciszak, Ewa; Gubarev, Mikhail; Gibson, Walter M.; Joy, Marshall K.; Whitaker, Ann F. (Technical Monitor)

2001-01-01

Standard x-ray systems for crystallography rely on massive generators coupled with optics that guide X-ray beams onto the crystal sample. Optics for single-crystal diffractometry include total reflection mirrors, polycapillary optics or graded multilayer monochromators. The benefit of using polycapillary optic is that it can collect x-rays over tile greatest solid angle, and thus most efficiently, utilize the greatest portion of X-rays emitted from the Source, The x-ray generator has to have a small anode spot, and thus its size and power requirements can be substantially reduced We present the design and results from the first high flux x-ray system for crystallography that combine's a microfocus X-ray generator (40microns FWHM Spot size at a power of 45 W) and a collimating, polycapillary optic. Diffraction data collected from small test crystals with cell dimensions up to 160A (lysozyme and thaumatin) are of high quality. For example, diffraction data collected from a lysozyme crystal at RT yielded R=5.0% for data extending to 1.70A. We compare these results with measurements taken from standard crystallographic systems. Our current microfocus X-ray diffraction system is attractive for supporting crystal growth research in the standard crystallography laboratory as well as in remote, automated crystal growth laboratory. Its small volume, light-weight, and low power requirements are sufficient to have it installed in unique environments, i.e.. on-board International Space Station.

Heteroepitaxial growth of Ge films on (100) GaAs by pyrolysis of digermane

NASA Astrophysics Data System (ADS)

Eres, Djula; Lowndes, Douglas H.; Tischler, J. Z.; Sharp, J. W.; Geohegan, D. B.; Pennycook, S. J.

1989-08-01

Pyrolysis of high-purity digermane (Ge2 H6 ) has been used to grow epitaxial Ge films of high crystalline quality on (100) GaAs substrates in a low-pressure environment. X-ray double-crystal diffractometry shows that fully commensurate, coherently strained epitaxial Ge films can be grown on (100) GaAs at digermane partial pressures of 0.05-40 mTorr for substrate temperatures of 380-600 °C. Amorphous films also were deposited. Information about the crystalline films surface morphology, growth mode, and microstructure was obtained from scanning electron microscopy, cross-section transmission electron microscopy, and in situ reflectivity measurements. The amorphous-to-crystalline transition temperature and the morphology of the crystalline films were both found to depend on deposition conditions (primarily the incidence rate of Ge-bearing species and the substrate temperature). Epitaxial growth rates using digermane were found to be about two orders of magnitude higher than rates using germane (GeH4 ) under similar experimental conditions.

Fine Structure Study of the Plasma Coatings B4C-Ni-P

NASA Astrophysics Data System (ADS)

Kornienko, E. E.; Bezrukova, V. A.; Kuz'min, V. I.; Lozhkin, V. S.; Tutunkova, M. K.

2017-12-01

The article considers structure of coatings formed of the B4C-Ni-P powder. The coatings were deposited using air-plasma spraying with the unit for annular injection of powder. The pipes from steel 20 (0.2 % C) were used as a substrate. The structure and phase composition of the coatings were studied by optical microscopy, scanning electron microscopy, transmission electron microscopy and X-ray diffractometry. It is shown that high-density composite coatings consisting of boron carbide particles distributed in the nickel boride metal matrix are formed using air-plasma spraying. The areas with round inclusions characterized by the increased amount of nickel, phosphorus and boron are located around the boron carbide particles. Boron oxides and nickel oxides are also present in the coatings. Thin interlayers with amorphous-crystalline structure are formed around the boron carbide particles. The thickness of these interlayers does not exceed 1 μm. The metal matrix material represents areas with nanocrystalline structure and columnar crystals.

Analysis of NiAlTa precipitates in beta-NiAl + 2 at. pct Ta alloy

NASA Technical Reports Server (NTRS)

Pathare, V.; Michal, G. M.; Vedula, K.; Nathal, M. V.

1987-01-01

Results are reported from experiments performed to identify the precipitates, and their orientation in the matrix, in a beta-NiAl alloy containing 2 at. pct. Ta after undergoing creep test at 1300 K. Test specimens formed by extruding hot powders were compressed at 1300 K for about 50 hr at a strain rate averaging 6/1 million per sec. The specimens were then thinned and examined under an electron microscope and by X-ray diffractometry. An intermetallic NiAlTa compound with a hexagonal Cl4 structure appeared as second phase precipitates in the samples, exhibiting plate-like shapes and a habit plane close to (012). The prism planes of the hexagonal NiAlTa precipitates paralleled the closest packed planes in the cubic beta-NiAl matrix.

Gold leaf counter electrodes for dye-sensitized solar cells

NASA Astrophysics Data System (ADS)

Shimada, Kazuhiro; Toyoda, Takeshi

2018-03-01

In this study, a gold leaf 100 nm thin film is used as the counter electrode in dye-sensitized solar cells. The traditional method of hammering gold foil to obtain a thin gold leaf, which requires only small amounts of gold, was employed. The gold leaf was then attached to the substrate using an adhesive to produce the gold electrode. The proposed approach for fabricating counter electrodes is demonstrated to be facile and cost-effective, as opposed to existing techniques. Compared with electrodes prepared with gold foil and sputtered gold, the gold leaf counter electrode demonstrates higher catalytic activity with a cobalt-complex electrolyte and higher cell efficiency. The origin of the improved performance was investigated by surface morphology examination (scanning electron microscopy), various electrochemical analyses (cyclic voltammetry, linear sweep voltammetry, and electrochemical impedance spectroscopy), and crystalline analysis (X-ray diffractometry).

[Study on the traditional lime mortar from the memorial archway in the southern Anhui province].

PubMed

Wei, Guo-Feng; Sun, Sheng; Wang, Cheng-Xing; Zhang, Bing-Jian; Chen, Xi-Min

2013-07-01

The traditional lime mortar was investigated by means of scanning electron microscope (SEM), X-ray diffractometry and Fourier transform infrared spectrometry (FTIR). The results show that the mortar from the memorial archway in the southern Anhui province was the organic-inorganic composite materials composed of lime with tung oil or sticky rice. It was found that the excellent performance of the tung oil-lime mortar can be explained by the compact lamellar organic-inorganic composite structure that was produced by carbonization reaction of lime, cross-linking reactions of tung oil and oxygen and complexing reaction of Ca2+ and -COO-. The compact micro-structure of sticky rice-lime mortar, which was produced due to carbonation process of lime controlled by amylopectin, should be the cause of the good performance of this kind of organic-inorganic mortar.

Ultrasonic spray pyrolysis synthesis of reduced graphene oxide/anatase TiO2 composite and its application in the photocatalytic degradation of methylene blue in water.

PubMed

Park, Jeong-Ann; Yang, Boram; Lee, Joongki; Kim, In Gyeom; Kim, Jae-Hyun; Choi, Jae-Woo; Park, Hee-Deung; Nah, In Wook; Lee, Sang-Hyup

2018-01-01

Reduced graphene oxide (RGO)/anatase TiO 2 composite was prepared using a simple one-step technique-ultrasonic spray pyrolysis-in order to inhibit the aggregation of TiO 2 nanoparticles and to improve the photocatalytic performance for degradation of methylene blue (MB). Different proportions (0-5 wt%) of RGO/TiO 2 composites were characterized by scanning electronic microscopy (SEM), dispersive X-ray spectrometry (EDS), transmission electron microscopy (TEM), Brunauer-Emmett-Teller (BET) surface area, X-ray photoelectron spectroscopy (XPS), X-ray diffractometry (XRD), Raman spectroscopy, UV-vis spectroscopy, and electrochemical impedance spectroscopy (EIS) to verify mechanism. From these analysis, TiO 2 nanoparticles are distributed uniformly on the RGO sheets with crumpled shape during ultrasonic spray pyrolysis and surface area is increasing by increasing portion of RGO. Band gap of RGO 5 /TiO 2 (5 wt% of RGO) composite is 2.72 eV and band gap was reduced by increasing portion of RGO in RGO/TiO 2 composites. The RGO 5 /TiO 2 composite was superior to other lower content of RGO/TiO 2 composites with a rapid transport of charge carriers and an effective charge separation. The highest removal efficiency of MB was obtained at the RGO 5 /TiO 2 composite under UVC irradiation, which coincided with the EIS, and the optimal dose of the composite was determined to be 0.5 g/L. The RGO 5 /TiO 2 composite improve the photocatalytic degradation rate of MB over the TiO 2 due to a retardation of electron-hole recombination. The MB adsorption capacity and photocatalytic degradation efficiency were greatly affected by pH changes and increased with increasing pH due to electrostatic interactions and generation of more hydroxyl radicals. The reusability of RGO 5 /TiO 2 composite was examined during 3 cycles. Copyright © 2017 Elsevier Ltd. All rights reserved.

Gradient doping - a case study with Ti-Fe2O3 towards an improved photoelectrochemical response.

PubMed

Srivastav, Anupam; Verma, Anuradha; Banerjee, Anamika; Khan, Saif A; Gupta, Mukul; Satsangi, Vibha Rani; Shrivastav, Rohit; Dass, Sahab

2016-12-07

The present study investigates the effect of gradient doping on modifying the photoelectrochemical response of Ti-doped Fe 2 O 3 photoanodes for their use in sunlight based water splitting for hydrogen evolution. The deposition of a thin film over the ITO (tin doped indium oxide) substrate was carried out using a spray pyrolysis method. The concentration of dopant was varied from 0.5-8.0 at% and two sets of samples were also prepared with low to high (0.5-8%) and high to low (8-0.5%) dopant concentrations in the direction towards the substrate. The prepared thin films were characterized using X-ray Diffractometry (XRD), Scanning Electron Microscopy (SEM), Energy Dispersive X-ray (EDX) Spectroscopy, Secondary Ion Mass Spectroscopy (SIMS), X-ray Photoelectron Spectroscopy (XPS) and UV-visible Spectroscopy. The photoelectrochemical studies revealed that the deposition of dopant layers with a low to high concentration towards the substrate exhibited a highly improved photoresponse (200 times) in comparison to the pristine sample and a two fold enhancement in comparison to 2% Ti-doped Fe 2 O 3 . The improvement in the photoresponse has been attributed to the values of a high flat band potential, low resistance, high open circuit voltage, carrier separation efficiency, applied bias photon-to-current conversion efficiency (ABPE), and incident photon-to-current conversion efficiency (IPCE). A reduced charge transfer resistance has been demonstrated with Nyquist plots.

An x-ray diffraction study of microstructural deformation induced by cyclic loading of selected steel

NASA Astrophysics Data System (ADS)

Fourspring, Patrick Michael

X-ray double crystal diffractometry (XRDCD) and X-ray scanning diffractometry (XRSD) were used to assess cyclic microstructural deformation in a face centered cubic (fcc) steel (AISI304) and a body centered cubic (bcc) steel (SA508 class 2). The objectives of the investigation were to determine if X-ray diffraction could be used effectively to monitor cyclic microstructural deformation in polycrystalline Fe alloys and to study the distribution of the microstructural deformation induced by cyclic loading in these alloys. The approach used in the investigation was to induce fatigue damage in a material and to characterize the resulting microstructural deformation at discrete fractions of the fatigue life of the material. Also, characterization of microstructural deformation was carried out to identify differences in the accumulation of damage from the surface to the bulk, focusing on the following three regions: near surface (0-10 mum), subsurface (10-300 mum), and bulk. Characterization of the subsurface region was performed only on the AISI304 material because of the limited availability of the SA508 material. The results from the XRDCD data indicate a measurable change induced by fatigue from the initial state to subsequent states of both the AISI304 and the SA508 materials. The results from the XRSD data show similar but less coherent trends than the results from the XRDCD data. Therefore, the XRDCD technique was shown to be sensitive to the microstructural deformation caused by fatigue in steels; thus, the technique can be used to monitor fatigue damage in steels. In addition, for the AISI304 material, the level of cyclic microstructural deformation in the bulk material was found to be greater than the level in the near surface material. In contrast, previous investigations have shown that the deformation is greater in the near surface than the bulk for Al alloys and bcc Fe alloys.

Pseudomorphic GeSiSn, SiSn and Ge layers in strained heterostructures

NASA Astrophysics Data System (ADS)

Timofeev, V. A.; Nikiforov, A. I.; Tuktamyshev, A. R.; Mashanov, V. I.; Loshkarev, I. D.; Bloshkin, A. A.; Gutakovskii, A. K.

2018-04-01

The GeSiSn, SiSn layer growth mechanisms on Si(100) were investigated and the kinetic diagrams of the morphological GeSiSn, SiSn film states in the temperature range of 150 °C-450 °C at the tin content from 0% to 35% were built. The phase diagram of the superstructural change on the surface of Sn grown on Si(100) in the annealing temperature range of 0 °C-850 °C was established. The specular beam oscillations were first obtained during the SiSn film growth from 150 °C to 300 °C at the Sn content up to 35%. The transmission electron microscopy and x-ray diffractometry data confirm the crystal perfection and the pseudomorphic GeSiSn, SiSn film state, and also the presence of smooth heterointerfaces between GeSiSn or SiSn and Si. The photoluminescence for the multilayer periodic GeSiSn/Si structures in the range of 0.6-0.8 eV was detected. The blue shift with the excitation power increase is observed suggesting the presence of a type II heterostructure. The creation of tensile strained Ge films, which are pseudomorphic to the underlying GeSn layer, is confirmed by the results of the formation and analysis of the reciprocal space map in the x-ray diffractometry. The tensile strain in the Ge films reached the value in the range of 0.86%-1.5%. The GeSn buffer layer growth in the Sn content range from 8% to 12% was studied. The band structure of heterosystems based on pseudomorphic GeSiSn, SiSn and Ge layers was calculated and the valence and conduction band subband position dependences on the Sn content were built. Based on the calculation, the Sn content range in the GeSiSn, SiSn, and GeSn layers, which corresponds to the direct bandgap GeSiSn, SiSn, and Ge material, was obtained.

Use of glancing angle X-ray powder diffractometry to depth-profile phase transformations during dissolution of indomethacin and theophylline tablets.

PubMed

Debnath, Smita; Predecki, Paul; Suryanarayanan, Raj

2004-01-01

The purpose of this study was (i) to develop glancing angle x-ray powder diffractometry (XRD) as a method for profiling phase transformations as a function of tablet depth; and (ii) to apply this technique to (a) study indomethacin crystallization during dissolution of partially amorphous indomethacin tablets and to (b) profile anhydrate --> hydrate transformations during dissolution of theophylline tablets. The intrinsic dissolution rates of indomethacin and theophylline were determined after different pharmaceutical processing steps. Phase transformations during dissolution were evaluated by various techniques. Transformation in the bulk and on the tablet surface was characterized by conventional XRD and scanning electron microscopy, respectively. Glancing angle XRD enabled us to profile these transformations as a function of depth from the tablet surface. Pharmaceutical processing resulted in a decrease in crystallinity of both indomethacin and theophylline. When placed in contact with the dissolution medium, while indomethacin recrystallized, theophylline anhydrate rapidly converted to theophylline monohydrate. Due to intimate contact with the dissolution medium, drug transformation occurred to a greater extent at or near the tablet surface. Glancing angle XRD enabled us to depth profile the extent of phase transformations as a function of the distance from the tablet surface. The processed sample (both indomethacin and theophylline) transformed more rapidly than did the corresponding unprocessed drug. Several challenges associated with the glancing angle technique, that is, the effects of sorbed water, phase transformations during the experimental timescale, and the influence of phase transformation on penetration depth, were addressed. Increased solubility, and consequently dissolution rate, is one of the potential advantages of metastable phases. This advantage is negated if, during dissolution, the metastable to stable transformation rate > dissolution rate. Glancing angle XRD enabled us to quantify and thereby profile phase transformations as a function of compact depth. The technique has potential utility in monitoring surface reactions, both chemical decomposition and physical transformations, in pharmaceutical systems.

Effect of Heat Treatment Temperature on Chemical Compositions of Extracted Hydroxyapatite from Bovine Bone Ash

NASA Astrophysics Data System (ADS)

Younesi, M.; Javadpour, S.; Bahrololoom, M. E.

2011-11-01

This article presents the effect of heat treating temperature on chemical composition of hydroxyapatite (HA) that was produced by burning bovine bone, and then heat treating the obtained bone ash at different temperatures in range of 600-1100 °C in air. Bone ash and the resulting white powder from heat treating were characterized by Fourier transformed infrared spectroscopy (FT-IR) and x-ray diffractometry (XRD). The FT-IR spectra confirmed that heat treating of bone ash at temperature of 800 °C removed the total of organic substances. x-ray diffraction analysis showed that the white powder was HA and HA was the only crystalline phase indicated in heat treating product. x-ray fluorescence analyses revealed that calcium and phosphorous were the main elements and magnesium and sodium were minor impurities of produced powder at 800 °C. The results of the energy dispersive x-ray analysis showed that Ca/P ratio in produced HA varies in range of 1.46-2.01. The resulting material was found to be thermally stable up to 1100 °C.

Synchrotron radiation beamline to study radioactive materials at the Photon Factory

NASA Astrophysics Data System (ADS)

Konishi, Hiroyuki; Yokoya, Akinari; Shiwaku, Hideaki; Motohashi, Haruhiko; Makita, Tomoko; Kashihara, Yasuharu; Hashimoto, Shinya; Harami, Taikan; Sasaki, Teikichi A.; Maeta, Hiroshi; Ohno, Hideo; Maezawa, Hideki; Asaoka, Seiji; Kanaya, Noriichi; Ito, Kenji; Usami, Noriko; Kobayashi, Katsumi

1996-02-01

Design and construction of a new beamline have been described. The beamline is housed in a specially designed area controlled for radioactive materials at the Photon Factory (PF) in the National Laboratory for High Energy Physics (KEK). The beamline system consists of a front-end and two branchlines. One of the branchlines is used for X-ray photoelectron spectroscopy and radiation biology in the energy range of 1.8-6 keV and the other for X-ray diffractometry and XAFS studies as well as radiation biology in the range of 4-20 keV. The former was particularly equipped for the protection against accidental scattering of radioactive materials both inside and outside of the vacuum system.

Characterization of ALD grown TixAlyN and TixAlyC thin films

NASA Astrophysics Data System (ADS)

Kinnunen, S. A.; Malm, J.; Arstila, K.; Lahtinen, M.; Sajavaara, T.

2017-09-01

Atomic layer deposition (ALD) was used to grow TixAlyN and TixAlyC thin films using trimethylaluminum (TMA), titanium tetrachloride and ammonia as precursors. Deposition temperature was varied between 325 °C and 500 °C. Films were also annealed in vacuum and N2-atmosphere at 600-1000 °C. Wide range of characterization methods was used including time-of-flight elastic recoil detection analysis (ToF-ERDA), X-ray diffractometry (XRD), X-ray reflectometry (XRR), Raman spectroscopy, ellipsometry, helium ion microscopy (HIM), atomic force microscopy (AFM) and 4-point probe measurement for resistivity. Deposited films were roughly 100 nm thick and contained mainly desired elements. Carbon, chlorine and hydrogen were found to be the main impurities.

Characterization of the modified nickel-zinc ferrite nanoparticles coated with APTES by salinization reaction

NASA Astrophysics Data System (ADS)

Zainal, Israa G.; Al-Shammari, Ahmed Majeed; Kachi, Wjeah

2018-05-01

Surface functionalization of magnetic iron oxide nanoparticles (NPs) is a kind of functional materials, which have been widely used in the biotechnology and catalysis. In this study, Nickel-Zinc ferrite nanoparticles was functionalized with amino propyl triethoxy silane (APTES) by silanization reaction and both non coated and organosilane-coated magnetite characterized by energy-dispersive X-ray spectroscopy (EDX), X-ray diffractometry, Fourier transformed infrared spectroscopy (FTIR) and atomic force microscopy. Basic groups of amino anchored on the external surface of the coated magnetite were observed. Our study procedure nanoparticles which have surface with free - NH2 groups which can carry out ionic interaction with carboxylic groups and act as a carrier of biological molecules, drugs and metals.

Investigations of interatomic interaction in InAs-InAs1-xSbx heterostructures on a base of x-ray diffractometry

NASA Astrophysics Data System (ADS)

Babjuck, T. I.; Buntar, A. G.; Shevtchuk, L. S.

2001-06-01

Hetero-transitions on a base of InAs and AnSb compounds permitted to obtain cheap light diodes and detectors with the atmosphere maximal transparency region sensibility. There is assumed simultaneously, that the phon radiation in InAs-InAs1-xSbx is not large, which positively effects on receiver parameters. Changing the composition of InAs-InAs1- xSbx solution, one may obtain the structure with the width of forbidden zone of the want of 0.35 to 0,1 eV. There is developed the heterostructures crystalline lattice parameters determining method (for substrate and film) with the DRON-3M x-ray diffractometer. There was found the nonlinear dependence of the heterostructures lattice parameter on the composition. Investigations of interatomic interaction in dependence on composition and also on the forbidden zone width Eg(x) have show, that solid solutions InAs-InAs1- xSbx may be used for the obtaining of infra-red receiver.

Investigation of recrystallization of amorphous trehalose through hot-humidity stage X-ray powder diffraction.

PubMed

Jójárt-Laczkovich, Orsolya; Katona, Gábor; Aigner, Zoltán; Szabó-Révész, Piroska

2016-12-01

The aim of this work was an investigation of the physical changes of the amorphous model material spray-dried trehalose through the use of various analytical techniques and to identify a suitable, rapid method able to quantify the changes. The crystallinity changes and recrystallization process of amorphous samples were investigated by hot-humidity stage X-ray powder diffractometry (HH-XRPD) with fresh samples, conventional X-ray powder diffractometry (XRPD) used stored samples and by differential scanning calorimetry (DSC). The data from the three methods were compared and the various forms of trehalose were analysed. HH-XRPD demonstrated that the recrystallization began at 40 and 60°C up to 45% RH and at 70°C up to 30% RH into dihydrate form. At 70°C up to 60% RH the anhydrous form of trehalose appeared too. Conventional XRPD results showed, that in the 28days stored samples the dihydrate form was detected at 40°C, 50% RH. Storage at 60°C, 40% RH resulted in the appearance of the anhydrous form and at 60°C, 50% RH both polymorphic forms were detected. By carrying out the DSC measurements at different temperatures the fraction of recrystallized trehalose dihydrate was detected. The recrystallization investigated by HH-XRPD and DSC followed Avrami kinetics, the calculated rate constants of isothermal crystallization (K) were same. Both HH-XRPD and conventional XRPD was suitable for the detection of the physical changes of the amorphous model material. DSC measurements showed similar results as HH-XRPD. Primarily HH-XRPD could be suggested for prediction, because the method is fast and every changes could be studied on one sample. Copyright © 2016 Elsevier B.V. All rights reserved.

Compression-induced crystallization of amorphous indomethacin in tablets: characterization of spatial heterogeneity by two-dimensional X-ray diffractometry.

PubMed

Thakral, Naveen K; Mohapatra, Sarat; Stephenson, Gregory A; Suryanarayanan, Raj

2015-01-05

Tablets of amorphous indomethacin were compressed at 10, 25, 50, or 100 MPa using either an unlubricated or a lubricated die and stored individually at 35 °C in sealed Mylar pouches. At selected time points, tablets were analyzed by two-dimensional X-ray diffractometry (2D-XRD), which enabled us to profile the extent of drug crystallization in tablets, in both the radial and axial directions. To evaluate the role of lubricant, magnesium stearate was used as "internal" and/or "external" lubricant. Indomethacin crystallization propensity increased as a function of compression pressure, with 100 MPa pressure causing crystallization immediately after compression (detected using synchrotron radiation). However, the drug crystallization was not uniform throughout the tablets. In unlubricated systems, pronounced crystallization at the radial surface could be attributed to die wall friction. The tablet core remained substantially amorphous, irrespective of the compression pressure. Lubrication of the die wall with magnesium stearate, as external lubricant, dramatically decreased drug crystallization at the radial surface. The spatial heterogeneity in drug crystallization, as a function of formulation composition and compression pressure, was systematically investigated. When formulating amorphous systems as tablets, the potential for compression induced crystallization warrants careful consideration. Very low levels of crystallization on the tablet surface, while profoundly affecting product performance (decrease in dissolution rate), may not be readily detected by conventional analytical techniques. Early detection of crystallization could be pivotal in the successful design of a dosage form where, in order to obtain the desired bioavailability, the drug may be in a high energy state. Specialized X-ray diffractometric techniques (2D; use of high intensity synchrotron radiation) enabled detection of very low levels of drug crystallization and revealed the heterogeneity in crystallization within the tablet.

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

Lan, Xiaodong; Wu, Hong, E-mail: wuhong927@126.com

Metallic glass composite coatings Ti{sub 45}Cu{sub 41}Ni{sub 9}Zr{sub 5} and Ti{sub 45}Cu{sub 41}Ni{sub 6}Zr{sub 5}Sn{sub 3} (at.%) on a Ti-30Nb-5Ta-7Zr (wt.%) (TNTZ) alloy were prepared by laser cladding. The microstructures of the coatings were characterized by means of X-ray diffractometry (XRD), scanning electron microscopy (SEM) equipped with energy dispersive X-ray analyzer (EDXA), and transmission electron microscopy (TEM). Results indicated that the coatings have an amorphous structure embedded with a few nanocrystalline phases and dendrites. A partial substitution of Ni by Sn can improve the glass forming ability of Ti-base metallic glass system, and induce the formation of nano-sized Ni{sub 2}SnTimore » phase during the cyclic laser heating. The tribological behavior of both the substrate and the coatings was investigated in detail. A significant improvement in both the hardness and the wear resistance of the coatings was achieved with the addition of Sn. The relationship between the wear resistance and the microstructures of the coatings was discussed. - Highlights: •Ti-based metallic glass composite coatings were prepared by laser cladding. •The wear resistance is greatly improved by laser cladding of composite coatings. •Substitution of Ni by Sn increases GFA and wear resistance of the coatings. •A good balance of crystalline/amorphous phases improves the wear resistance. •Adhesive wear serves as the dominant wear mechanism of the composite coatings.« less

Fluorine incorporation into SnO2 nanoparticles by co-milling with polyvinylidene fluoride

NASA Astrophysics Data System (ADS)

Senna, Mamoru; Turianicová, Erika; Šepelák, Vladimír; Bruns, Michael; Scholz, Gudrun; Lebedkin, Sergei; Kübel, Christian; Wang, Di; Kaňuchová, Mária; Kaus, Maximilian; Hahn, Horst

2014-04-01

Fluorine was incorporated into SnO2 nanoparticles from polyvinylidene fluoride (PVdF) by co-milling. The incorporation process was triggered by an oxidative partial decomposition of PVdF due to the abstraction of oxygen atoms, and began soon after milling with a simultaneous decrease in the crystallite size of SnO2 from 56 nm to 19 nm, and increase in the lattice strain by a factor 7. Appearance of D and G Raman peaks indicated that the decomposition of PVdF was accompanied by the formation of nanometric carbon species. Decomposing processes of PVdF were accompanied by the continuous change in the states of F, with a decrease of C-F in PVdF and increase in Sn-F. This indicates the gradual incorporation of F into SnO2, by replacing a part of oxygen in the oxide with fluorine. These serial mechanochemical reaction processes were discussed on the basis of X-ray diffractometry, FT-IR, Raman and UV-Vis diffuse reflectance spectroscopy, transmission electron microscopy, F1s, Sn3d and C1s X-ray photoelectron spectroscopy and Auger electron spectra, as well as magic angle spinning NMR spectroscopy of 19F and 119Sn. The present findings serve as an initial stage of incorporating fluorine into SnO2 via a solvent-free solid-state process, toward the rational fabrication of fluorine doped SnO2 powders.

Synthesis of core–shell structured FAU/SBA-15 composite molecular sieves and their performance in catalytic cracking of polystyrene

PubMed Central

Du, Jinlong; Shi, Chunwei; Wu, Wenyuan; Bian, Xue; Chen, Ping; Cui, Qingzhu; Cui, Zhixuan

2017-01-01

Abstract Composite molecular sieves, FAU/SBA-15, having core-shell structure were synthesized. The synthesized composite sieves were characterized by X-ray diffractometry (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive X-ray spectroscopy (EDS), pyrolysis fourier transform infrared (Py-FTIR) spectroscopy, temperature programmed desorption spectra (NH3-TPD), UV Raman spectroscopy, nuclear magnetic resonance (NMR) and other techniques. XRD, SEM, TEM, N2 adsorption-desorption, mass spectrometry, NMR and EDS results showed that the composite molecular sieve contained two pore channels. Py-FTIR results showed that the addition of HY molecular sieves improved the acidity of the composite zeolite. The crystallization mechanism during the growth of FAU/SBA-15 shell was deduced from the influence of crystallization time on the synthesis of FAU/SBA-15 core-shell structured composite molecular sieve. HY dissociated partially in H2SO4 solution, and consisted of secondary structural units. This framework structure was more stable than its presence in the isolated form on the same ring or in the absence of Al. Thus it played a guiding role and connected with SBA-15 closely through the Si-O bond. This resulted in the gradual covering of the exterior surface of FAU phase by SBA-15 molecular sieves. The presence of SBA-15 restricted the formation of the other high mass components and increased the selectivity towards ethylbenzene. PMID:29383044

Effect of milling atmosphere on structural and magnetic properties of Ni-Zn ferrite nanocrystalline

NASA Astrophysics Data System (ADS)

Hajalilou, Abdollah; Hashim, Mansor; Ebrahimi-Kahrizsangi, Reza; Masoudi Mohamad, Taghi

2015-04-01

Powder mixtures of Zn, NiO, and Fe2O3 are mechanically alloyed by high energy ball milling to produce Ni-Zn ferrite with a nominal composition of Ni0.36Zn0.64Fe2O4. The effects of milling atmospheres (argon, air, and oxygen), milling time (from 0 to 30 h) and heat treatment are studied. The products are characterized using x-ray diffractometry, field emission scanning electron microscopy equipped with energy-dispersive x-ray spectroscopy, and transmitted electron microscopy. The results indicate that the desired ferrite is not produced during the milling in the samples milled under either air or oxygen atmospheres. In those samples milled under argon, however, Zn/NiO/Fe2O3 reacts with a solid-state diffusion mode to produce Ni-Zn ferrite nanocrystalline in a size of 8 nm after 30-h-milling. The average crystallite sizes decrease to 9 nm and 10 nm in 30-h-milling samples under air and oxygen atmospheres, respectively. Annealing the 30-h-milling samples at 600 °C for 2 h leads to the formation of a single phase of Ni-Zn ferrite, an increase of crystallite size, and a reduction of internal lattice strain. Finally, the effects of the milling atmosphere and heating temperature on the magnetic properties of the 30-h-milling samples are investigated. Project supported by the University Putra Malaysia Graduate Research Fellowship Section.

Enhancing the bioavailability of magnolol in rabbits using melting solid dispersion with polyvinylpyrrolidone.

PubMed

Lin, Shiuan-Pey; Hou, Yu-Chi; Liao, Tzu-Yun; Tsai, Shang-Yuan

2014-03-01

Preparation of magnolol-loaded amorphous solid dispersion was investigated for improving the bioavailability. A solid dispersion of magnolol was prepared with polyvinylpyrrolidone K-30 (PVP) by melting method, and the physical properties were characterized by using differential scanning calorimetry, powder X-ray diffractometry, Fourier transformation-infrared spectroscopy and scanning electron microscope. In addition, dissolution test was also performed. Subsequently, the bioavailability of magnolol pure compound, its physical mixture and solid dispersion were compared in rabbits. The blood samples withdrawn via marginal ear vein at specific time points were assayed by HPLC method. Oral administration of the solid dispersion of magnolol with PVP significantly increased the systemic exposures of magnolol and magnolol sulfates/glucuronides by 80.1% and 142.8%, respectively, compared to those given with magnolol pure compound. Magnolol-loaded amorphous solid dispersion with PVP has demonstrated enhanced bioavailability of magnolol in rabbits.

Asbestiform minerals in ophiolitic rocks of Calabria (southern Italy).

PubMed

Campopiano, Antonella; Olori, Angelo; Spadafora, Alessandra; Rosaria Bruno, Maria; Angelosanto, Federica; Iannò, Antonino; Casciardi, Stefano; Giardino, Renato; Conte, Maurizio; Oranges, Teresa; Iavicoli, Sergio

2018-03-22

Ophiolitic rocks cropping on Calabria territory, southern Italy, can hold asbestiform minerals potentially harmful for human health. The aim of this work was to detect the fibrous phases of ophiolites along the Coastal Chain of northern Calabria and southern part of the Sila massif. Above 220 massive samples were collected in the study areas and analyzed using optical and electron microscopy, X-ray diffractometry, and Fourier transform infra-red spectrometry. The main fibrous constituent belonged to tremolite-actinolite series followed by fibrous antigorite that becomes more abundant in the samples collected in Reventino Mount surroundings. Results highlighted that serpentinites samples mainly consisted of antigorite and minor chrysotile. Samples collected along the coastal chain of northern Calabria did not hold fibrous materials. The results will be useful for Italian natural occurrences of asbestos (NOA) mapping in order to avoid an unintentional exposition by human activity or weathering processes.

Nacre-like calcium carbonate controlled by ionic liquid/graphene oxide composite template.

PubMed

Yao, Chengli; Xie, Anjian; Shen, Yuhua; Zhu, Jinmiao; Li, Hongying

2015-06-01

Nacre-like calcium carbonate nanostructures have been mediated by an ionic liquid (IL)-graphene oxide (GO) composite template. The resultant crystals were characterized by scanning electron microscopy (SEM), Fourier transform infrared (FT-IR) spectroscopy, and X-ray powder diffractometry (XRD). The results showed that either 1-butyl-3-methylimidazolium tetrafluoroborate ([BMIM]BF4) or graphene oxide can act as a soft template for calcium carbonate formation with unusual morphologies. Based on the time-dependent morphology changes of calcium carbonate particles, it is concluded that nacre-like calcium carbonate nanostructures can be formed gradually utilizing [BMIM]BF4/GO composite template. During the process of calcium carbonate formation, [BMIM]BF4 acted not only as solvents but also as morphology templates for the fabrication of calcium carbonate materials with nacre-like morphology. Based on the observations, the possible mechanisms were also discussed. Copyright © 2015 Elsevier B.V. All rights reserved.

Different decay patterns observed in a nineteenth-century building (Palma, Spain).

PubMed

Genestar, Catalina; Pons, Carmen; Cerro, José Carlos; Cerdà, Víctor

2014-01-01

The effects of atmospheric pollutants and climatic conditions were studied in a decayed column in the Seminary of Sant Pere. This nineteenth-century building is situated in the historic centre of Palma (Mallorca, Spain), less than 0.5 km from the sea. Samples were collected from the internal and external part of the crusts formed in the four sides of the column. The samples were analysed by means of thermal analysis, X-ray diffractometry, scanning electron microscopy, Fourier transform infrared spectroscopy and ion chromatography. Results show significant differences in the four sides of the column. A high degree of carbonate stone sulfation is observed in all of the samples analysed. A synergistic effect between atmospheric factors and micropollutants on the deterioration of stone is observed. A high uptake of atmospheric particulate matter is found in the external part of the black crusts.

Synthesis of vaterite and aragonite crystals using biomolecules of tomato and capsicum

NASA Astrophysics Data System (ADS)

Chen, Long; Xu, Wang-Hua; Zhao, Ying-Guo; Kang, Yan; Liu, Shao-Hua; Zhang, Zai-Yong

2012-12-01

In this paper, biomimetic synthesis of calcium carbonate (CaCO3) in the presence of biomolecules of two vegetables-tomato and capsicum is investigated. Scanning electron microscopy and X-ray powder diffractometry were used to characterize the CaCO3 obtained. The biomolecules in the extracts of two vegetables are determined by UV-vis or FTIR. The results indicate that a mixture of calcite and vaterite spheres constructed from small particles is produced with the extract of tomato, while aragonite rods or ellipsoids are formed in the presence of extract of capsicum. The possible formation mechanism of the CaCO3 crystals with tomato biomolecules can be interpreted by particle-aggregation based non-classical crystallization laws. The proteins and/or other biomolecules in tomato and capsicum may control the formation of vaterite and aragonite crystals by adsorbing onto facets of them.

Gold nanoparticle decorated multi-walled carbon nanotubes as counter electrode for dye sensitized solar cells.

PubMed

Kaniyoor, Adarsh; Ramaprabhu, Sundara

2012-11-01

A novel counter electrode material for dye sensitized solar cells (DSSCs) composed of nanostructured Au particles decorated on functionalized multi-walled carbon nanotubes (f-MWNTs) is demonstrated for the first time. MWNTs synthesized by catalytic chemical vapor deposition technique are purified and functionalized by treating with concentrated acids. Au nanoparticles are decorated on f-MWNTs by a rapid and facile microwave assisted polyol reduction method. The materials are characterized by X-ray diffractometry, Fourier transform infra red spectroscopy and electron microscopy. The DSSC fabricated with Au/f-MWNTs based counter electrode shows enhanced power conversion efficiency (eta) of 4.9% under AM 1.5G simulated solar radiation. In comparison, the reference DSSCs fabricated with f-MWNTs and Pt counter electrodes show eta of 2.1% and 4.5%. This high performance of Au/f-MWNTs counter electrode is investigated using electrochemical impedance spectroscopy and cyclic voltammetry studies.

Improvement in the Shape Memory Response of Ti50.5Ni24.5Pd25 High-Temperature Shape Memory Alloy with Scandium Microalloying

NASA Technical Reports Server (NTRS)

Atli, K. C.; Karaman, I; Noebe, R. D.; Garg, A.; Chumlyakov, Y. I.; Kireeva, I. V.

2010-01-01

A Ti(50.5)Ni(24.5)Pd25 high-temperature shape memory alloy (HTSMA) is microalloyed with 0.5 at. pct scandium (Sc) to enhance its shape-memory characteristics, in particular, dimensional stability under repeated thermomechanical cycles. For both Ti(50.5)Ni(24.5)Pd25 and the Sc-alloyed material, differential scanning calorimetry is conducted for multiple cycles to characterize cyclic stability of the transformation temperatures. The microstructure is evaluated using electron microscopy, X-ray diffractometry, and wavelength dispersive spectroscopy. Isobaric thermal cycling experiments are used to determine transformation temperatures, dimensional stability, and work output as a function of stress. The Sc-doped alloy displays more stable shape memory response with smaller irrecoverable strain and narrower thermal hysteresis than the baseline ternary alloy. This improvement in performance is attributed to the solid solution hardening effect of Sc.

Petro-mineralogical Studies of the Paleoproterozoic Phosphorites in the Sonrai basin, Lalitpur District, Uttar Pradesh, India

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

Dar, Shamim A., E-mail: sjshamim@gmail.com; Khan, K. F.; Khan, Saif A.

2015-09-15

The Paleoproterozoic phosphorites constitute an economically significant component of the Sonrai basin of Lalitpur district. These are associated with ferruginous shale, ironstone, limestone and quartz breccia. Petro-mineralogical studies of samples of the phosphorites, using X-ray diffractometry and scanning electron microscopy, reveal that the collophane (carbonate-fluorapatite) is the dominant phosphate mineral. Calcite, dolomite, quartz, mica and haematite are the dominant gangue constituents. The phosphate minerals occur as oolites mutually replaced by carbonate and silica. The presence of iron oxides has been found in most of the thin sections. There is meagre evidence of organic matter in the form of filaments ofmore » microbial phosphate laminae in the samples of phosphorite. The mineral assemblages, their texture and various forms in these phosphorites may be due to some environmental vicissitudes followed by replacement processes and biogenic activities.« less

Fabrication of Ti-0.48Al Alloy by Centrifugal Casting.

PubMed

Park, Jong Bum; Lee, Jung-Il; Ryu, Jeong Ho

2018-09-01

Many of the unique properties of TiAl alloys that make are attractive for use in high-temperature structural applications also make it challenging to process them into useful products. Cast TiAl is rapidly nearing commercialization, particularly in the vehicle industry, owing to its low production cost. In this study, the centrifugal casting of a TiAl (Ti-48%Al, mole fraction) turbocharger was simulated and an experimental casting was created in vacuum using an induction melting furnace coupled to a ceramic composite mold. Numerical simulation results agreed with the experiment. The crystal structure, microstructure, and chemical composition of the TiAl prepared by centrifugal casting were studied by X-ray diffractometry, optical microscopy, field emission scanning electron microscopy (FE-SEM) and energy dispersive spectroscopy (EDS). FE-SEM and EDS examinations of the TiAl casting revealed that the thickness of the oxide layer (α-case) was typically less than 35 μm.

Preparation and characterization of silk sericin/PVA blend film with silver nanoparticles for potential antimicrobial application.

PubMed

He, Huawei; Cai, Rui; Wang, Yejing; Tao, Gang; Guo, Pengchao; Zuo, Hua; Chen, Liqun; Liu, Xinyu; Zhao, Ping; Xia, Qingyou

2017-11-01

Sericin has great potentials in biomedical applications for its good reactive activity, biocompatibility and biodegradability. However, the undesirable mechanical performance limits its application. Here, we developed a green, facile and economic approach to prepare sericin/polyvinyl alcohol (PVA) blend film. Further, silver nanoparticles (AgNPs) were synthesized in situ on the surface of sericin/PVA film via UV-assisted green synthesis method. Mechanical performance, swelling, mass losing and water retention tests showed the blend film had good mechanical performance, hygroscopicity, water retention capacity and low mass losing ratio. Scanning electron microscopy, fourier transfer infrared spectroscopy, X-ray diffractometry diffraction and X-ray photoelectron spectroscopy indicated the blending of PVA and sericin promoted the formation of hydrogen bond network between sericin and PVA, thus enhanced the mechanical performance and the stability of sericin, as well as the hygroscopicity and water retention capacity. UV irradiation and AgNPs modification did not affect the inner crystalline structure of sericin/PVA blend film. The inhibition zone and bacteria growth curve assay suggested AgNPs-sericin/PVA film had good antibacterial activities against E. coli and S. aureus. This novel AgNPs-sericin/PVA film shows great potentials in biomedical materials such as wound dressing and skin tissue engineering. Copyright © 2017 Elsevier B.V. All rights reserved.

Synthesis of microsphere silicon carbide/nanoneedle manganese oxide composites and their electrochemical properties as supercapacitors

NASA Astrophysics Data System (ADS)

Kim, Myeongjin; Yoo, Youngjae; Kim, Jooheon

2014-11-01

Synthesis of microsphere silicon carbide/nanoneedle MnO2 (SiC/N-MnO2) composites for use as high-performance materials in supercapacitors is reported herein. The synthesis procedure involves the initial treatment of silicon carbide (SiC) with hydrogen peroxide to obtain oxygen-containing functional groups to provide anchoring sites for connection of SiC and the MnO2 nanoneedles (N-MnO2). MnO2 nanoneedles are subsequently formed on the SiC surface. The morphology and microstructure of the as-prepared composites are characterized via X-ray diffractometry, field-emission scanning electron microscopy, thermogravimetric analysis, and X-ray photoelectron spectroscopy. The characterizations indicate that MnO2 nanoneedles are homogeneously formed on the SiC surface in the composite. The capacitive properties of the as-prepared SiC/N-MnO2 electrodes are evaluated using cyclic voltammetry, galvanostatic charge/discharge testing, and electrochemical impedance spectroscopy in a three-electrode experimental setup using a 1-M Na2SO4 aqueous solution as the electrolyte. The SiC/N-MnO2(5) electrode, for which the MnO2/SiC feed ratio is 5:1, displays a specific capacitance as high as 273.2 F g-1 at 10 mV s-1.

Synthesis of Ti-6Al-4V alloy with nano-TiN microstructure via spark plasma sintering technique

NASA Astrophysics Data System (ADS)

E Falodun, O.; Obadele, B. A.; Oke, S. R.; E Maja, M.; Olubambi, P. A.

2017-12-01

The effect of nano-TiN dispersion strengthened Ti-6Al-4V via spark plasma sintering method has been investigated. Ti-6Al-4V with 4 vol. percent of nano-TiN were mixed in a Turbula shaker mixer for 8 h at a speed of 49 rpm and the admixed powders were sintered at sintering temperature range of 1000 - 1100 °C, holding time of 10-30 mins, heating rate of 100 °C/min under an applied pressure of 50 MPa. The morphology of the as-received and sintered compacts was examined by scanning electron microscopy (SEM) equipped with energy dispersive X-ray spectroscopy (EDS) and phase analysis was done by X-ray diffractometry (XRD). The sintered compacts without nano-TiN reveal lamellar structure while reinforced Ti-6Al-4V with nano-TiN shows a bimodal structure and titanium nitride has a great influence on a grain growth at high temperature. Furthermore, the microstructural formation mechanism was investigated. With the addition of the content of Ti-6Al-4V with 4 vol.% of nano-TiN, the micro-hardness also improved and this was due to homogenous distribution of TiN in Ti-6Al-4V matrix.

Influence of Sintering Temperature on Mechanical and Physical properties of Mill Scale based Bipolar Plates for PEMFC

NASA Astrophysics Data System (ADS)

Khaerudini, Deni S.; Berliana, Rina; Prakoso, Gatra B.; Insiyanda, Dita R.; Alva, Sagir

2018-03-01

This work concerns the utilization of mill scale, a by-product of iron and steel formed during the hot rolling of steel, as a potential material for use as bipolar plates in proton exchange membrane fuel cells (PEMFCs). On the other hand, mill scale is considered a very rich in iron source having characteristic required such as for current collector in bipolar plate and would significantly contribute to lower the overall cost of PEMFC based fuel cell systems. In this study, the iron reach source of mill scale powder, after sieving of 150 mesh, was mechanically alloyed with the aluminium source containing 30 wt.% using a shaker mill for 3 h. The mixed powders were then pressed at 300 MPa and sintered at various temperatures of 400, 450 and 500 °C for 1 h under inert gas atmosphere. The structural changes of powder particles during mechanical alloying and after sintering were studied by x-ray diffractometry, scanning electron microscopy (SEM) with energy dispersive X-ray spectroscopy (EDX), microhardness measurement, and density - porosity analysis. The details of the performance variation of three different sintering conditions can be preliminary explained by the metallographic and crystallographic structure and phase analysis as well as sufficient mechanical strength of the sintered materials was presented in this report.

Formation of Al3Ti/Mg composite by powder metallurgy of Mg-Al-Ti system.

PubMed

Yang, Zi R; Qi Wang, Shu; Cui, Xiang H; Zhao, Yu T; Gao, Ming J; Wei, Min X

2008-07-01

An in situ titanium trialuminide (Al 3 Ti)-particle-reinforced magnesium matrix composite has been successfully fabricated by the powder metallurgy of a Mg-Al-Ti system. The reaction processes and formation mechanism for synthesizing the composite were studied by differential scanning calorimetry (DSC), x-ray diffractometry (XRD), scanning electron microscopy (SEM) and energy-dispersive x-ray spectroscopy (EDS). Al 3 Ti particles are found to be synthesized in situ in the Mg alloy matrix. During the reaction sintering of the Mg-Al-Ti system, Al 3 Ti particles are formed through the reaction of liquid Al with as-dissolved Ti around the Ti particles. The formed intermetallic particles accumulate at the original sites of the Ti particles. As sintering time increases, the accumulated intermetallic particles disperse and reach a relatively homogeneous distribution in the matrix. It is found that the reaction process of the Mg-Al-Ti system is almost the same as that of the Al-Ti system. Mg also acts as a catalytic agent and a diluent in the reactions and shifts the reactions of Al and Ti to lower temperatures. An additional amount of Al is required for eliminating residual Ti and solid-solution strengthening of the Mg matrix.

X-ray reciprocal space mapping of dislocation-mediated strain relaxation during InGaAs/GaAs(001) epitaxial growth

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

Sasaki, Takuo; Ohshita, Yoshio; Kamiya, Itaru

2011-12-01

Dislocation-mediated strain relaxation during lattice-mismatched InGaAs/GaAs(001) heteroepitaxy was studied through in situ x-ray reciprocal space mapping (in situ RSM). At the synchrotron radiation facility SPring-8, a hybrid system of molecular beam epitaxy and x-ray diffractometry with a two-dimensional detector enabled us to perform in situ RSM at high-speed and high-resolution. Using this experimental setup, four results in terms of film properties were simultaneously extracted as functions of film thickness. These were the lattice constants, the diffraction broadenings along in-plane and out-of-plane directions, and the diffuse scattering. Based on correlations among these results, the strain relaxation processes were classified into fourmore » thickness ranges with different dislocation behavior. In addition, the existence of transition regimes between the thickness ranges was identified. Finally, the dominant dislocation behavior corresponding to each of the four thickness ranges and transition regimes was noted.« less

A novel analytical method for pharmaceutical polymorphs by terahertz spectroscopy and the optimization of crystal form at the discovery stage.

PubMed

Ikeda, Yukihiro; Ishihara, Yoko; Moriwaki, Toshiya; Kato, Eiji; Terada, Katsuhide

2010-01-01

A novel analytical method for the determination of pharmaceutical polymorphs was developed using terahertz spectroscopy. It was found out that each polymorph of a substance showed a specific terahertz absorption spectrum. In particular, analysis of the second derivative spectrum was enormously beneficial in the discrimination of closely related polymorphs that were difficult to discern by powder X-ray diffractometry. Crystal forms that were obtained by crystallization from various solvents and stored under various conditions were specifically characterized by the second derivative of each terahertz spectrum. Fractional polymorphic transformation for substances stored under stressed conditions was also identified by terahertz spectroscopy during solid-state stability test, but could not be detected by powder X-ray diffractometry. Since polymorphs could be characterized clearly by terahertz spectroscopy, further physicochemical studies could be conducted in a timely manner. The development form of compound examined was determined by the results of comprehensive physicochemical studies that included thermodynamic relationships, as well as chemical and physicochemical stability. In conclusion, terahertz spectroscopy, which has unique power in the elucidation of molecular interaction within a crystal lattice, can play more important role in physicochemical research. Terahertz spectroscopy has a great potential as a tool for polymorphic determination, particularly since the second derivative of the terahertz spectrum possesses high sensitivity for pharmaceutical polymorphs.

Quantitative determination of airborne respirable non-fibrous alpha-silicon carbide by x-ray powder diffractometry.

PubMed

Bye, E; Føreland, S; Lundgren, L; Kruse, K; Rønning, R

2009-06-01

The purpose of the present investigation was to establish a method for the determination of airborne respirable non-fibrous silicon carbide (SiC). The main application is within the industrial production of SiC. Due to the complex airborne aerosol mixture of crystalline compounds in the SiC industry, X-ray powder diffractometry was selected as the most appropriate method. Without any international standard material for the respirable fraction of non-fibrous SiC, pure and suitable products from three SiC plants in Norway were selected. These products have a median particle diameter in the range 4.4-5.1 mum. The method is based on thin sample technique, with the dust deposited on a polycarbonate filter. Absorption correction is done by standard procedures with the use of a silver filter, situated below the polycarbonate filter. The diffraction line used for quantitative determination was selected carefully. This was done to avoid interferences from quartz, cristobalite, and graphite, which all are airborne components present in the atmosphere during the industrial process. The instrumental limit of detection for the method is 12 microg. This method has been used to determine airborne non-fibrous SiC in a comprehensive ongoing project in the Norwegian SiC industry for further epidemiological studies. The method is fully applicable for compliance work.

Structural properties of ultrafine Ba-hexaferrite nanoparticles

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

Makovec, Darko, E-mail: Darko.Makovec@ijs.si; Primc, Darinka; Sturm, Saso

2012-12-15

Crystal structure of ultrafine Ba-hexaferrite (BaFe{sub 12}O{sub 19}) nanoparticles was studied using X-ray diffractometry (XRD), high-resolution transmission electron microscopy (HRTEM), energy-dispersive X-ray spectroscopy (EDXS), X-ray absorption fine structure (XAFS), and Moessbauer spectroscopy (MS), to be compared to the structure of larger nanoparticles and the bulk. The nanoparticles were synthesized with hydrothermal treatment of an appropriate suspension of Ba and Fe hydroxides in the presence of a large excess of OH{sup -}. The ultrafine nanoparticles were formed in a discoid shape, {approx}10 nm wide and only {approx}3 nm thick, comparable to the size of the hexagonal unit cell in the c-direction.more » The HRTEM image analysis confirmed the hexaferrite structure, whereas EDXS showed the composition matching the BaFe{sub 12}O{sub 19} formula. XAFS and MS analyses showed considerable disorder of the structure, most probably responsible for the low magnetization. - Graphical abstract: Left: HREM image of an ultrafine Ba-hexaferrite nanoparticle (inset: TEM image of the nanoparticles); Right: the experimental HRTEM image is compared with calculated image and corresponding atomic model. Highlights: Black-Right-Pointing-Pointer Crystal structure of ultrafine Ba-hexaferrite (BaFe{sub 12}O{sub 19}) nanoparticles was compared to the structure of the bulk. Black-Right-Pointing-Pointer Thickness the discoid nanoparticles was comparable to the size of the hexagonal unit cell in the c-direction. Black-Right-Pointing-Pointer Considerable disorder of the nanoparticles' structure is most probably responsible for their low magnetization.« less

Triaxial Measurement Method for Analysis of Residual Stress after High Feed Milling by X-Ray Diffraction

NASA Astrophysics Data System (ADS)

Čuma, Matúš; Török, Jozef; Telišková, Monika

2016-12-01

Surface integrity is a broad term which includes various quality factors affecting the functional properties of parts. Residual stress is one of these factors. Machining generates residual stresses in the surface and subsurface layers of the structural elements. X-ray diffractometry is a non-destructive method applicable for the measurement of residual stresses in surface and subsurface layers of components. The article is focused on the non-destructive progressive method of triaxial measurement of residual stress after machining the surface of sample by high feed milling technology. Significance of triaxial measuring is the capability of measuring in different angles so it is possible to acquire stress tensor containing normal and shear stress components acting in the spot of measuring, using a Cartesian coordinate system.

Morphological characterization and in vitro biocompatibility of a porous nickel-titanium alloy.

PubMed

Prymak, Oleg; Bogdanski, Denise; Köller, Manfred; Esenwein, Stefan A; Muhr, Gert; Beckmann, Felix; Donath, Tilmann; Assad, Michel; Epple, Matthias

2005-10-01

Disks consisting of macroporous nickel-titanium alloy (NiTi, Nitinol, Actipore) are used as implants in clinical surgery, e.g. for fixation of spinal dysfunctions. The morphological properties were studied by scanning electron microscopy (SEM) and by synchrotron radiation-based microtomography (SRmuCT). The composition was studied by X-ray diffractometry (XRD), differential scanning calorimetry (DSC), and energy-dispersive X-ray spectroscopy (EDX). The mechanical properties were studied with temperature-dependent dynamical mechanical analysis (DMA). Studies on the biocompatibility were performed by co-incubation of porous NiTi samples with isolated peripheral blood leukocyte fractions (polymorphonuclear neutrophil granulocytes, PMN; peripheral blood mononuclear leukocytes, PBMC) in comparison with control cultures without NiTi samples. The cell adherence to the NiTi surface was analyzed by fluorescence microscopy and scanning electron microscopy. The activation of adherent leukocytes was analyzed by measurement of the released cytokines using enzyme-linked immunosorbent assay (ELISA). The cytokine response of PMN (analyzed by the release of IL-1ra and IL-8) was not significantly different between cell cultures with or without NiTi. There was a significant increase in the release of IL-1ra (p<0.001), IL-6 (p<0.05), and IL-8 (p<0.05) from PBMC in the presence of NiTi samples. In contrast, the release of TNF-alpha by PBMC was not significantly elevated in the presence of NiTi. IL-2 was released from PBMC only in the range of the lower detection limit in all cell cultures. The material, clearly macroporous with an interconnecting porosity, consists of NiTi (martensite; monoclinic, and austenite; cubic) with small impurities of NiTi2 and possibly NiC(x). The material is not superelastic upon manual compression and shows a good biocompatibility.

Archaeometallurgy in Messina: Iron Slug From A Dig at Blog P, Laboratory Analyses and Interpretation.

NASA Astrophysics Data System (ADS)

Caterina, Ingoglia; Maurizio, Triscari; Giuseppe, Sabatino

The archaeological site in Via La Farina, Block P, in Messina, is unique in many ways, due also to the high quantity of samples of iron slag. The slag was examined to identify the production centres of such materials, and, after characterization, was compared to similar material, exclusively for product typology, from different archaeological sites in the province of Messina, situated in the Peloritani Mountains (Messina city, S. Marco d'Alunzio, Milazzo, Francavilla di Sicilia, Novara di Sicilia as well as the archaeological site of Halaesa, near Tusa). Mineralogical characterization of the phases carried out by X-ray diffractometry (XRD) and Rietveld data elaboration, morphological study of slag findings and a semi-quantitative analysis by scanning electronic microscope (SEM+EDX) were performed. A chemical investigation was carried out by electron probe micro analysis (EPMA), to determine major element,. Minor and trace elements were determined by LA-ICP-MS. All the examined slag is related to iron metallurgy, and, in the case of Via La Farina, there is firm archaeological evidence pinpointing to smelting activity.

Synthesis of Copper-Antimony-Sulfide Nanocrystals for Solution-Processed Solar Cells.

PubMed

Suehiro, Satoshi; Horita, Keisuke; Yuasa, Masayoshi; Tanaka, Tooru; Fujita, Katsuhiko; Ishiwata, Yoichi; Shimanoe, Kengo; Kida, Tetsuya

2015-08-17

The p-type nanocrystals (NCs) of copper-based chalcogenides, such as CuInSe2 and Cu2ZnSnS4, have attracted increasing attention in photovoltaic applications due to their potential to produce cheap solution-processed solar cells. Herein, we report the synthesis of copper-antimony-sulfide (CAS) NCs with different crystal phases including CuSbS2, Cu3SbS4, and Cu12Sb4S13. In addition, their morphology, crystal phase, and optical properties were characterized using transmission electron microscopy, X-ray diffractometry, UV-vis-near-IR spectroscopy, and photoemission yield spectroscopy. The morphology, crystal phase, and electronic structure were significantly dependent on the chemical composition in the CAS system. Devices were fabricated using particulate films consisting of CAS NCs prepared by spin coating without a high-temperature treatment. The CAS NC-based devices exhibited a diode-like current-voltage characteristic when coupled with an n-type CdS layer. In particular, the CuSbS2 NC devices exhibited photovoltaic responses under simulated sunlight, demonstrating its applicability for use in solution-processed solar cells.

Reduced graphene oxide-CdS nanocomposite with enhanced photocatalytic 4-Nitrophenol degradation

NASA Astrophysics Data System (ADS)

Chakraborty, Koushik; Ibrahim, Sk; Das, Poulomi; Ghosh, Surajit; Pal, Tanusri

2017-05-01

We report the photocatalytic activity of reduced graphene oxide cadmium sulfide (RGO-CdS) composite towards the degradation of 4-Nitrophenol (4-NP) under simulated solar light illumination. The solution processable RGO-CdS composite was synthesized by one pot single step low cost solvothermal process, where the reduction of graphene oxide (GO), synthesis and attachment of CdS onto RGO sheets were done simultaneously. The structural and morphological characterization of the RGO-CdS composite and the reduction of GO was confirmed by X-ray diffractometry, TEM imaging and Fourier transform infrared spectroscopy respectively. The photocatalytic efficiency of RGO-CdS composite is 2.6 times higher in compare to controlled CdS. In RGO-CdS composite the photo induced electrons transfer from CdS nanorod to RGO sheets, which reduces the recombination probability of photo generated electron-hole in the CdS. These well separated photoinduced charges enhanced the photocatalytic activity of the RGO-CdS composite. Our study establishes the RGO-CdS composite as a potential photocatalyst for the degradation of organic water pollutant.

Different preparation methods and characterization of magnetic maghemite coated with chitosan

NASA Astrophysics Data System (ADS)

Hojnik Podrepšek, Gordana; Knez, Željko; Leitgeb, Maja

2013-06-01

The preparation of maghemite (γ-Fe2O3) micro- and nanoparticles coated with chitosan, used as carriers for immobilized enzymes, was investigated. γ-Fe2O3 nanoparticles were synthesized by coprecipitation of Fe2+ and Fe3+ ions in the presence of ammonium. They were coated with chitosan by the microemulsion process, suspension cross-linking technique, and covalent binding of chitosan on the γ-Fe2O3 surface. The methods distinguished the concentration of chitosan, concentration of acetic acid solution, concentration of a cross-linking agent, temperature of synthesis, pH of the medium, and time of synthesis. γ-Fe2O3 micro- and nanoparticles coated with chitosan prepared after three preparation methods were evaluated by scanning electron microscopy, transmission electron microscopy, Fourier transform infrared spectroscopy analysis, energy dispersive spectrometry, thermogravimetric analysis, differential scanning calorimetry analysis, vibrating sample magnetometry, dynamic light scattering, laser diffraction granulometry, and X-ray diffractometry. These positive attributes demonstrated that these magnetic micro- and nanoparticles coated with chitosan may be used as a promising carrier for further diverse biomedical applications.

Electronic, optical and photocatalytic behavior of Mn, N doped and co-doped TiO{sub 2}: Experiment and simulation

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

Zhao, Ya Fei; Li, Can, E-mail: canli1983@gmail.com; Lu, Song

2016-03-15

The crystal phase structure, surface morphology, chemical states and optical properties of Mn, N mono-doped and co-doped TiO{sub 2} nanoparticles were investigated by X-ray powder diffractometry, Raman spectra, scanning electron microscopy, X-ray photoelectron spectroscopy and UV–vis diffuse reflectance spectroscopy. Meanwhile, geometry structures, formation energies, electronic and optical properties of all systems have been also analyzed by density functional theory. The results showed that the band gap values and the carrier mobility in the valence band, conduction band and impurity levels have a synergetic influence on the visible-light absorption and photocatalytic activity of the doped TiO{sub 2}. The number and themore » carrier mobility of impurity level jointly influence the photocatalytic activity of catalyst under visible-light. Especially, the photocatalytic activity of Mn-2N co-doped TiO{sub 2} beyond three-fold than that of pure TiO{sub 2} under visible-light. - Graphical abstract: The ILs formed by N-2p orbital in N single doped specimen lie above the VB, while the ILs formed by Mn-3d orbital in Mn single doped specimen appear below the CB. However, a large amount of ILs formed by N-2p orbital and Mn-3d orbital in N and Mn codoped specimens. The band gap values and the carrier mobility in the valence band, conduction band and impurity levels have a synergetic influence on the visible-light absorption and photocatalytic activity of the doped TiO{sub 2}. The number and the carrier mobility of impurity level jointly influence the photocatalytic activity of catalyst under visible-light.« less

Effect of heavy tempering on microstructure and yield strength of 28CrMo48VTiB martensitic steel

NASA Astrophysics Data System (ADS)

Sun, Yu; Gu, Shunjie; Wang, Qian; Wang, Huibin; Wang, Qingfeng; Zhang, Fucheng

2018-02-01

The 28CrMo48VTiB martensitic steel for sulfide stress cracking (SSC) resistance oil country tubular goods (OCTG) of C110 grade was thermally processed through quenching at 890 °C and tempering at 600 °C-720 °C for 30-90 min. The microstructures of all samples were characterized using field emission scanning electron microscopy (FESEM), electron backscattering diffraction (EBSD), transmission electron microscopy (TEM) and x-ray diffractometry (XRD). Also, the tensile properties were measured. The results indicated that the yield strength (YS) decreased as both the tempering temperature and duration increased, due to the coarsening of martensitic packet/block/lath structures, the reduction of dislocation density, as well as the increase of both the volume fraction and average diameter of the precipitates. The martensitic lath width was the key microstructural parameter controlling the YS of this heavily-tempered martensitic steel, whereas the corresponding relationship was in accordance with the Langford-Cohen model. Furthermore, the martensitic structure boundary and the solid solution strengthening were the two most significant factors dominating the YS, in comparison with the dislocation and precipitation strengthening.

Observation of defect-induced Photoresponse and charge carrier transport in single GeSe2 nanobelt devices

NASA Astrophysics Data System (ADS)

Mukherjee, Bablu; Tok, Eng Soon; Haur Sow, Chorng

2013-03-01

Single crystal GeSe2 nanobelts were grown using chemical vapor deposition techniques. Morphology of the nanostructures was characterized using scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffractometry (XRD) and Raman spectroscopy. Electronic transport properties, impedance spectroscopy, photoconductive characteristics and temperature-dependent electrical resistivity measurements were carried out on individual GeSe2 nanobelt devices. The photosensitivity of single GeSe2 nanobelt (NB) devices was examined with two different excitation wavelengths of laser beams with photon energies above band gap and at sub-band gap of the NB. A maximum photoconductive gain 106 % was achieved at a wavelength of 808 nm. The magnitude of the photocurrent and response time of the individual GeSe2 NB device indicate that the photoresponse could be attributed to the presence of isolated mid band gap defect levels. Temperature dependent photocurrent measurements indicate the rough estimation of the energy levels for the defect states. Localized photostudy shows that the large photoresponse of the device primarily occurs at the metal-NB contact regions. Department of Physics, 2 Science Drive 3, National University of Singapore (NUS), Singapore 117542

Modified extrusion-spheronization as a technique of microencapsulation for stabilization of choline bitartrate using hydrogenated soya bean oil.

PubMed

Gangurde, Avinash Bhaskar; Sav, Ajay Kumar; Javeer, Sharadchandra Dagadu; Moravkar, Kailas K; Pawar, Jaywant N; Amin, Purnima D

2015-01-01

Choline bitartrate (CBT) is a vital nutrient for fetal brain development and memory function. It is hygroscopic in nature which is associated with stability related problem during storage such as development of fishy odor and discoloration. Microencapsulation method was adopted to resolve the stability problem and for this hydrogenated soya bean oil (HSO) was used as encapsulating agent. Industrially feasible modified extrusion-spheronization technique was selected for microencapsulation. HSO was used as encapsulating agent, hydroxypropyl methyl cellulose E5/E15 as binder and microcrystalline cellulose as spheronization aid. Formulated pellets were evaluated for parameters such as flow property, morphological characteristics, hardness-friability index (HFI), drug content, encapsulation efficiency, and in vitro drug release. The optimized formulations were also characterized for particle size (by laser diffractometry), differential scanning calorimetry, powder X-ray diffractometry (PXRD), Fourier transform infrared spectroscopy, and scanning electron microscopy. The results from the study showed that coating of 90% and 60% CBT was successful with respect to all desired evaluation parameters. Optimized formulation was kept for 6 months stability study as per ICH guidelines, and there was no change in color, moisture content, drug content, and no fishy odor was observed. Microencapsulated pellets of CBT using HSO as encapsulating agent were developed using modified extrusion spheronization technique. Optimized formulations, CBT 90% (F5), and CBT 60% (F10), were found to be stable for 4M and 6M, respectively, at accelerated conditions.

Mineralogical variation in the size fractions of a Ranong kaolin, southern Thailand

NASA Astrophysics Data System (ADS)

Pisutha-Arnond, Visut; Phuvichit, Suraphol; Leepowpanth, Quanchai

A representative crude Ranong kaolin from the Thungkla-Ranong mine was separated into > 2 mm (granule), 2-1 mm (very coarse sand), 1-0.5 mm (coarse sand), 0.5-0.25 mm (medium sand), 0.25-0.125 mm (fine sand), 0.125-0.062 mm (very fine sand) and 62-28, 28-14, 17-7, 7-4, 4-2, 2-1 and < 1 μ m size fractions. Those size fractions were analyzed by X-ray powder diffractometry (XRD), differential thermal analysis (DTA), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) with attached energy dispersive X-ray spectrometer (EDX). Kaolin group minerals were differentiated by using XRD in combination with various chemical and heat treatments together with TEM, SEM and DTA. The Ranong kaolin consists predominantly of tubular halloysite, poorly crystallized kaolinite and quartz with minor amounts of mica and K-feldspars. Other trace constituents include gibbsite, tourmaline, zircon and colored impurities (i.e. extractable iron hydroxide coating on clay mineral surface). The kaolin minerals are found in all size fractions by which their contents and halloysite/kaolinite ratios increase as the particle sizes become finer. Quartz and mica are also detected in almost all size fractions. They are, however, more abundant with coarsening particle size. Gibbsite, K-feldspar and tourmaline are mainly concentrated in the fine sand to silt size fractions. Crystallinity of kaolin minerals as measured by XRD varied moderately with size. Relatively pure kaolin minerals, predominantly halloysite and kaolinite, can be obtained in the particle size below 1 or 2 μm.

Shocked Quartz Aggregates of the Cretaceous-Tertiary Boundary at Colorado, USA

NASA Astrophysics Data System (ADS)

Miura, Y.; Okamoto, M.; Iancu, O. G.

1993-07-01

Shock-metamorphosed quartz (i.e., shocked quartz) at the Cretaceous-Tertiary boundary (K/T) at Colorado [1,2] reveals the following mineralogical data by X-ray diffractometry and high-resolution electron micrograph with energy- dispersive spectrometry. 1. Shocked quartz is not normal (perfect crystalline) quartz mineral but various quartz aggregates that show relatively low X-ray intensity (i.e., imperfect crystalline) and shock lamellae with crystalline quartz and amorphous glass [3]. 2. Analytical electron micrographs indicate that crystalline quartz silica with spotty dislocation features is included in dendritic amorphous glasses of potassium (K) feldspar composition. Various compositions of glassy materials are found in shocked quartz aggregates as matrix or alternate shock lamellae, which is important to estimate the target rock of impact. The composition of glassy matrix is dendritic K-feldspar in the K/T boundary at Clear Creak North (CCN), Colorado, whereas that in the Barringer Crater is quartz-rich composition from the target rock of sandstone (or some mixture with iron meteorite), and that in artificial impact rock [3] is dendritic silica composition. It is found in this study that shocked quartz aggregates from the CCN K/T boundary samples are supplied from quartz and K-feldspar-bearing target rock at impact event (Table 1). Table 1, which appears here in the hard copy, shows the compositions, texture, and origin of shocked quartz aggregates. References: [1] Alvarez L. W. et al. (1980) Science, 208, 1095-1107. [2] Izett G. (1989) GSA Spec. Pap. 249, 1-194. [3] Miura Y. (1991) Shock Waves, 1, 35-41, Springer-Verlag.

Thermal behavior of potato starch and water-vaporization behavior of its paste controlled with amino acid and peptide-rich food materials.

PubMed

Sakauchi, Satoshi; Hattori, Makoto; Yoshida, Tadashi; Yagishita, Takahiro; Ito, Koichi; Akemitsu, Shin-Ichi; Takahashi, Koji

2010-03-01

The particular effect of 4 kinds of amino acid and peptide-rich food material (APRM) containing different charged amino acid contents on the gelatinization and retrogradation behavior of potato starch granules and on the water-vaporization behavior was analyzed by differential scanning calorimetry, rapid viscoanalysis, x-ray diffractometry, thermal gravimetry-differential thermal analysis, and pulsed NMR. APRM with a high-charged amino acid content produced unique gelatinization and retrogradation behavior in terms of an elevated gelatinization temperature, reduced viscosity, higher setback, and lower retrograded starch melting enthalpy. The recovered x-ray diffraction intensity decreased with increasing charged amino acid content. APRM with high-charged amino acid content could provide an improved paste having easy vaporization of external water in the swollen starch granules due to the reduced swelling.

In vitro biocompatibility of magnesium-incorporated submicro-porous titanium oxide surface produced by hydrothermal treatment

NASA Astrophysics Data System (ADS)

Park, Jin-Woo; Kim, Youn-Jeong; Jang, Je-Hee; An, Chang-Hyeon

2010-11-01

This study investigated the surface characteristics and in vitro biocompatibility of titanium (Ti) oxide surface incorporating magnesium ions (Mg), produced by hydrothermal treatment using an alkaline Mg-containing solution, for future biomedical applications. The surface characteristics were evaluated by scanning electron microscopy, thin-film X-ray diffractometry, X-ray photoelectron spectroscopy, inductively coupled plasma-atomic emission spectroscopy (ICP-AES) and optical profilometry. Mouse calvaria-derived osteoblastic cell (MC3T3-E1) attachment, spreading, proliferation, alkaline phosphatase (ALP) activity, and osteoblastic gene expression on Mg-containing surfaces were compared with untreated Ti surfaces. Hydrothermal treatment resulted in Mg-incorporated Ti oxide layer with submicro-porous surface structures approximately 2 μm in thickness. ICP-AES analysis revealed Mg ions release from treated surfaces into the solution. The Mg-incorporated surface displayed significantly increased cellular attachment and ALP activity compared with untreated surface ( p < 0.05), and supported better cell spreading. Real-time polymerase chain reaction analysis showed notably higher mRNA expression of the osteoblast transcription factor genes (Dlx5, Runx2) and the osteoblast phenotype genes (ALP, bone sialoprotein and osteocalcin) in cells grown on the Mg-incorporated surfaces than untreated surfaces. These results demonstrate that the Mg-incorporated submicro-porous Ti oxide surface produced by hydrothermal treatment may improve implant osseointegration by enhancing the attachment, spreading and differentiation of osteoblastic cells.

Enhancement of the dissolution rate and bioavailability of fenofibrate by a melt-adsorption method using supercritical carbon dioxide

PubMed Central

Cha, Kwang-Ho; Cho, Kyung-Jin; Kim, Min-Soo; Kim, Jeong-Soo; Park, Hee Jun; Park, Junsung; Cho, Wonkyung; Park, Jeong-Sook; Hwang, Sung-Joo

2012-01-01

Background: The aim of this study was to enhance the bioavailability of fenofibrate, a poorly water-soluble drug, using a melt-adsorption method with supercritical CO2. Methods: Fenofibrate was loaded onto Neusilin® UFL2 at different weight ratios of fenofibrate to Neusilin UFL2 by melt-adsorption using supercritical CO2. For comparison, fenofibrate-loaded Neusilin UFL2 was prepared by solvent evaporation and hot melt-adsorption methods. The fenofibrate formulations prepared were characterized by differential scanning calorimetry, powder x-ray diffractometry, specific surface area, pore size distribution, scanning electron microscopy, and energy-dispersive x-ray spectrometry. In vitro dissolution and in vivo bioavailability were also investigated. Results: Fenofibrate was distributed into the pores of Neusilin UFL2 and showed reduced crystal formation following adsorption. Supercritical CO2 facilitated the introduction of fenofibrate into the pores of Neusilin UFL2. Compared with raw fenofibrate, fenofibrate from the prepared powders showed a significantly increased dissolution rate and better bioavailability. In particular, the area under the drug concentration-time curve and maximal serum concentration of the powders prepared using supercritical CO2 were 4.62-fold and 4.52-fold greater than the corresponding values for raw fenofibrate. Conclusion: The results of this study highlight the usefulness of the melt-adsorption method using supercritical CO2 for improving the bioavailability of fenofibrate. PMID:23118538

Modeling the formation of the quench product in municipal solid waste incineration (MSWI) bottom ash.

PubMed

Inkaew, Kanawut; Saffarzadeh, Amirhomayoun; Shimaoka, Takayuki

2016-06-01

This study investigated changes in bottom ash morphology and mineralogy under lab-scale quenching conditions. The main purpose was to clarify the mechanisms behind the formation of the quench product/layer around bottom ash particles. In the experiments, the unquenched bottom ashes were heated to 300°C for 1h, and were quenched by warm water (65°C) with different simulated conditions. After having filtered and dried, the ashes were analyzed by a combination of methodologies namely, particle size distribution analysis, intact particle and thin-section observation, X-ray diffractometry, and scanning electron microscope with energy dispersive X-ray spectroscopy. The results indicated that after quenching, the morphology and mineralogy of the bottom ash changed significantly. The freshly quenched bottom ash was dominated by a quench product that was characterized by amorphous and microcrystalline calcium-silicate-hydrate (CSH) phases. This product also enclosed tiny minerals, glasses, ceramics, metals, and organic materials. The dominant mineral phases produced by quenching process and detected by XRD were calcite, Friedel's salt, hydrocalumite and portlandite. The formation of quench product was controlled by the fine fraction of the bottom ash (particle size <0.425mm). From the observations, a conceptual model of the ash-water reactions and formation of the quench product in the bottom ash was proposed. Copyright © 2016 Elsevier Ltd. All rights reserved.

Mechanochemical synthesis and intercalation of Ca(II)Fe(III)-layered double hydroxides

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

Ferencz, Zs.; Szabados, M.; Varga, G.

2016-01-15

A mechanochemical method (grinding the components without added water – dry grinding, followed by further grinding in the presence of minute amount of water or NaOH solution – wet grinding) was used in this work for the preparation and intercalation of CaFe-layered double hydroxides (LDHs). Both the pristine LDHs and the amino acid anion (cystinate and tyrosinate) intercalated varieties were prepared by the two-step grinding procedure in a mixer mill. By systematically changing the conditions of the preparation method, a set of parameters could be determined, which led to the formation of close to phase-pure LDH. The optimisation procedure wasmore » also applied for the intercalation processes of the amino acid anions. The resulting materials were structurally characterised by a range of methods (X-ray diffractometry, scanning electron microscopy, energy dispersive analysis, thermogravimetry, X-ray absorption and infra-red spectroscopies). It was proven that this simple mechanochemical procedure was able to produce complex organic–inorganic nanocomposites: LDHs intercalated with amino acid anions. - Graphical abstract: Amino acid anion-Ca(II)Fe(III)-LDHs were successfully prepared by a two-step milling procedure. - Highlights: • Synthesis of pristine and amino acid intercalated CaFe-LDHs by two-step milling. • Identifying the optimum synthesis and intercalation parameters. • Characterisation of the samples with a range of instrumental methods.« less

Oxidation study of coated Crofer 22 APU steel in dry oxygen

NASA Astrophysics Data System (ADS)

Molin, Sebastian; Chen, Ming; Hendriksen, Peter Vang

2014-04-01

The effect of a dual layer coating composed of a layer of a Co3O4 and a layer of a La0.85Sr0.15MnO3/Co3O4 mixture on the high temperature corrosion of the Crofer 22 APU alloy is reported. Oxidation experiments were performed in dry oxygen at three temperatures: 800 °C, 850 °C and 900 °C for periods up to 1000 h. Additionally at 850 °C a 5000 h long oxidation test was performed to evaluate longer term suitability of the proposed coating. Corrosion kinetics were evaluated by measuring mass gain during oxidation. The corrosion kinetics for the coated samples are analyzed in terms of a parabolic rate law. Microstructural features were investigated by scanning electron microscopy, energy dispersive X-ray analysis and X-ray diffractometry. The coating is effective in reducing the corrosion rate and in ensuring long lifetime of coated alloys. The calculated activation energy for the corrosion process is around 1.8 eV. A complex Co-Mn-Cr spinel is formed caused by diffusion of Cr and Mn from the alloy into the Co3O4 coating and by additional diffusion of Mn from the LSM layer. Adding a layer of LSM/Co3O4, acting as an additional Mn source, on top of the cobalt spinel is beneficial for the improved corrosion resistance.

The effect of nanoparticles size on photocatalytic and antimicrobial properties of Ag-Pt/TiO2 photocatalysts

NASA Astrophysics Data System (ADS)

Zielińska-Jurek, Anna; Wei, Zhishun; Wysocka, Izabela; Szweda, Piotr; Kowalska, Ewa

2015-10-01

Ag-Pt-modified TiO2 nanocomposites were synthesized using the sol-gel method. Bimetallic modified TiO2 nanoparticles exhibited improved photocatalytic activity under visible-light irradiation, better than monometallic Ag/TiO2 and Pt/TiO2 nanoparticles (NPs). All modified powders showed localized surface plasmon resonance (LSPR) in visible region. The photocatalysts' characteristics by X-ray diffractometry (XRD), scanning transmission electron microscopy (STEM), diffuse reflectance spectroscopy (DRS), X-ray photoelectron spectroscopy (XPS), nitrogen adsorption (BET method for specific surface area) showed that sample with the highest photocatalytic activity had anatase structure, about 93 m2/g specific surface area, maximum plasmon absorption at ca. 420 nm and contained small NPs of silver of 6 nm and very fine platinum NPs of 3 nm. The photocatalytic activity was estimated by measuring the decomposition rate of phenol in 0.2 mM aqueous solution under Vis and UV/vis light irradiation. It was found that size of platinum was decisive for the photocatalytic activity under visible light irradiation, i.e., the smaller Pt NPs were, the higher was photocatalytic activity. While, antimicrobial activities, estimated for bacteria Escherichia coli and Staphylococcus aureus, and pathogenic fungi belonging to Candida family, were only observed for photocatalysts containing silver, i.e., Ag/TiO2 and Ag-Pt/TiO2 nanocomposites.

Surface modification using the biomimetic method in alumina-zirconia porous ceramics obtained by the replica method.

PubMed

Silva, André D R; Rigoli, Willian R; Osiro, Denise; Mello, Daphne C R; Vasconcellos, Luana M R; Lobo, Anderson O; Pallone, Eliria M J A

2018-01-12

The modification of biomaterials approved by the Food and Drug Administration could be an alternative to reduce the period of use in humans. Porous bioceramics are widely used as support structures for bone formation and repair. This composite has essential characteristics for an implant, including good mechanical properties, high chemical stability, biocompatibility and adequate aesthetic appearance. Here, three-dimensional porous scaffolds of Al 2 O 3 containing 5% by volume of ZrO 2 were produced by the replica method. These scaffolds had their surfaces chemically treated with phosphoric acid and were coated with calcium phosphate using the biomimetic method simulated body fluid (SBF, 5×) for 14 days. The scaffolds, before and after biomimetic coating, were characterized mechanically, morphologically and structurally by axial compression tests, scanning electron microscopy, microtomography, apparent porosity, X-ray diffractometry, near-infrared spectroscopy, inductively coupled plasma optical emission spectroscopy, energy dispersive X-ray spectroscopy and reactivity. The in vitro cell viability and formation of mineralization nodules were used to identify the potential for bone regeneration. The produced scaffols after immersion in SBF were able to induce the nodules formation. These characteristics are advantaged by the formation of different phases of calcium phosphates on the material surface in a reduced incubation period. © 2018 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater, 2018. © 2018 Wiley Periodicals, Inc.

Antibacterial activity and cytotoxicity of multi-walled carbon nanotubes decorated with silver nanoparticles

PubMed Central

Seo, Youngmin; Hwang, Jangsun; Kim, Jieun; Jeong, Yoon; Hwang, Mintai P; Choi, Jonghoon

2014-01-01

Recently, various nanoscale materials, including silver (Ag) nanoparticles, have been actively studied for their capacity to effectively prevent bacterial growth. A critical challenge is to enhance the antibacterial properties of nanomaterials while maintaining their biocompatibility. The conjugation of multiple nanomaterials with different dimensions, such as spherical nanoparticles and high-aspect-ratio nanotubes, may increase the target-specific antibacterial capacity of the consequent nanostructure while retaining an optimal biocompatibility. In this study, multi-walled carbon nanotubes (MWCNTs) were treated with a mixture of acids and decorated with Ag nanoparticles via a chemical reduction of Ag cations by ethanol solution. The synthesized Ag-MWCNT complexes were characterized by transmission electron microscopy, X-ray diffractometry, and energy-dispersive X-ray spectroscopy. The antibacterial function of Ag-MWCNTs was evaluated against Methylobacterium spp. and Sphingomonas spp. In addition, the biocompatibility of Ag-MWCNTs was evaluated using both mouse liver hepatocytes (AML 12) and human peripheral blood mononuclear cells. Finally, we determined the minimum amount of Ag-MWCNTs required for a biocompatible yet effective antibacterial treatment modality. We report that 30 μg/mL of Ag-MWCNTs confers antibacterial functionality while maintaining minimal cytotoxicity toward both human and animal cells. The results reported herein would be beneficial for researchers interested in the efficient preparation of hybrid nanostructures and in determining the minimum amount of Ag-MWCNTs necessary to effectively hinder the growth of bacteria. PMID:25336943

Application of film-casting technique to investigate drug-polymer miscibility in solid dispersion and hot-melt extrudate.

PubMed

Parikh, Tapan; Gupta, Simerdeep Singh; Meena, Anuprabha K; Vitez, Imre; Mahajan, Nidhi; Serajuddin, Abu T M

2015-07-01

Determination of drug-polymer miscibility is critical for successful development of solid dispersions. This report details a practical method to predict miscibility and physical stability of drug with various polymers in solid dispersion and, especially, in melt extrudates by applying a film-casting technique. Mixtures of itraconazole (ITZ) with hydroxypropylmethylcellulose phthalate (HPMCP), Kollidon(®) VA 64, Eudragit(®) E PO, and Soluplus(®) were film-casted, exposed to 40°C/75% RH for 1 month and then analyzed using differential scanning calorimetry (DSC), powder X-ray diffractometry, and polarized light microscopy (PLM). ITZ had the highest miscibility with HPMCP, being miscible at drug to polymer ratio of 6:4 (w/w). There was a downward trend of lower miscibility with Soluplus(®) (miscible at 3:7, w/w, and a few microcrystals present at 4:6, w/w), Kollidon(®) VA 64 (2:8, w/w) and Eudragit(®) E PO (<1:9, w/w). PLM was found more sensitive to detect drug crystallization than DSC and powder X-ray diffractometry. There was general correlation between results of film casting and hot-melt extrusion (HME) using a twin screw extruder. For ITZ-Soluplus(®) mixtures, HME at 4:6 (w/w) resulted in a single phase, whereas drug crystallization was observed at higher drug load. HME of ITZ-Kollidon(®) VA 64 mixtures also correlated well with the miscibility predicted by film casting. © 2015 Wiley Periodicals, Inc. and the American Pharmacists Association.

W{sub 18}O{sub 49} nanorods decorated with Ag/AgCl nanoparticles as highly-sensitive gas-sensing material and visible-light-driven photocatalyst

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

Sun Shibin; Chang Xueting, E-mail: xuetingchang@yahoo.cn; Dong Lihua

2011-08-15

A novel gas-sensing material and photocatalyst was successfully obtained by decorating Ag/AgCl nanoparticles on the W{sub 18}O{sub 49} nanorods through a clean photochemical route. The as-prepared samples were characterized using combined techniques of X-ray diffractometry, electron microscopy, energy dispersive X-ray spectrometry, and X-ray photoelectron spectroscopy. Gas-sensing measurements indicate that the Ag/AgCl/W{sub 18}O{sub 49} NRs sensors exhibit superior reducing gas-sensing properties to those of bare W{sub 18}O{sub 49} NRs, and they are highly selective and sensitive to NH{sub 3}, acetone, and H{sub 2}S with short response and recovery times. The Ag/AgCl/W{sub 18}O{sub 49} NRs photocatlysts also possess higher photocatalytic performance thanmore » bare W{sub 18}O{sub 49} NRs for degradation of methyl orange under simulated sunlight irradiation. Possible mechanisms concerning the enhancement of gas-sensing and photocatalytic activities of the Ag/AgCl/W{sub 18}O{sub 49} NRs composite were proposed. - Graphical Abstract: The Ag/AgCl nanoparticles adhered well to the W{sub 18}O{sub 49} nanorod. The Ag could act as transfer center of the photoexcited carriers, prohibiting their recombinations in both W{sub 18}O{sub 49} and AgCl. Highlights: > Ag/AgCl/W{sub 18}O{sub 49} NRs were successfully obtained via a clean photochemical route. > The Ag/AgCl nanoparticles decorated on the W{sub 18}O{sub 49} NRs possessed cladding structure. > The Ag/AgCl/W{sub 18}O{sub 49} NRs exhibited excellent gas-sensing and photocatalytic properties.« less

5-Arylidene derivatives of Meldrum's acid: Synthesis, structural characterization using single crystal and powder crystal X-ray diffraction, and electronic properties

NASA Astrophysics Data System (ADS)

Dey, Tanusri; Ghosh, Soumen; Ghosh, Somnath; Mukherjee, Alok Kumar

2015-07-01

Four 5-arylidene derivatives of Meldrum's acid, 5-(4-chlorobenzylidene)-2,2-dimethyl-1,3-dioxane-4,6-dione (2), 5-(3-hydroxybenzylidene)-2,2-dimethyl-1,3-dioxane-4,6-dione (3), 5-(3,4-dimethoxybenzylidene)-2,2-dimethyl-1,3-dioxane-4,6-dione (4) and 5-(2,4-dimethoxy benzylidene)-2,2-dimethyl-1,3-dioxane-4,6-dione (5) have been synthesized and their crystal structures have been determined using single crystal X-ray diffractometry for 2, 4 and 5 and X-ray powder diffraction for 3. The nature of intermolecular interactions in 2-5 has been analyzed through Hirshfeld surfaces and 2D fingerprint plots. The DFT optimized molecular geometries in 2-5 agree closely with those obtained from the crystallographic studies. The crystal packing in 2-5 exhibits an interplay of Osbnd H⋯O, Csbnd H⋯O, Csbnd H⋯Cl and Csbnd H⋯π (arene) hydrogen bonds and π⋯π interactions, which assemble molecules into three-dimensional architecture in 2, 3 and 5 and two-dimensional framework in 4. The Hirshfeld surface analyses of 2-5, Meldrum's acid (1) and a few related 5-arylidene derivatives of Meldrum's acid retrieved from the Cambridge Structural Database (CSD) indicate that about 85% of the Hirshfeld surface area (72% in 2 where H⋯Cl contribution is about 13%) in this class of compounds are due to H⋯H, O⋯H and C⋯H contacts. The HOMO-LUMO energy gap (>2.2 eV) in 2-5 indicates a significant degree of internal charge transfer within the molecule.

Ultrasonically-enhanced preparation, characterization of CaFe-layered double hydroxides with various interlayer halide, azide and oxo anions (CO32-, NO3-, ClO4-).

PubMed

Szabados, Márton; Varga, Gábor; Kónya, Zoltán; Kukovecz, Ákos; Carlson, Stefan; Sipos, Pál; Pálinkó, István

2018-01-01

An ultrasonically-enhanced mechanochemical method was developed to synthesize CaFe-layered double hydroxides (LDHs) with various interlayer anions (CO 3 2- , NO 3 - , ClO 4 - , N 3 - , F - , Cl - , Br - and I - ). The duration of pre-milling and ultrasonic irradiation and the variation of synthesis temperature in the wet chemical step were investigated to obtain the optimal parameters of preparation. The main method to characterize the products was X-ray diffractometry, but infrared and synchrotron-based X-ray absorption spectroscopies as well as thermogravimetric measurements were also used to learn about fine structural details. The synthesis method afforded successful intercalation of the anions, among others the azide anion, a rarely used counter ion providing a system, which enables safe handling the otherwise highly reactive anion. The X-ray absorption spectroscopic measurements revealed that the quality of the interlayered anions could modulate the spatial arrangement of the calcium ions around the iron(III) ions, but only in the second coordination sphere. Copyright © 2017 Elsevier B.V. All rights reserved.

Phase transition behavior of (K,Na)NbO3-based high-performance lead-free piezoelectric ceramic composite with different phase compositions depending on Na fraction

NASA Astrophysics Data System (ADS)

Yamada, Hideto; Matsuoka, Takayuki; Yamazaki, Masato; Ohbayashi, Kazushige; Ida, Takashi

2018-01-01

The structures of the main (K1- x Na x )NbO3 perovskite in a high-performance lead-free piezoelectric ceramic composite (K1- x Na x )0.86Ca0.04Li0.02Nb0.85O3-δ-K0.85Ti0.85Nb1.15O5-BaZrO3-MgO-Fe2O3 (x = 0.52 and 0.70) with trace amounts of LiMgFeTiO4 inverse spinel and (Li,K)2(Mg,Fe,Ti,Nb)6O13 layered structure have been investigated by transmission electron microscopy (TEM) and synchrotron powder X-ray diffractometry (XRD) with varying temperatures. The bright-field TEM images have shown tetragonal 90°-domain contrasts at 80 and 40 °C, and the XRD profile has been simulated by adding an average structure of two differently oriented tetragonal structures bound by a 90°-domain wall for the x = 0.52 sample. Aggregates of tilted NbO6 nanodomains have been observed in a high-resolution TEM image, and the crossover of P4mm-Amm2 features from 60 to 20 °C and diffuse 2 × 2 × 2 superlattice reflections of the tilted NbO6 Imm2 structure have been observed in XRD data for the x = 0.70 sample.

Alkyl group effects on CO insertion into coordinatively unsaturated early-transition-metal alkyls. Preparations and the first structural characterizations of tantalum enolate-O and tantalum. eta. sup 2 -acyl complexes

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

Meyer, T.Y.; Garner, L.R.; Baenziger, N.C.

1990-10-03

Low-pressure carbonylation of the mono(peralkylcyclopentadienyl)tantalum(V) alkyls ({eta}-C{sub 5}Me{sub 4}R)TaR{prime}Cl{sub 3} (R = Me, Et; R{prime} = CH{sub 2}C{sub 6}H{sub 4}-p-Me, CH{sub 2}CMe{sub 3}) yields either the O-bound enolate or the {eta}{sup 2}-acyl as shown by ir/NMR spectroscopy and x-ray diffractometry. The p-tolyl enolate ({eta}-C{sub 5}Me{sub 5})Ta(OCH{double bond}CHC{sub 6}H{sub 4}-p-Me)Cl{sub 3}, derived directly from carbonylation of the tantalum 4-methylbenzyl precursor, is shown to possess a cis configuration in solution and in the solid state. Key structural features from a single-crystal x-ray diffraction study of the tetrahydrofuran-ligated enolate complex are reported. The mechanism of formation of the enolate from carbonylation of themore » 4-methylbenzyl complex is discussed. The previously reported acyl ({eta}-C{sub 5}Me{sub 4}R)Ta(C(O)CH{sub 2}CMe{sub 3})Cl{sub 3} has been reexamined and found to possess a symmetric, strongly distorted {eta}{sup 2}-acyl coordination by solution {sup 1}H NMR spectroscopy and solid-state x-ray diffractometry. The molecular structures of ({eta}-C{sub 5}Me{sub 5})Ta(OCH{double bond}CHC{sub 6}H{sub 4}-p-Me)Cl{sub 3} and ({eta}-C{sub 5}Me{sub 5})Ta(C(O)CH{sub 2}CMe{sub 3})Cl{sub 3}, which are reported here, are the first structural determinations of a tantalum enolate and of a tantalum {eta}{sup 2}-acyl. 41 refs., 2 figs., 8 tabs.« less

The Synergistic Effect of Iodide and Sodium Nitrite on the Corrosion Inhibition of Mild Steel in Bicarbonate-Chloride Solution.

PubMed

Eyu, Gaius Debi; Will, Geoffrey; Dekkers, Willem; MacLeod, Jennifer

2016-10-26

The effect of potassium iodide (KI) and sodium nitrite (NaNO₂ inhibitor on the corrosion inhibition of mild steel in chloride bicarbonate solution has been studied using electrochemical techniques. Potentiodynamic polarisation data suggest that, when used in combination, KI and NaNO₂ function together to inhibit reactions at both the anode and the cathode, but predominantly anodic. KI/NO₂ - concentration ratios varied from 2:1 to 2:5; inhibition efficiency was optimized for a ratio of 1:1. The surface morphology and corrosion products were analysed using scanning electron microscopy (SEM) and X-ray diffractometry (XRD). The latter shows that the addition of I - to NO₂ facilitates the formation of a passivating oxide (γ-Fe₂O₃) as compared to NO₂ - alone, decreasing the rate of metal dissolution observed in electrochemical testing. The synergistic effect of KI/NO₂ - inhibition was enhanced under the dynamic conditions associated with testing in a rotating disc electrode.

Structural investigation of chitosan-based microspheres with some anti-inflammatory drugs

NASA Astrophysics Data System (ADS)

Dreve, Simina; Kacso, Iren; Popa, Adriana; Raita, Oana; Dragan, Felicia; Bende, A.; Borodi, Gh.; Bratu, I.

2011-06-01

The use of chitosan as an excipient in oral formulations, as a drug delivery vehicle for ulcerogenic anti-inflammatory drugs and as base in polyelectrolyte complex systems, to prepare solid release systems as sponges was investigated. The preparation by double emulsification of chitosan hydrogels carrying diclofenac, acetyl-salycilic acid and hydrocortisone acetate as anti-inflammatory drugs is reported. The concentration of anti-inflammatory drug in the chitosan hydrogel generating the sponges was 0.08 mmol. Chitosan-drug loaded sponges with anti-inflammatory drugs were prepared by freeze-drying at -60 °C and 0.009 atm. Structural investigations of the solid formulations were done by Fourier-transformed infrared and ultraviolet-visible spectroscopy, spectrofluorimetry, differential scanning calorimetry and X-ray diffractometry. The results indicated that the drug molecules are forming temporary chelates in chitosan hydrogels and sponges. Electron paramagnetic resonance demonstrates the presence of free radicals in a wide range and the antioxidant activity for chitosan-drug supramolecular cross-linked assemblies.

Mortar radiocarbon dating: preliminary accuracy evaluation of a novel methodology.

PubMed

Marzaioli, Fabio; Lubritto, Carmine; Nonni, Sara; Passariello, Isabella; Capano, Manuela; Terrasi, Filippo

2011-03-15

Mortars represent a class of building and art materials that are widespread at archeological sites from the Neolithic period on. After about 50 years of experimentation, the possibility to evaluate their absolute chronology by means of radiocarbon ((14)C) remains still uncertain. With the use of a simplified mortar production process in the laboratory environment, this study shows the overall feasibility of a novel physical pretreatment for the isolation of the atmospheric (14)CO(2) (i.e., binder) signal absorbed by the mortars during their setting. This methodology is based on the assumption that an ultrasonic attack in liquid phase isolates a suspension of binder carbonates from bulk mortars. Isotopic ((13)C and (14)C), % C, X-ray diffractometry (XRD), and scanning electron microscopy (SEM) analyses were performed to characterize the proposed methodology. The applied protocol allows suppression of the fossil carbon (C) contamination originating from the incomplete burning of the limestone during the quick lime production, providing unbiased dating for "laboratory" mortars produced operating at historically adopted burning temperatures.

Phase purity of NiCo2O4, a catalyst candidate for electrolysis of water

NASA Technical Reports Server (NTRS)

Singer, J.; Fielder, W. L.; Garlick, R. G.; Negas, T.

1987-01-01

NiCo2O4 is shown to be difficult to obtain as a pure phase, and may never have been so obtained. High resolution x-ray diffractometry is required for its precise characterization. Film XRD is not likely to show the asymmetry in the spinel diffraction lines, caused by poorly crystallized NiO, as seen in diffractometer traces. The Co3O4 which is expected to accompany NiO as an impurity in NiCo2O4 syntheses has the same diffraction pattern as the binary oxide. Firings of the co-precipitated hydroxides at 300, 350, and 400 C, including one in pure O2, failed to produce single phase cobaltate. Scanning electron microscopy showed all the sintered products to range over several orders of magnitude in agglomerate/particle size. Surface areas by BET were all in the range 40 to 110 m sq/g, equivalent to particles of 200 to 100 Angstrom diameter. The spinel diffraction line breadths were compatible with those approximate dimensions.

Hydrothermal synthesis of nanostructured Y2O3 and (Y0.75Gd0.25)2O3 based phosphors

NASA Astrophysics Data System (ADS)

Mančić, Lidija; Lojpur, Vesna; Marinković, Bojan A.; Dramićanin, Miroslav D.; Milošević, Olivera

2013-08-01

Examples of (Y2O3-Gd2O3):Eu3+ and Y2O3:(Yb3+/Er3+) rare earth oxide-based phosphors are presented to highlight the controlled synthesis of 1D and 2D nanostructures through simple hydrothermal method. Conversion of the starting nitrates mixture into carbonate hydrate phase is performed with the help of ammonium hydrogen carbonate solution during hydrothermal treatment at 200 °C/3 h. Morphological architectures of rare earth oxides obtained after subsequent powders thermal treatment at 600 and 1100 °C for 3 and 12 h and their correlation with the optical characteristics are discussed based on X-ray powder diffractometry, field emission scanning electron microscopy, infrared spectroscopy and photoluminescence measurements. Strong red and green emission followed by the superior decay times are attributed to the high powders purity and homogeneous dopants distribution over the host lattice matrix.

Effect of Laser Powder Bed Fusion Parameters on the Microstructure and Texture Development in Superelastic Ti-18Zr-14Nb Alloy

NASA Astrophysics Data System (ADS)

Kreitcberg, A.; Brailovski, V.; Sheremetyev, V.; Prokoshkin, S.

2017-12-01

The effect of different laser powder bed fusion (L-PBF) parameters on the phase composition, microstructure, and crystallographic texture of Ti-18Zr-14Nb alloy was studied. Two levels of laser power, scanning speed, and hatching space were used, while the layer thickness was kept constant. The resulting volume energy density was ranged from 20 to 60 J/mm3, and the build rate, from 12 to 36 cm3/h. The manufactured coupons were analyzed by X-ray diffractometry, transmission, and scanning electron microscopy. It was found that the greater influence observed on the microstructure and texture development was caused by the value of laser power, while the lowest, by that of hatching space. Based on the results obtained, the processing optimization strategy aimed at improving the density, superelastic, and fatigue properties of the L-PBF manufactured Ti-18Zr-14Nb alloy was proposed.

Synthesis of barium and strontium carbonate crystals with unusual morphologies using an organic additive

NASA Astrophysics Data System (ADS)

Chen, Long; Jiang, Jizhong; Bao, Zuben; Pan, Jian; Xu, Weibing; Zhou, Lili; Wu, Zhigang; Chen, Xu

2013-12-01

In this paper, strontium carbonate (SrCO3) and barium carbonate (BaCO3) crystals were synthesized in the presence of an organic additive-hexamethylenetetramine (HMT) using two CO2 sources. Scanning electron microscopy and X-ray powder diffractometry were used to characterize the products. The results showed that the morphologies of orthorhombic strontianite SrCO3 transformed from branch-like to flower-like, and to capsicum-like at last, while the morphologies of BaCO3 change from fiber-like to branchlike, and to rod-like finally with an increase of the molar ratio HMT/Sr2+ and HMT/Ba2+ from 0.2 to 10 using ammonium carbonate as CO2 source. When using diethyl carbonate instead of ammonium carbonate as CO2 source, SrCO3 flowers aggregated by rods and BaCO3 shuttles were formed. The possible formation mechanisms of SrCO3 and BaCO3 crystals obtained in different conditions were also discussed.

Hierarchical macro-mesoporous structures in the system TiO{sub 2}-Al{sub 2}O{sub 3}, obtained by hydrothermal synthesis using Tween-20 as a directing agent

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

Garcia-Benjume, M.L.; Espitia-Cabrera, M.I.; Contreras-Garcia, M.E., E-mail: eucontre@zeus.umich.mx

2009-12-15

Macro-mesoporous powders of titania, alumina, and mixed titania-20%alumina systems were obtained by hydrothermal synthesis employing surfactant Tween-20 as structural directing agent in order to promote the textural properties of titania. The effect of the alumina in the titania phase and on textural properties was analyzed. The obtained powders presented a macroporous channel structure that was characterized by X-ray diffractometry, scanning and transmission electron microscopy, N{sub 2} adsorption-desorption analysis, pore size distribution, Fourier transform infrared spectrometry, and thermogravimetric analysis. It was found that alumina content retarded the anatase phase crystallization and increased the Brunauer-Emmet-Teller surface area from 136 to 210 m{supmore » 2}/g. The powders calcined at 400 deg. C are thermally stable and possess an interconnected macro-mesoporous hierarchical structure; the results indicate that this synthesis can be employed to prepare mixed titania-alumina with good textural properties.« less

Analysis of microstructure and mechanical properties of aluminium-copper joints welded by FSW process

NASA Astrophysics Data System (ADS)

Iordache, M.; Sicoe, G.; Iacomi, D.; Niţu, E.; Ducu, C.

2017-08-01

The research conducted in this article aimed to check the quality of joining some dissimilar materials Al-Cu by determining the mechanical properties and microstructure analysis. For the experimental measurements there were used tin alloy Al - EN-AW-1050A with a thickness of 2 mm and Cu99 sheet with a thickness of 2 mm, joined by FSW weld overlay. The main welding parameters were: rotating speed of the rotating element 1400 rev/min, speed of the rotating element 50 mm/min. The experimental results were determined on samples specially prepared for metallographic analysis. In order to prepare samples for their characterization, there was designed and built a device that allowed simultaneous positioning and fixing for grinding. The characteristics analyzed in the joint welded samples were mictrostructure, microhardness and residual stresses. The techniques used to determine these characteristics were optical microscopy, electron microscopy with fluorescence radioactive elemental analysis (EDS), Vickers microhardness line - HV0.3 and X-ray diffractometry.

Chitosan-based nanocarriers for antimalarials

NASA Astrophysics Data System (ADS)

Dreve, Simina; Kacso, Iren; Popa, Adriana; Raita, Oana; Bende, A.; Borodi, Gh.; Bratu, I.

2012-02-01

The objective of this research was to synthesize and characterize chitosan-based liquid and solid materials with unique absorptive and mechanical properties as carriers for quinine - one of the most used antimalarial drug. The use of chitosan (CTS) as base in polyelectrolyte complex systems, to prepare solid release systems as sponges is presented. The preparation by double emulsification of CTS hydrogels carrying quinine as anti-malarial drug is reported. The concentration of quinine in the CTS hydrogel was 0.08 mmol. Chitosan - drug loaded hydrogel was used to generate solid sponges by freeze-drying at -610°C and 0.09 atm. Structural investigations of the solid formulations were done by Fourier-transformed infrared spectroscopy (FTIR), ultraviolet-visible spectroscopy (UV-VIS), spectrofluorimetry, differential scanning calorimetry (DSC) and X-ray diffractometry. The results indicated that the drug molecule is forming temporary chelates in CTS hydrogels and sponges. Electron paramagnetic resonance (EPR) demonstrates the presence of free radicals in a wide range and the antioxidant activity for chitosan - drug supramolecular cross-linked assemblies.

Preparation of CMC-modified melamine resin spherical nano-phase change energy storage materials.

PubMed

Hu, Xiaofeng; Huang, Zhanhua; Zhang, Yanhua

2014-01-30

A novel carboxymethyl cellulose (CMC)-modified melamine-formaldehyde (MF) phase change capsule with excellent encapsulation was prepared by in situ polymerization. Effects of CMC on the properties of the capsules were studied by Fourier transformation infrared spectroscopy (FTIR), differential scanning calorimetry (DSC), scanning electronic microscopy (SEM), X-ray diffractometry (XRD), and thermogravimetric analysis (TGA). The results showed that the CMC-modified capsules had an average diameter of about 50nm and good uniformity. The phase change enthalpy of the capsules was increased and the cracking ratio decreased by incorporating a suitable amount of CMC. The optimum phase change enthalpy of the nanocapsules was 83.46J/g, and their paraffin content was 63.1%. The heat resistance of the capsule shells decreased after CMC modification. In addition, the nanocapsule cracking ratio of the nanocapsules was 11.0%, which is highly attractive for their application as nano phase change materials. Copyright © 2013 Elsevier Ltd. All rights reserved.

Change Spectrum Characteristics Modification of Films Deposited by Magnetron Sputtering with the Assistance of Argon Ions Beam

NASA Astrophysics Data System (ADS)

Umnov, S.; Asainov, O.

2015-04-01

Thin aluminum films were prepared using the method of magnetron sputtering with and without argon ion beam assistance. The influence of argon ion beam on the reflectivity in the UV range and the structure of aluminum films was studied. The structure of the films was studied by transmission electron microscopy (TEM), X-ray diffractometry (XRD) and atomic- force microscope (AFM). The study has shown that the films deposed with the assistance of the argon ion beam have more significant microstresses associated with an increase of crystallites microstructure defects as compared to the films deposed without ion assistance. Comparison of the measured reflectivity of aluminum films deposed without and with the assistance of the ion beam has shown that the films characterized by a higher level of microstructure def ects have increased reflectivity in the UV range. The studies suggest that the defects of thin aluminum films crystal structure influence its optical properties.

Encapsulation of Ethylene Gas into Granular Cold-Water-Soluble Starch: Structure and Release Kinetics.

PubMed

Shi, Linfan; Fu, Xiong; Tan, Chin Ping; Huang, Qiang; Zhang, Bin

2017-03-15

Ethylene gas was introduced into granular cold-water-soluble (GCWS) starches using a solid encapsulation method. The morphological and structural properties of the novel inclusion complexes (ICs) were characterized using scanning electron microscopy, X-ray diffractometry, and Raman spectroscopy. The V-type single helix of GCWS starches was formed through controlled gelatinization and ethanol precipitation and was approved to host ethylene gas. The controlled release characteristics of ICs were also investigated at various temperature and relative humidity conditions. Avrami's equation was fitted to understand the release kinetics and showed that the release of ethylene from the ICs was accelerated by increasing temperature or RH and was decelerated by increased degree of amylose polymerization. The IC of Hylon-7 had the highest ethylene concentration (31.8%, w/w) among the five starches, and the IC of normal potato starch showed the best controlled release characteristics. As a renewable and inexpensive material, GCWS starch is a desirable solid encapsulation matrix with potential in agricultural and food applications.

Synthesization, Characterization, and in Vitro Evaluation of Cytotoxicity of Biomaterials Based on Halloysite Nanotubes.

PubMed

Sánchez-Fernández, Antonio; Peña-Parás, Laura; Vidaltamayo, Román; Cué-Sampedro, Rodrigo; Mendoza-Martínez, Ana; Zomosa-Signoret, Viviana C; Rivas-Estilla, Ana M; Riojas, Paulina

2014-12-04

Halloysite is an aluminosilicate clay that has been widely used for controlled drug delivery, immobilization of enzymes, and for the capture of circulating tumor cells (CTCs). Surface modification of halloysite by organosilanes has been explored to improve their properties. In this study halloysite clay nanotubes (HNTs) were functionalized by two different organosilanes: Trimethoxy(propyl)silane (TMPS), and Triethoxy(octyl)silane (EOS). Untreated and modified samples were characterized by scanning electron microscopy (SEM), X-ray diffractometry (XRD), thermogravimetrical analysis (TGA), and Fourier transform infrared spectroscopy (FTIR). Results showed a strong interaction of organosilanes with the chemical groups present in HNTs. Biocompatibility and cytotoxicity of these nanomaterials were determined using C6 rat glioblastoma cells. Our results indicate that prior to functionalization, HNTs show a high biocompatibility and low cytotoxicity. However, HNTs functionalized with EOS and TMPS showed high cytotoxicity by inducing apoptosis. These results allow the identification of potential applications in biomedical areas for HNTs.

Synthesization, Characterization, and in Vitro Evaluation of Cytotoxicity of Biomaterials Based on Halloysite Nanotubes

PubMed Central

Sánchez-Fernández, Antonio; Peña-Parás, Laura; Vidaltamayo, Román; Cué-Sampedro, Rodrigo; Mendoza-Martínez, Ana; Zomosa-Signoret, Viviana C.; Rivas-Estilla, Ana M.; Riojas, Paulina

2014-01-01

Halloysite is an aluminosilicate clay that has been widely used for controlled drug delivery, immobilization of enzymes, and for the capture of circulating tumor cells (CTCs). Surface modification of halloysite by organosilanes has been explored to improve their properties. In this study halloysite clay nanotubes (HNTs) were functionalized by two different organosilanes: Trimethoxy(propyl)silane (TMPS), and Triethoxy(octyl)silane (EOS). Untreated and modified samples were characterized by scanning electron microscopy (SEM), X-ray diffractometry (XRD), thermogravimetrical analysis (TGA), and Fourier transform infrared spectroscopy (FTIR). Results showed a strong interaction of organosilanes with the chemical groups present in HNTs. Biocompatibility and cytotoxicity of these nanomaterials were determined using C6 rat glioblastoma cells. Our results indicate that prior to functionalization, HNTs show a high biocompatibility and low cytotoxicity. However, HNTs functionalized with EOS and TMPS showed high cytotoxicity by inducing apoptosis. These results allow the identification of potential applications in biomedical areas for HNTs. PMID:28788274

Characterization of the bioactive and mechanical behavior of dental ceramic/sol-gel derived bioactive glass mixtures.

PubMed

Abbasi, Zahra; Bahrololoum, Mohammad E; Bagheri, Rafat; Shariat, Mohammad H

2016-02-01

Dental ceramics can be modified by bioactive glasses in order to develop apatite layer on their surface. One of the benefits of such modification is to prolong the lifetime of the fixed dental prosthesis by preventing the formation of secondary caries. Dental ceramic/sol-gel derived bioactive glass mixture is one of the options for this modification. In the current study, mixtures of dental ceramic/bioactive glass with different compositions were successfully produced. To evaluate their bioactive behavior, prepared samples were immersed in a simulated body fluid at various time intervals. The prepared and soaked specimens were characterized using Fourier transform infrared spectroscopy, X-ray diffractometry and scanning electron microscopy. Since bioactive glasses have deleterious effects on the mechanical properties of dental ceramics, 3-point bending tests were used to evaluate the flexural strength, flexural strain, tangent modulus of elasticity and Weibull modulus of the specimens in order to find the optimal relationship between mechanical and bioactive properties. Copyright © 2015 Elsevier Ltd. All rights reserved.

Compact x-ray source and panel

DOEpatents

Sampayon, Stephen E [Manteca, CA

2008-02-12

A compact, self-contained x-ray source, and a compact x-ray source panel having a plurality of such x-ray sources arranged in a preferably broad-area pixelized array. Each x-ray source includes an electron source for producing an electron beam, an x-ray conversion target, and a multilayer insulator separating the electron source and the x-ray conversion target from each other. The multi-layer insulator preferably has a cylindrical configuration with a plurality of alternating insulator and conductor layers surrounding an acceleration channel leading from the electron source to the x-ray conversion target. A power source is connected to each x-ray source of the array to produce an accelerating gradient between the electron source and x-ray conversion target in any one or more of the x-ray sources independent of other x-ray sources in the array, so as to accelerate an electron beam towards the x-ray conversion target. The multilayer insulator enables relatively short separation distances between the electron source and the x-ray conversion target so that a thin panel is possible for compactness. This is due to the ability of the plurality of alternating insulator and conductor layers of the multilayer insulators to resist surface flashover when sufficiently high acceleration energies necessary for x-ray generation are supplied by the power source to the x-ray sources.

Thermally Stable Nanocrystalline Steel

NASA Astrophysics Data System (ADS)

Hulme-Smith, Christopher Neil; Ooi, Shgh Woei; Bhadeshia, Harshad K. D. H.

2017-10-01

Two novel nanocrystalline steels were designed to withstand elevated temperatures without catastrophic microstructural changes. In the most successful alloy, a large quantity of nickel was added to stabilize austenite and allow a reduction in the carbon content. A 50 kg cast of the novel alloy was produced and used to verify the formation of nanocrystalline bainite. Synchrotron X-ray diffractometry using in situ heating showed that austenite was able to survive more than 1 hour at 773 K (500 °C) and subsequent cooling to ambient temperature. This is the first reported nanocrystalline steel with high-temperature capability.

Unidirectional growth, rocking curve, linear and nonlinear optical properties of LPHCl single crystals

NASA Astrophysics Data System (ADS)

Kumar, P. Ramesh; Gunaseelan, R.; Raj, A. Antony; Selvakumar, S.; Sagayaraj, P.

2012-06-01

Nonlinear optical amino-acid single crystal of L-phenylalanine hydrochloride (LPHCl) was successfully grown by unidirectional Sankaranarayanan-Ramasamy (SR) method under ambient conditions for the first time. The grown single crystal was subjected to different characterization analyses in order to find out its suitability for device fabrication. The crystalline perfection was evaluated using high-resolution X-ray diffractometry. It is evident from the optical absorption study that crystal has excellent transmission in the entire visible region with its lower cut off wavelength around 290 nm.

Femtosecond laser-electron x-ray source

DOEpatents

Hartemann, Frederic V.; Baldis, Hector A.; Barty, Chris P.; Gibson, David J.; Rupp, Bernhard

2004-04-20

A femtosecond laser-electron X-ray source. A high-brightness relativistic electron injector produces an electron beam pulse train. A system accelerates the electron beam pulse train. The femtosecond laser-electron X-ray source includes a high intra-cavity power, mode-locked laser and an x-ray optics system.

Formation and morphology of Zn(2)Ti(3)O(8) powders using hydrothermal process without dispersant agent or mineralizer.

PubMed

Wang, Cheng-Li; Hwang, Weng-Sing; Chang, Kuo-Ming; Ko, Horng-Huey; Hsi, Chi-Shiung; Huang, Hong-Hsin; Wang, Moo-Chin

2011-01-28

Synthesis of Zn(2)Ti(3)O(8) powders for attenuating UVA using TiCl(4), Zn(NO(3))(2)·6H(2)O and NH(4)OH as precursor materials by hydrothermal process has been investigated. The X-ray diffractometry (XRD) results show the phases of ZnO, anatase TiO(2) and Zn(2)Ti(3)O(8) coexisted when the zinc titanate powders were calcined at 600 °C for 1 h. When calcined at 900 °C for 1 h, the XRD results reveal the existence of ZnO, Zn(2)TiO(4), rutile TiO(2) and ZnTiO(3). Scanning electron microscope (SEM) observations show extensive large agglomeration in the samples. Transmission electron microscope (TEM) and electron diffraction (ED) examination results indicate that ZnTiO(3) crystallites formed with a size of about 5 nm on the matrix of plate-like ZnO when calcined at 700 °C for 1 h. The calcination samples have acceptable absorbance at a wavelength of 400 nm, indicating that the zinc titanate precursor powders calcined at 700 °C for 1 h can be used as an UVA-attenuating agent.

Formation and Morphology of Zn2Ti3O8 Powders Using Hydrothermal Process without Dispersant Agent or Mineralizer

PubMed Central

Wang, Cheng-Li; Hwang, Weng-Sing; Chang, Kuo-Ming; Ko, Horng-Huey; Hsi, Chi-Shiung; Huang, Hong-Hsin; Wang, Moo-Chin

2011-01-01

Synthesis of Zn2Ti3O8 powders for attenuating UVA using TiCl4, Zn(NO3)2·6H2O and NH4OH as precursor materials by hydrothermal process has been investigated. The X-ray diffractometry (XRD) results show the phases of ZnO, anatase TiO2 and Zn2Ti3O8 coexisted when the zinc titanate powders were calcined at 600 °C for 1 h. When calcined at 900 °C for 1 h, the XRD results reveal the existence of ZnO, Zn2TiO4, rutile TiO2 and ZnTiO3. Scanning electron microscope (SEM) observations show extensive large agglomeration in the samples. Transmission electron microscope (TEM) and electron diffraction (ED) examination results indicate that ZnTiO3 crystallites formed with a size of about 5 nm on the matrix of plate-like ZnO when calcined at 700 °C for 1 h. The calcination samples have acceptable absorbance at a wavelength of 400 nm, indicating that the zinc titanate precursor powders calcined at 700 °C for 1 h can be used as an UVA-attenuating agent. PMID:21541035

Microstructure and properties of Fe-based composite coating by laser cladding Fe-Ti-V-Cr-C-CeO2 powder

NASA Astrophysics Data System (ADS)

Zhang, Hui; Zou, Yong; Zou, Zengda; Wu, Dongting

2015-01-01

In situ TiC-VC reinforced Fe-based cladding layer was obtained on low carbon steel surface by laser cladding with Fe-Ti-V-Cr-C-CeO2 alloy powder. The microstructure, phases and properties of the cladding layer were investigated by X-ray diffractometry (XRD), scanning electron microscopy (SEM), energy dispersive spectrometry (EDS), transmission electron microscopy (TEM), potentio-dynamic polarization and electro-chemical impedance spectroscopy (EIS). Results showed Fe-Ti-V-Cr-C-CeO2 alloy powder formed a good cladding layer without defects such as cracks and pores. The phases of the cladding layer were α-Fe, γ-Fe, TiC, VC and TiVC2. The microstructures of the cladding layer matrix were lath martensite and retained austenite. The carbides were polygonal blocks with a size of 0.5-2 μm and distributed uniformly in the cladding layer. High resolution transmission electron microscopy showed the carbide was a complex matter composed of nano TiC, VC and TiVC2. The cladding layer with a hardness of 1030 HV0.2 possessed good wear and corrosion resistance, which was about 16.85 and 9.06 times than that of the substrate respectively.

Ferric ion-assisted in situ synthesis of silver nanoplates on polydopamine-coated silk.

PubMed

Xiao, Jing; Zhang, Huihui; Mao, Cuiping; Wang, Ying; Wang, Ling; Lu, Zhisong

2016-10-01

In the present study, a ferric ion (Fe(3+))-assisted in situ synthesis approach was developed to grow silver (Ag) nanoplates on the polydopamine (PDA)-coated silk without the use of additional reductants. The essential role of Fe(3+) in the formation of Ag nanoplates is revealed by comparing the morphologies of Ag nanostructures prepared on the silk-coated PDA film with/without Fe(3+) doping. Scanning electron micrographs show that high-density Ag nanoplates could be synthesized in the reaction system containing 50μg/mL FeCl3 and 50mM AgNO3. The size of the Ag nanoplate could be tuned by adjusting the reaction duration. Based on the data, a mechanism involving the Fe(3+)-selected growth of Ag atoms along the certain crystal faces was proposed to explain the fabrication process. Transmission electron microscopy and X-ray diffractometry indicate that the Ag nanoplates possess good crystalline structures. Raman spectra demonstrate that the nanoplates could strongly enhance the Raman scattering of the PDA molecules. The Ag nanoplate-coated silk could be utilized as a flexible substrate for the development of surface-enhanced Raman scattering biosensors. Copyright © 2016 Elsevier Inc. All rights reserved.

Synthesis of high generation thermo-sensitive dendrimers for extraction of rivaroxaban from human fluid and pharmaceutic samples.

PubMed

Parham, Negin; Panahi, Homayon Ahmad; Feizbakhsh, Alireza; Moniri, Elham

2018-04-13

In this present study, poly (N-isopropylacrylamide) as a thermo-sensitive agent was grafted onto magnetic nanoparticles, then ethylenediamine and methylmethacrylate were used to synthesize the first generation of poly amidoamine (PAMAM) dendrimers successively and the process continued alternatively until the ten generations of dendrimers. The synthesized nanocomposite was investigated using Fourier transform infrared spectrometry, thermalgravimetry analysis, X-ray diffractometry, elemental analysis and vibrating-sample magnetometer. The particle size and morphology were characterized using dynamic light scattering, field emission scanning electron microscopy and transmission electron microscopy. Batch experiments were conducted to investigate the parameters affecting adsorption and desorption of rivaroxaban by synthesized nanocomposite. The maximum sorption of rivaroxaban by the synthesized nanocomposite was obtained at pH of 8. The resulting grafted magnetic nanoparticle dendrimers were applied for extraction of rivaroxaban from biologic human liquids and medicinal samples. The specifications of rivaroxaban sorbed by a magnetic nanoparticle dendrimer showed good accessibility and high capacity of the active sites within the dendrimers. Urine and drug matrix extraction recoveries of more than 92.5 and 99.8 were obtained, respectively. Copyright © 2018 Elsevier B.V. All rights reserved.

Chitosan microparticles: influence of the gelation process on the release profile and oral bioavailability of albendazole, a class II compound.

PubMed

Piccirilli, Gisela N; García, Agustina; Leonardi, Darío; Mamprin, María E; Bolmaro, Raúl E; Salomón, Claudio J; Lamas, María C

2014-11-01

Encapsulation of albendazole, a class II compound, into polymeric microparticles based on chitosan-sodium lauryl sulfate was investigated as a strategy to improve drug dissolution and oral bioavailability. The microparticles were prepared by spray drying technique and further characterized by means of X-ray powder diffractometry, infrared spectroscopy and scanning electron microscopy. The formation of a novel polymeric structure between chitosan and sodium lauryl sulfate, after the internal or external gelation process, was observed by infrared spectroscopy. The efficiency of encapsulation was found to be between 60 and 85% depending on the internal or external gelation process. Almost spherically spray dried microparticles were observed using scanning electron microscopy. In vitro dissolution results indicated that the microparticles prepared by internal gelation released 8% of the drug within 30 min, while the microparticles prepared by external gelation released 67% within 30 min. It was observed that the AUC and Cmax values of ABZ from microparticles were greatly improved, in comparison with the non-encapsulated drug. In conclusion, the release properties and oral bioavailability of albendazole were greatly improved by using spraydried chitosan-sodium lauryl sulphate microparticles.

Nanocrystalline Ce 1- xY xO 2- x/2 (0≤ x≤0.35) Oxides via Carbonate Precipitation: Synthesis and Characterization

NASA Astrophysics Data System (ADS)

Li, Ji-Guang; Ikegami, Takayasu; Wang, Yarong; Mori, Toshiyuki

2002-10-01

A novel carbonate (co)precipitation method, employing nitrates as the starting salts and ammonium carbonate as the precipitant, has been used to synthesize nanocrystalline CeO 2 and Ce 1- xY xO 2- x/2 ( x≤0.35) solid-solutions. The resultant powders are characterized by elemental analysis, differential thermal analysis/thermogravimetry (DTA/TG), X-ray diffractometry (XRD), Brunauer-Emmett-Teller (BET) analysis, and high-resolution scanning electron microscopy (HRSEM). Due to the direct formation of carbonate solid-solutions during precipitation, Ce 1- xY xO 2- x/2 solid-solution oxides are formed directly during calcination at a very low temperature of ˜300°C for 2 h. The thus-produced oxide nanopowders are essentially non-agglomerated, as revealed by BET in conjunction with XRD analysis. The solubility of YO 1.5 in CeO 2 is determined via XRD to be somewhere in the range from 27 to 35 mol%, from which a Y 2O 3-related type-C phase appears in the final product. Y 3+-doping promotes the formation of spherical nanoparticles, retards thermal decomposition of the precursors, and suppresses significantly crystallite coarsening of the oxides during calcination. The activation energy for crystallite coarsening increases gradually from 68.7 kJ mol -1 for pure CeO 2 to 138.6 kJ mol -1 for CeO 2 doped with 35 mol% YO 1.5. The dopant effects on crystallite coarsening is elaborated from the view point of solid-state chemistry.

Synthesis of magnetic mesoporous metal-organic framework-5 for the effective enrichment of malachite green and crystal violet in fish samples.

PubMed

Zhou, Zhihui; Fu, Yanqing; Qin, Qian; Lu, Xin; Shi, Xianzhe; Zhao, Chunxia; Xu, Guowang

2018-07-27

A novel, magnetic and mesoporous Fe 3 O 4 @PEI-MOF-5 material was synthesized for the effective enrichment of malachite green (MG) and crystal violet (CV) in fish samples. The Fe 3 O 4 @PEI-MOF-5 material was prepared by a facile two-step solvothermal approach in which Fe 3 O 4 @PEI and MOF-5 were connected through chemical bonds. Characterization of the newly synthesized Fe 3 O 4 @PEI-MOF-5 material was performed by Fourier transform infrared spectroscopy, X-ray diffractometry, vibrating sample magnetometry, scanning electron microscopy, transmission electron microscopy, thermogravimetric analysis and X-ray photoelectron spectroscopy. This new material was determined to have high magnetization and chemical stability, a large surface area and a distinctive morphology. An effective enrichment and detection method for MG and CV was subsequently developed by combining the Fe 3 O 4 @PEI-MOF-5 material with ultra-high-performance liquid chromatography-tandem mass spectrometry. The linearity ranges of this approach for MG and CV were 1-500ng/mL and 0.25-500ng/mL, respectively, with correlation coefficients (R 2 ) of 0.999. The limits of detection (LODs) of the method for MG and CV were 0.30ng/mL and 0.08ng/mL, respectively, indicating that the Fe 3 O 4 @PEI-MOF-5 material had good adsorption properties for MG and CV. Fe 3 O 4 @PEI-MOF-5 can be expected to also provide efficient enrichment of MG and CV in other complex matrices. Copyright © 2018 Elsevier B.V. All rights reserved.

Blue–green afterglow of BaAl{sub 2}O{sub 4}:Dy{sup 3+} phosphors

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

Zhai, Bao-gai; Ma, Qing-lan; School of Electronics and Information, Nantong University, Jiangsu 226019

Highlights: • Afterglow can be achieved when Eu{sup 2+} is absent in the DyAl{sub 2}O{sub 4}:Dy{sup 3+} phosphors. • The afterglow of DyAl{sub 2}O{sub 4}:Dy{sup 3+} phosphors is discernible to naked eyes for minutes. • Dy{sup 3+} introduced trap centers are believed to be responsible for the afterglow. - Abstract: Dy{sup 3+} doped barium aluminate (BaAl{sub 2}O{sub 4}:Dy{sup 3+}) phosphors were prepared via the sol–gel combustion route at the ignition temperature of 600 °C. The phosphors were characterized with X-ray diffractometry, scanning electron microscopy, transmission electron microscopy, photoluminescence spectroscopy, Fourier transform infrared spectroscopy and X-ray photoelectron spectroscopy. Regardless of themore » absence of Eu{sup 2+} luminescent centers, broadband blue–green afterglow with its peak at about 490 nm was recorded in the BaAl{sub 2}O{sub 4}:Dy{sup 3+} phosphors. The decay profile of the blue–green afterglow can be best fitted into a two-component exponential function with the two lifetime decay constants to be 8.81 and 45.25 s, respectively. The observation of blue–green afterglow from BaAl{sub 2}O{sub 4}:Dy{sup 3+} in the absence of Eu{sup 2+} provides unique opportunity in unveiling the afterglow mechanisms of rare-earth doped alkaline-metal aluminates. Possible mechanisms on the blue–green afterglow in BaAl{sub 2}O{sub 4}:Dy{sup 3+} phosphors are discussed in terms of the Dy{sup 3+} ions introduced trap centers as well as luminescent centers in the crystal lattice.« less

The effect of metal cluster deposition route on structure and photocatalytic activity of mono- and bimetallic nanoparticles supported on TiO2 by radiolytic method

NASA Astrophysics Data System (ADS)

Klein, Marek; Nadolna, Joanna; Gołąbiewska, Anna; Mazierski, Paweł; Klimczuk, Tomasz; Remita, Hynd; Zaleska-Medynska, Adriana

2016-08-01

TiO2 (P25) was modified with small and relatively monodisperse mono- and bimetallic clusters (Ag, Pd, Pt, Ag/Pd, Ag/Pt and Pd/Pt) induced by radiolysis to improve its photocatalytic activity. The as-prepared samples were characterized by X-ray fluorescence spectrometry (XRF), photoluminescence spectrometry (PL), diffuse reflectance spectroscopy (DRS), X-ray powder diffractometry (XRD), scanning transition electron microscopy (STEM) and BET surface area analysis. The effect of metal type (mono- and bimetallic modification) as well as deposition method (simultaneous or subsequent deposition of two metals) on the photocatalytic activity in toluene removal in gas phase under UV-vis irradiation (light-emitting diodes- LEDs) and phenol degradation in liquid phase under visible light irradiation (λ > 420 nm) were investigated. The highest photoactivity under Vis light was observed for TiO2 co-loaded with platinum (0.1%) and palladium (0.1%) clusters. Simultaneous addition of metal precursors results in formation of larger metal nanoparticles (15-30 nm) on TiO2 surface and enhances the Vis-induced activity of Ag/Pd-TiO2 up to four times, while the subsequent metal ions addition results in formation of metal particle size ranging from 4 to 20 nm. Subsequent addition of metal precursors results in formation of BNPs (bimetallic nanoparticle) composites showing higher stability in four cycles of toluene degradation under UV-vis. Obtained results indicated that direct electron transfer from the BNPs to the conduction band of the semiconductor is responsible for visible light photoactivity, whereas superoxide radicals (such as O2rad- and rad OOH) are responsible for pollutants degradation over metal-TiO2 composites.

Modified extrusion-spheronization as a technique of microencapsulation for stabilization of choline bitartrate using hydrogenated soya bean oil

PubMed Central

Gangurde, Avinash Bhaskar; Sav, Ajay Kumar; Javeer, Sharadchandra Dagadu; Moravkar, Kailas K; Pawar, Jaywant N; Amin, Purnima D

2015-01-01

Introduction: Choline bitartrate (CBT) is a vital nutrient for fetal brain development and memory function. It is hygroscopic in nature which is associated with stability related problem during storage such as development of fishy odor and discoloration. Aim: Microencapsulation method was adopted to resolve the stability problem and for this hydrogenated soya bean oil (HSO) was used as encapsulating agent. Materials and Methods: Industrially feasible modified extrusion-spheronization technique was selected for microencapsulation. HSO was used as encapsulating agent, hydroxypropyl methyl cellulose E5/E15 as binder and microcrystalline cellulose as spheronization aid. Formulated pellets were evaluated for parameters such as flow property, morphological characteristics, hardness-friability index (HFI), drug content, encapsulation efficiency, and in vitro drug release. The optimized formulations were also characterized for particle size (by laser diffractometry), differential scanning calorimetry, powder X-ray diffractometry (PXRD), Fourier transform infrared spectroscopy, and scanning electron microscopy. Results and Discussions: The results from the study showed that coating of 90% and 60% CBT was successful with respect to all desired evaluation parameters. Optimized formulation was kept for 6 months stability study as per ICH guidelines, and there was no change in color, moisture content, drug content, and no fishy odor was observed. Conclusion: Microencapsulated pellets of CBT using HSO as encapsulating agent were developed using modified extrusion spheronization technique. Optimized formulations, CBT 90% (F5), and CBT 60% (F10), were found to be stable for 4M and 6M, respectively, at accelerated conditions. PMID:26682198

Atmospheric electron x-ray spectrometer

NASA Technical Reports Server (NTRS)

Feldman, Jason E. (Inventor); George, Thomas (Inventor); Wilcox, Jaroslava Z. (Inventor)

2002-01-01

The present invention comprises an apparatus for performing in-situ elemental analyses of surfaces. The invention comprises an atmospheric electron x-ray spectrometer with an electron column which generates, accelerates, and focuses electrons in a column which is isolated from ambient pressure by a:thin, electron transparent membrane. After passing through the membrane, the electrons impinge on the sample in atmosphere to generate characteristic x-rays. An x-ray detector, shaping amplifier, and multi-channel analyzer are used for x-ray detection and signal analysis. By comparing the resultant data to known x-ray spectral signatures, the elemental composition of the surface can be determined.

Rapid disintegrating tablets of simvastatin dispersions in polyoxyethylene–polypropylene block copolymer for maximized disintegration and dissolution

PubMed Central

Balata, Gehan F; Zidan, Ahmad S; Abourehab, Mohamad AS; Essa, Ebtessam A

2016-01-01

The objective of this research was to improve the dissolution of simvastatin and to incorporate it in rapid disintegrating tablets (RDTs) with an optimized disintegration and dissolution characteristics. Polyoxyethylene–polypropylene block copolymer (poloxamer 188) was employed as a hydrophilic carrier to prepare simvastatin solid dispersions (SDs). Fourier transform infrared spectroscopy, differential scanning calorimetry (DSC) and X-ray diffractometry were employed to understand the interaction between the drug and the carrier in the solid state. The results obtained from Fourier transform infrared spectroscopy showed absence of any chemical interaction between the drug and poloxamer. The results of differential scanning calorimetry and X-ray diffractometry confirmed the conversion of simvastatin to distorted crystalline state. The SD of 1:2 w/w drug to carrier ratio showed the highest dissolution; hence, it was incorporated in RDT formulations using a 32 full factorial design and response surface methodology. The initial assessments of RDTs demonstrated an acceptable flow, hardness, and friability to indicate good mechanical strength. The interaction and Pareto charts indicated that percentage of croscarmellose sodium incorporated was the most important factor affecting the disintegration time and dissolution parameter followed by the hardness value and their interaction effect. Compression force showed a superior influence to increase RDT’s porosity and to fasten disintegration rather than swelling action by croscarmellose sodium. On the other hand, croscarmellose sodium was most important for the initial simvastatin release. The results suggest the potential use of poloxamer 188-based SD in RDT for the oral delivery of poor water-soluble antihyperlipidemic drug, simvastatin. PMID:27757012

Thin calcium phosphate coatings on titanium by electrochemical deposition in modified simulated body fluid.

PubMed

Peng, Ping; Kumar, Sunil; Voelcker, Nicolas H; Szili, Endre; Smart, Roger St C; Griesser, Hans J

2006-02-01

Adherent and optically semitransparent thin calcium phosphate (CaP) films were electrochemically deposited on titanium substrates in a modified simulated body fluid at 37 degrees C. Coatings deposited by using periodic pulsed potentials showed better adhesion and better mechanical properties than coatings deposited with use of a constant potential. Scanning electron microscopy was used to study the morphology of the coatings. The coatings displayed a polydispersed porous structure with pores in the range of a few nanometers to 1 mum. Furthermore, X-ray diffractometry and the O(1s) satellite peaks in X-ray photoelectron spectroscopy indicated that the coatings possessed a similar surface chemistry to that of natural bone minerals. These results were confirmed by inductively coupled plasma optical emission spectrometry, which yielded a Ca:P ratio of 1.65, close to that of hydroxyapatite. Contact mode atomic force microscopy (AFM) showed the average thickness of the coatings was in the order of 200 nm. Root-mean-square (RMS) roughness values, also derived by AFM, were shown to be much higher on the titanium-CaP surfaces in comparison with untreated titanium substrates, with RMS values of about 300 and 110 nm, respectively. Cell culture experiments showed that the CaP surfaces are nontoxic to MG63 osteoblastic cells in vitro and were able to support cell growth for up to 4 days, outperforming the untreated titanium surface in a direct comparison. These easily prepared coatings show promise for hard-tissue biomaterials. (c) 2005 Wiley Periodicals, Inc.

Fluorescence properties of alloyed ZnSeS quantum dots overcoated with ZnTe and ZnTe/ZnS shells

NASA Astrophysics Data System (ADS)

Adegoke, Oluwasesan; Mashazi, Philani; Nyokong, Tebello; Forbes, Patricia B. C.

2016-04-01

Fluorescent alloyed ternary ZnSeS quantum dots (QDs) have been synthesized via the pyrolysis of organometallic precursors. The effects of passivation of ZnTe and ZnTe/ZnS shells on the optical properties of the ternary alloyed ZnSeS core have been studied. A ligand exchange reaction using L-cysteine as a capping ligand was used to obtain water-soluble nanocrystals. The nanocrystals were each characterized by UV/vis absorption and fluorescence spectroscopy, transmission electron microscopy, X-ray diffractometry (XRD) and X-ray photoelectron spectroscopy (XPS). The photoluminescence (PL) quantum yield (QY) of alloyed ZnSeS QDs was 14% and this value increased to 27% when ZnTe was overcoated around the surface but further coating with a ZnS shell decreased the PL QY slightly to 24%. This implies that ZnTe shell suppressed non-radiative recombination exciton states in the alloyed core while further layering with a ZnS shell offered no further improvement in suppressing the defect states. XPS analysis confirmed the presence of the first shell layering but showed a weakened intensity signal of S (2p) and Se (3d) for the ZnSeS/ZnTe/ZnS QDs. Our work demonstrates for the first time that shell passivation of alloyed Zn-based QDs can offer improved optical properties. We hope the optical information presented in this work will be useful in the selection of alloyed Zn-based QDs appropriate for the intended application.

SHS synthesis of Si-SiC composite powders using Mg and reactants from industrial waste

NASA Astrophysics Data System (ADS)

Chanadee, Tawat

2017-11-01

Si-SiC composite powders were synthesized by self-propagating high-temperature synthesis (SHS) using reactants of fly ash-based silica, sawdust-based activated carbon, and magnesium. Fly ash-based silica and sawdust-based activated carbon were prepared from coal mining fly ash and Para rubber-wood sawdust, respectively. The work investigated the effects of the synthesis atmosphere (air and Ar) on the phase and morphology of the SHS products. The SHS product was leached by a two-step acid leaching processes, to obtain the Si-SiC composite powder. The SHS product and SHS product after leaching were characterized by X-ray diffractometry, scanning electron microscopy and energy dispersive X-ray spectrometry. The results indicated that the SHS product synthesized in air consisted of Si, SiC, MgO, and intermediate phases (SiO2, Mg, Mg2SiO4, Mg2Si), whereas the SHS product synthesized in Ar consisted of Si, SiC, MgO and a little Mg2SiO4. The SiC content in the leached-SHS product was higher when Ar was used as the synthesis atmosphere. As well as affecting the purity, the synthesis atmospheres also affected the average crystalline sizes of the products. The crystalline size of the product synthesized in Ar was smaller than that of the product synthesized in air. All of the results showed that fly ash and sawdust could be effective waste-material reactants for the synthesis of Si-SiC composite powders.

Growth and Characteristic of Amorphous Nano-Granular TeO2-V2O5-NiO Thin Films

NASA Astrophysics Data System (ADS)

Hosseinzadeh, Sh.; Rahmati, A.; Bidadi, H.

2016-12-01

TeO2-V2O5-NiO thin films were deposited using thermal evaporation from 40TeO2-(60-y)V2O5-yNiO (y=0-30mol%) target. Structural analysis of the films was identified by X-ray diffractometry (XRD) and scanning electron microscopy (SEM). The amorphous TeO2-V2O5-NiO films have nanosized clear grain structure and sharp grain boundaries. DC conductivity and current-voltage (I-V) characteristic of TeO2-V2O5-NiO thin films were measured in the temperature range of 300-423K. As nickel oxide (NiO) content increases, the DC conductivity decreases up to two orders in value (10-9-10-11Sṡcm-1). Temperature dependence of conductivity is described using the small polaron hopping (SPH) model as well. Poole-Frenkel effect is observed at high external electric field. The optical absorption spectra of the TeO2-V2O5-NiO thin films were recorded in the wavelength range of 380-1100nm. The absorption coefficient revealed bandgap shrinkage (3.01-2.3eV) and band tail widening, due to an increase in NiO content. Energy dispersive X-ray spectroscopy (EDX) was used to determine elemental composition. In TeO2-V2O5-NiO thin films, the NiO content is around fifth of the initial target.

Surface engineering of nanoparticles with macromolecules for epoxy curing: Development of super-reactive nitrogen-rich nanosilica through surface chemistry manipulation

NASA Astrophysics Data System (ADS)

Jouyandeh, Maryam; Jazani, Omid Moini; Navarchian, Amir H.; Shabanian, Meisam; Vahabi, Henri; Saeb, Mohammad Reza

2018-07-01

Curing behavior of epoxy-based nanocomposites depends on dispersion state of nanofillers and their physical and chemical interactions with the curing moieties. In this work, a systematic approach was introduced for chemical functionalization of nanoparticles with macromolecules in order to enrich crosslinking potential of epoxy/amine systems, particularly at late stages of cure where the curing is diffusion-controlled. Super-reactive hyperbranched polyethylenimine (PEI)-attached nanosilica was materialized in this work to facilitate epoxy-amine curing. Starting from coupling [3-(2,3-epoxypropoxy) propyl] trimethoxysilane (EPPTMS) with hyperbranched PEI, a super-reactive macromolecule was obtained and subsequently grafted onto the nanosilica surface. Eventually, a thermally-stable highly-curable nanocomposite was attained by replacement of amine and imine groups of the PEI with imide and amide groups through the reaction with pyromellitic acid dianhydride. Fourier-transform infrared spectrophotometry, X-ray diffractometry, X-ray photoelectron spectroscopy and transmission electron microscopy approved successful grafting of polymer chains onto the nanosilica surface. Thermogravimetric analyses approved a relatively high grafting ratio of ca. 21%. Curing potential of the developed super-reactive nanoparticle was uncovered through nonisothermal differential scanning calorimetry signifying an enthalpy rise of ca. 120 J/g by addition of 2 wt.% to epoxy at 5 °C/min heating rate. Even at low concentration of 0.5 wt.%, the glass transition temperature of epoxy increased from 128 to 156 °C, demonstrating prolonged crosslinking.

Electron and fluorescence spectra of a water molecule irradiated by an x-ray free-electron laser pulse

NASA Astrophysics Data System (ADS)

Schäfer, Julia M.; Inhester, Ludger; Son, Sang-Kil; Fink, Reinhold F.; Santra, Robin

2018-05-01

With the highly intense x-ray light generated by x-ray free-electron lasers (XFELs), molecular samples can be ionized many times in a single pulse. Here we report on a computational study of molecular spectroscopy at the high x-ray intensity provided by XFELs. Calculated photoelectron, Auger electron, and x-ray fluorescence spectra are presented for a single water molecule that reaches many electronic hole configurations through repeated ionization steps. The rich details shown in the spectra depend on the x-ray pulse parameters in a nonintuitive way. We discuss how the observed trends can be explained by the competition of microscopic electronic transition processes. A detailed comparison between spectra calculated within the independent-atom model and within the molecular-orbital framework highlights the chemical sensitivity of the spectral lines of multiple-hole configurations. Our results demonstrate how x-ray multiphoton ionization-related effects such as charge-rearrangement-enhanced x-ray ionization of molecules and frustrated absorption manifest themselves in the electron and fluorescence spectra.

Hydration reactivity of crystalline and vitrified diopside under hydrothermal conditions

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

Grzeszczyk, S.; Szuba, J.

1990-07-01

Hydration reactivity of diopside in both the crystalline and amorphous (glassy) phase was studied under hydrothermal conditions. Samples were treated in an autoclave at 200{degrees}C in saturated vapor for 24 and 72 h. The progress of hydration was determined by X-ray powder diffractometry and IR spectroscopy. Results indicate that crystalline diopside possessed poor hydraulic activity. However, once vitrified it proved to be much more reactive. The principal hydration products found for the glassy diopside after 24 and 72 h of treatment were calcium silicate hydrate (xonotlite) and magnesium silicate hydrates (chrysotile and tremolite).

Structural and mechanical behaviour of LLDPE/HNT nanocomposite films

NASA Astrophysics Data System (ADS)

Čermák, M.; Kadlec, P.; Šutta, P.; Polanský, R.

2016-03-01

The paper briefly describes structural and mechanical influences of Halloysite nanotubes (HNT) in different level of fulfilment (0, 1, 3, 7 wt%) in the LLDPE commonly used in the cable industry. The influence of HNT on the polymer has been observed and evaluated through the average crystallite size and the micro- deformation by X-Ray diffractometry and the imaging of SEM. Despite the certain inter-phase tension between the polymer and HNT, the influence on the mechanical and combustion behaviour was observed. Measurement showed a higher content of agglomerates in the sample with 7 wt% HNT fulfilment.

Atomic force microscope studies of fullerene films - Highly stable C60 fcc (311) free surfaces

NASA Technical Reports Server (NTRS)

Snyder, Eric J.; Tong, William M.; Williams, R. S.; Anz, Samir J.; Anderson, Mark S.

1991-01-01

Atomic force microscopy and X-ray diffractometry were used to study 1500 A-thick films of pure C60 grown by sublimation in ultrahigh vacuum onto a CaF2 (111) substrte. Topographs of the films did not reveal the expected close-packed structures, but they showed instead large regions that correspond to a face-centered cubic (311) surface and distortions of this surface. The open (311) structure may have a relatively low free energy because the low packing density contributes to a high entropy of the exposed surface.

Preparation and Thermoelectric Properties of IR(sub x)Co(sub 1-x)Sb(sub 2) Alloys

NASA Technical Reports Server (NTRS)

Caillat, Thierry

1995-01-01

The preparation and characterization of the binary arsenopyrite compounds CoSb2 and IrSb2 and IrxCo1-xSb2 alloys is reported. Single crystals of CoSb2 were grown by the vertical gradient freeze technique from solution rich in antimony. Polycrystalline samples of IrSb2 and IrxCo1-xSb2 alloys were prepared by hot-pressing of prereacted elemental powders. Samples were investigated by X-ray diffractometry, microprobe analysis and density measurements. It was found that a range of solid solution exist in the system IrxCo1-xSb2 for 0.1

Investigation of the hard x-ray background in backlit pinhole imagers.

PubMed

Fein, J R; Peebles, J L; Keiter, P A; Holloway, J P; Klein, S R; Kuranz, C C; Manuel, M J-E; Drake, R P

2014-11-01

Hard x-rays from laser-produced hot electrons (>10 keV) in backlit pinhole imagers can give rise to a background signal that decreases signal dynamic range in radiographs. Consequently, significant uncertainties are introduced to the measured optical depth of imaged plasmas. Past experiments have demonstrated that hard x-rays are produced when hot electrons interact with the high-Z pinhole substrate used to collimate the softer He-α x-ray source. Results are presented from recent experiments performed on the OMEGA-60 laser to further study the production of hard x-rays in the pinhole substrate and how these x-rays contribute to the background signal in radiographs. Radiographic image plates measured hard x-rays from pinhole imagers with Mo, Sn, and Ta pinhole substrates. The variation in background signal between pinhole substrates provides evidence that much of this background comes from x-rays produced in the pinhole substrate itself. A Monte Carlo electron transport code was used to model x-ray production from hot electrons interacting in the pinhole substrate, as well as to model measurements of x-rays from the irradiated side of the targets, recorded by a bremsstrahlung x-ray spectrometer. Inconsistencies in inferred hot electron distributions between the different pinhole substrate materials demonstrate that additional sources of hot electrons beyond those modeled may produce hard x-rays in the pinhole substrate.

Investigation of the hard x-ray background in backlit pinhole imagers

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

Fein, J. R., E-mail: jrfein@umich.edu; Holloway, J. P.; Peebles, J. L.

Hard x-rays from laser-produced hot electrons (>10 keV) in backlit pinhole imagers can give rise to a background signal that decreases signal dynamic range in radiographs. Consequently, significant uncertainties are introduced to the measured optical depth of imaged plasmas. Past experiments have demonstrated that hard x-rays are produced when hot electrons interact with the high-Z pinhole substrate used to collimate the softer He-α x-ray source. Results are presented from recent experiments performed on the OMEGA-60 laser to further study the production of hard x-rays in the pinhole substrate and how these x-rays contribute to the background signal in radiographs. Radiographicmore » image plates measured hard x-rays from pinhole imagers with Mo, Sn, and Ta pinhole substrates. The variation in background signal between pinhole substrates provides evidence that much of this background comes from x-rays produced in the pinhole substrate itself. A Monte Carlo electron transport code was used to model x-ray production from hot electrons interacting in the pinhole substrate, as well as to model measurements of x-rays from the irradiated side of the targets, recorded by a bremsstrahlung x-ray spectrometer. Inconsistencies in inferred hot electron distributions between the different pinhole substrate materials demonstrate that additional sources of hot electrons beyond those modeled may produce hard x-rays in the pinhole substrate.« less

Miniaturized High-Speed Modulated X-Ray Source

NASA Technical Reports Server (NTRS)

Gendreau, Keith C. (Inventor); Arzoumanian, Zaven (Inventor); Kenyon, Steven J. (Inventor); Spartana, Nick Salvatore (Inventor)

2015-01-01

A miniaturized high-speed modulated X-ray source (MXS) device and a method for rapidly and arbitrarily varying with time the output X-ray photon intensities and energies. The MXS device includes an ultraviolet emitter that emits ultraviolet light, a photocathode operably coupled to the ultraviolet light-emitting diode that emits electrons, an electron multiplier operably coupled to the photocathode that multiplies incident electrons, and an anode operably coupled to the electron multiplier that is configured to produce X-rays. The method for modulating MXS includes modulating an intensity of an ultraviolet emitter to emit ultraviolet light, generating electrons in response to the ultraviolet light, multiplying the electrons to become more electrons, and producing X-rays by an anode that includes a target material configured to produce X-rays in response to impact of the more electrons.

Relationship between crystal structure and solid-state properties of pharmaceuticals

NASA Astrophysics Data System (ADS)

Sheth, Agam R.

This thesis strives to understand the structure-property relationships of some pharmaceutical crystals at the molecular level with emphasis on the effect of secondary processing on the solid phase. Using single crystal X-ray diffractometry (SCXRD), the structure of warfarin sodium 2-propanol adduct (W) was established to be a true solvate, contrary to previous reports. Using dynamic water vapor sorption, optical and environmental scanning electron microscopy, SCXRD, powder X-ray diffractometry (PXRD), volume computations and molecular modeling, the effect of relative humidity and temperature on the crystal structure of W was investigated. Ab initio calculations on piroxicam showed that the difference in energy between the two polymorphs, I and II, arises predominantly from the difference between their lattice energies. The detailed hydrogen bonding networks of the two polymorphs are described and compared using graph sets. Despite stabilization of the polymorphs by hydrogen bonds, pair-wise distribution function transforms show a loss of polymorphic memory upon cryogrinding the two polymorphs, leading to a difference in recrystallization behavior between amorphous piroxicam prepared from polymorphs I and II. Structural and solid-state changes of piroxicam polymorphs under mechanical stress were investigated using cryogenic grinding, PXRD, diffuse-reflectance solid-state ultraviolet-visible spectroscopy, 13C solid-state nuclear magnetic resonance spectroscopy, and diffuse-reflectance solid-state Fourier-transform infrared spectroscopy. Intermolecular proton transfer was found to accompany changes in phase and color observed upon cryogrinding the two polymorphs. Model-free and model-fitting studies of the dehydration kinetics of piroxicam monohydrate (PM) showed the dependence of activation energy ( Ea) on both isothermal and non-isothermal heating conditions, and on the fraction of conversion. In the constant-E a region, isothermal dehydration follows the two-dimensional phase boundary model, while non-isothermal dehydration follows a mechanism intermediate between two- and three-dimensional diffusion that cannot be described by any of the common models. Structural studies suggest that the complex hydrogen bond pattern in PM is responsible for the observed dehydration behavior. Ab initio calculations provide an explanation for the changes in the molecular and crystal structures accompanying the reversible change in hydration state between anhydrous piroxicam Form I and PM. The thesis further demonstrates the utility of model-free analysis in describing complex dehydration kinetics.

Note: Measurement of the runaway electrons in the J-TEXT tokamak

NASA Astrophysics Data System (ADS)

Chen, Z. Y.; Zhang, Y.; Zhang, X. Q.; Luo, Y. H.; Jin, W.; Li, J. C.; Chen, Z. P.; Wang, Z. J.; Yang, Z. J.; Zhuang, G.

2012-05-01

The runaway electrons have been measured by hard x-ray detectors and soft x-ray array in the J-TEXT tokamak. The hard x-ray radiations in the energy ranges of 0.5-5 MeV are measured by two NaI detectors. The flux of lost runaway electrons can be obtained routinely. The soft x-ray array diagnostics are used to monitor the runaway beam generated in disruptions since the soft x-ray is dominated by the interaction between runaway electrons and metallic impurities inside the plasma. With the aid of soft x-ray array, runaway electron beam has been detected directly during the formation of runaway current plateau following the disruptions.

Estimation of Crystallinity of Nifedipine-Polyvinylpyrrolidone Solid Dispersion by Usage of Terahertz Time-Domain Spectroscopy and of X-Ray Powder Diffractometer.

PubMed

Takeuchi, Issei; Shimakura, Kemmaro; Kuroda, Hideki; Nakajima, Takehisa; Goto, Satoru; Makino, Kimiko

2015-12-01

Crystalline state of pharmaceutical materials is of great importance in preparation of pharmaceutics, because their physicochemical properties affect bioavailability, quality of products, therapeutic level and manufacturing process. In this study, we have estimated time-dependent changes of nifedipine in nifedipine-polyvinylpyrrolidone (PVP) solid dispersion by measuring terahertz time-domain spectroscopy (THz-TDS) and by X-ray powder diffractometry (XRPD), and compared their correlativity. Crystallinity of nifedipine-PVP solid dispersion was changed by storing the amorphous sample at 25°C-75°C and relative humidity of over 80% for 0.25-24.00 h. To compare the results of two types of measurements, we have used a general method of linear regression analysis. Crystallinities estimated using THz-TDS were plotted on the x-axis and that of XRPD were on the y-axis. From the result of the calculation, the correlativity of them was confirmed. THz-TDS has the capability of becoming the replacement of XRPD. © 2015 Wiley Periodicals, Inc. and the American Pharmacists Association.

CT Colonography (Virtual Colonoscopy)

MedlinePlus

... Rotating around you, the x-ray tube and electronic x-ray detectors are located opposite each other ... numerous x-ray beams and a set of electronic x-ray detectors rotate around you, measuring the ...

Few-femtosecond time-resolved measurements of X-ray free-electron lasers.

PubMed

Behrens, C; Decker, F-J; Ding, Y; Dolgashev, V A; Frisch, J; Huang, Z; Krejcik, P; Loos, H; Lutman, A; Maxwell, T J; Turner, J; Wang, J; Wang, M-H; Welch, J; Wu, J

2014-04-30

X-ray free-electron lasers, with pulse durations ranging from a few to several hundred femtoseconds, are uniquely suited for studying atomic, molecular, chemical and biological systems. Characterizing the temporal profiles of these femtosecond X-ray pulses that vary from shot to shot is not only challenging but also important for data interpretation. Here we report the time-resolved measurements of X-ray free-electron lasers by using an X-band radiofrequency transverse deflector at the Linac Coherent Light Source. We demonstrate this method to be a simple, non-invasive technique with a large dynamic range for single-shot electron and X-ray temporal characterization. A resolution of less than 1 fs root mean square has been achieved for soft X-ray pulses. The lasing evolution along the undulator has been studied with the electron trapping being observed as the X-ray peak power approaches 100 GW.

Electrochromic Properties of Tungsten Oxide Films Prepared by Reactive Sputtering

NASA Astrophysics Data System (ADS)

Kim, Min Hong; Kang, Tai Young; Jung, Yu Sup; Kim, Kyung Hwan

2013-05-01

WO3-x thin films were deposited on induim tin oxide (ITO) glass substrates with various oxygen flow ratios from 0.55 to 0.7 by the reactive facing-target sputtering method, at a power density of 4 W/cm2 and room temperature. The structural properties of the WO3-x thin films were measured by X-ray diffractometry and Raman spectral analysis. As-deposited WO3-x thin films had an amorphous structure. In the Raman spectra, WO3-x thin films exhibited two strong peaks at 770 and 950 cm-1 attributed to the vibrations of W6+-O and W6+=O bonds, respectively. The electrochemical and optical properties of WO3-x thin films were measured by cyclic voltammetry and UV/vis spectrometry. The results showed the highest charge density at an oxygen flow ratio of 0.7 and the highest transmittance in the visible range. The maximum coloration efficiency was 30.82 cm2/C at an oxygen flow ratio of 0.7.

Development of scanning electron and x-ray microscope

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

Matsumura, Tomokazu, E-mail: tomokzau.matsumura@etd.hpk.co.jp; Hirano, Tomohiko, E-mail: tomohiko.hirano@etd.hpk.co.jp; Suyama, Motohiro, E-mail: suyama@etd.hpk.co.jp

We have developed a new type of microscope possessing a unique feature of observing both scanning electron and X-ray images under one unit. Unlike former X-ray microscopes using SEM [1, 2], this scanning electron and X-ray (SELX) microscope has a sample in vacuum, thus it enables one to observe a surface structure of a sample by SEM mode, to search the region of interest, and to observe an X-ray image which transmits the region. For the X-ray observation, we have been focusing on the soft X-ray region from 280 eV to 3 keV to observe some bio samples and softmore » materials. The resolutions of SEM and X-ray modes are 50 nm and 100 nm, respectively, at the electron energy of 7 keV.« less

Toxicological aspects of photocatalytic degradation of selected xenobiotics with nano-sized Mn-doped TiO2.

PubMed

Ozmen, Murat; Güngördü, Abbas; Erdemoglu, Sema; Ozmen, Nesrin; Asilturk, Meltem

2015-08-01

The toxic effects of two selected xenobiotics, bisphenol A (BPA) and atrazine (ATZ), were evaluated after photocatalytic degradation using nano-sized, Mn-doped TiO2. Undoped and Mn-doped TiO2 nanoparticles were synthesized. The samples were characterized by X-ray diffractometry (XRD), scanning electron microscopy (SEM), UV-vis-diffuse reflectance spectra (DRS), X-ray fluorescence spectroscopy (XRF), and BET surface area. The photocatalytic efficiency of the undoped and Mn-doped TiO2 was evaluated for BPA and ATZ. The toxicity of the synthesized photocatalysts and photocatalytic by-products of BPA and ATZ was determined using frog embryos and tadpoles, zebrafish embryos, and bioluminescent bacteria. Possible toxic effects were also evaluated using selected enzyme biomarkers. The results showed that Mn-doped TiO2 nanoparticles did not cause significant lethality in Xenopus laevis embryos and tadpoles, but nonfiltered samples caused lethality in zebrafish. Furthermore, Mn-doping of TiO2 increased the photocatalytic degradation capability of nanoparticles, and it successfully degraded BPA and AZT, but degradation of AZT caused an increase of the lethal effects on both tadpoles and fish embryos. Degradation of BPA caused a significant reduction of lethal effects, especially after 2-4h of degradation. However, biochemical assays showed that both Mn-doped TiO2 and the degradation by-products caused a significant change of selected biomarkers on X. laevis tadpoles; thus, the ecological risks of Mn-doped TiO2 should be considered due to nanomaterial applications and for spilled nanoparticles in an aquatic ecosystem. Also, the risk of nanoparticles should be considered using indicator reference biochemical markers to verify the environmental health impacts. Copyright © 2015 Elsevier B.V. All rights reserved.

Optical, Fluorescence with quantum analysis of hydrazine (1, 3- Dinitro Phenyl) by DFT and Ab initio approach

NASA Astrophysics Data System (ADS)

Cecily Mary Glory, D.; Sambathkumar, K.; Madivanane, R.; Velmurugan, G.; Gayathri, R.; Nithiyanantham, S.; Venkatachalapathy, M.; Rajkamal, N.

2018-07-01

Experimental and computational study of molecular structure, vibrational and UV-spectral analysis of Hydrazine (1, 3- Dinitrophenyl) (HDP) derivatives. The crystal was grown by slow cooling method and the crystalline perfection of single crystals was evaluated by high resolution X-ray diffractometry (HRXRD) using a multicrystal X-ray diffractometer. Fluorescence, FT-IR and FT-Raman spectra of HDP crystal were recorded. The assignments of the vibrational spectra have been carried out with the help of normal co-ordinate analysis (NCA) followed by scaled quantum force field methodology (SQMFF). NMR studies have confirmed respectively the crystal structure and functional groups of the grown crystal. The energy and oscillator strength calculated by Time-Dependent Density Functional Theory (TD-DFT) result complements the experimental findings. The calculated MESP, UV, HOMO-LUMO energies show that charge transfer done within the molecule. And various thermodynamic parameters are studied. Fukui determines the local reactive site of electrophilic, nucleophilic, descriptor.

Electrochemical properties of monolithic nickel sulfide electrodes for use in sodium batteries

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

Go, Dae-Yeon; Park, Jinsoo, E-mail: jsp@ikw.ac.kr; Noh, Pan-Jin

2014-10-15

Highlights: • We succeeded in preparing monolithic Ni{sub 3}S{sub 2} integrated electrode through the sulfuration. • The sulfuration is a facile and useful method to synthesize metal sulfides with nanostructure. • As-prepared monolithic Ni{sub 3}S{sub 2} electrodes showed very stable and cycle performance over charge/discharge cycling. - Abstract: Monolithic nickel sulfide electrodes were prepared using a facile synthesis method, sulfuration and annealing. As-prepared Ni{sub 3}S{sub 2} electrodes were characterized by X-ray diffractometry and field emission scanning electron microscopy. Thermal stability was determined by thermal gravimetric analysis and differential scanning calorimetry. Electrochemical properties were measured by galvanostatic charge and discharge cyclingmore » for Na-ion batteries. Three kinds of Ni{sub 3}S{sub 2} electrodes were prepared by varying the sulfuration time (5, 15 and 25 min). The electrochemical results indicated that the capacities increased with an increase in sulfuration time and the cycle performance was stable as a result of monolithic integration of nanostructured Ni{sub 3}S{sub 2} on Ni plates, leading to low interfacial resistance.« less

Preparation and physical properties of tara gum film reinforced with cellulose nanocrystals.

PubMed

Ma, Qianyun; Hu, Dongying; Wang, Lijuan

2016-05-01

Cellulose nanocrystals (CNC) prepared from microcrystalline cellulose were blended in tara gum solution to prepare nanocomposite films. The morphology, crystallinity, and thermal properties of the CNC and films were evaluated by using transmission electron microscopy, X-ray diffractometry, and thermogravimetric analysis, respectively. The resultant CNC was rod-shaped with diameters of around 8.6 nm. The effect of CNC content on physical and thermal properties of films was studied. The composite film tensile strength increased from 27.86 to 65.73 MPa, elastic modulus increased from 160.98 MPa to 882.49 MPa and the contact angle increased from 55.8° to 98.7° with increasing CNC content from 0 to 6 wt%. However, CNC addition increased the thermal stability slightly and CNC content above 6 wt% decreased the tensile strength by CNC aggregation in the matrix. The nanocomposite film containing 6 wt% CNC possessed the highest light transmittance, mechanical properties, and lowest oxygen permeability. CNC addition is a suitable method to modify tara gum matrix polymer properties. Copyright © 2016 Elsevier B.V. All rights reserved.

Fundamentals of Passive Oxidation In SiC and Si3N4

NASA Technical Reports Server (NTRS)

Thomas-Ogbuji, Linus U.

1998-01-01

The very slow oxidation kinetics of silicon carbide and silicon nitride, which derive from their adherent and passivating oxide films, has been explored at length in a broad series of studies utilizing thermogravimetric analysis, electron and optical micrography, energy dispersive spectrometry, x-ray diffractometry, micro-analytical depth profiling, etc. Some interesting microstructural phenomena accompanying the process of oxidation in the two materials will be presented. In Si3N4 the oxide is stratified, with an SiO2 topscale (which is relatively impervious to O2)underlain by a coherent subscale of silicon oxynitride which is even less permeable to O2- Such "defence in depth" endows Si3N4 with what is perhaps the highest oxidation resistance of any material, and results in a unique set of oxidation processes. In SiC the oxidation reactions are much simpler, yet new issues still emerge; for instance, studies involving controlled devitrification of the amorphous silica scale confirmed that the oxidation rate of SiC drops by more than an order of magnitude when the oxide scale fully crystallizes.

Synthesis of Lithium Metal Oxide Nanoparticles by Induction Thermal Plasmas.

PubMed

Tanaka, Manabu; Kageyama, Takuya; Sone, Hirotaka; Yoshida, Shuhei; Okamoto, Daisuke; Watanabe, Takayuki

2016-04-06

Lithium metal oxide nanoparticles were synthesized by induction thermal plasma. Four different systems-Li-Mn, Li-Cr, Li-Co, and Li-Ni-were compared to understand formation mechanism of Li-Me oxide nanoparticles in thermal plasma process. Analyses of X-ray diffractometry and electron microscopy showed that Li-Me oxide nanoparticles were successfully synthesized in Li-Mn, Li-Cr, and Li-Co systems. Spinel structured LiMn₂O₄ with truncated octahedral shape was formed. Layer structured LiCrO₂ or LiCoO₂ nanoparticles with polyhedral shapes were also synthesized in Li-Cr or Li-Co systems. By contrast, Li-Ni oxide nanoparticles were not synthesized in the Li-Ni system. Nucleation temperatures of each metal in the considered system were evaluated. The relationship between the nucleation temperature and melting and boiling points suggests that the melting points of metal oxides have a strong influence on the formation of lithium metal oxide nanoparticles. A lower melting temperature leads to a longer reaction time, resulting in a higher fraction of the lithium metal oxide nanoparticles in the prepared nanoparticles.

World's Largest Gold Crystal Studied at Los Alamos

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

Vogel, Sven; Nakotte, Heinz

2014-04-03

When geologist John Rakovan needed better tools to investigate whether a dazzling 217.78-gram piece of gold was in fact the world's largest single-crystal specimen - a distinguishing factor that would not only drastically increase its market value but also provide a unique research opportunity - he traveled to Los Alamos National Laboratory's Lujan Neutron Scattering Center to peer deep inside the mineral using neutron diffractometry. Neutrons, different from other probes such as X-rays and electrons, are able to penetrate many centimeters deep into most materials. Revealing the inner structure of a crystal without destroying the sample - imperative, as thismore » one is worth an estimated $1.5 million - would allow Rakovan and Lujan Center collaborators Sven Vogel and Heinz Nakotte to prove that this exquisite nugget, which seemed almost too perfect and too big to be real, was a single crystal and hence a creation of nature. Its owner, who lives in the United States, provided the samples to Rakovan to assess the crystallinity of four specimens, all of which had been found decades ago in Venezuela.« less

Preparation and characterization of non-crystalline granular starch and corresponding carboxymethyl starch.

PubMed

Zhang, Bao; Li, Xiaomin; Xie, Qiutao; Tao, Han; Wang, Wu; Chen, Han-Qing

2017-10-01

Native corn starch slurried in 50% ethanol solution was treated at 60°C, 70°C, 80°C, and 85°C, respectively. The resultant starches were investigated by polarized microscopy, scanning electron microscopy (SEM), differential scanning calorimetry (DSC), and X-ray diffractometry (XRD). The Maltese cross of ethanol-heating treated starch gradually weaken with increasing temperature and completely disappeared at 85°C. SEM data indicated the treated granular exhibited a rougher surface with more pores and grooves than native starch granular, but the shape of the treated starch was still intact. DSC and XRD data confirmed ethanol-heating treated starch changed from crystalline to non-crystalline structure at 85°C. The highest degree of substitution (DS) and corresponding reaction efficiency (RE) for the carboxymethylation of native starch were 0.66 and 36.7%, respectively, while the corresponding DS and RE for non-crystalline granular starches increased by 0.29 and 16.1% at the same reaction condition, respectively. Copyright © 2017 Elsevier B.V. All rights reserved.

World's Largest Gold Crystal Studied at Los Alamos

ScienceCinema

Vogel, Sven; Nakotte, Heinz

2018-02-07

When geologist John Rakovan needed better tools to investigate whether a dazzling 217.78-gram piece of gold was in fact the world's largest single-crystal specimen - a distinguishing factor that would not only drastically increase its market value but also provide a unique research opportunity - he traveled to Los Alamos National Laboratory's Lujan Neutron Scattering Center to peer deep inside the mineral using neutron diffractometry. Neutrons, different from other probes such as X-rays and electrons, are able to penetrate many centimeters deep into most materials. Revealing the inner structure of a crystal without destroying the sample - imperative, as this one is worth an estimated $1.5 million - would allow Rakovan and Lujan Center collaborators Sven Vogel and Heinz Nakotte to prove that this exquisite nugget, which seemed almost too perfect and too big to be real, was a single crystal and hence a creation of nature. Its owner, who lives in the United States, provided the samples to Rakovan to assess the crystallinity of four specimens, all of which had been found decades ago in Venezuela.

Preparation, characterization and in vitro evaluation of solid dispersions containing docetaxel.

PubMed

Chen, Jie; Qiu, Liyan; Hu, Minxin; Jin, Yi; Han, Jieru

2008-06-01

Solid dispersions using water-soluble carriers were studied for improving the dissolution of docetaxel, a poorly soluble compound. In order to obtain the most optimized formulation, we prepared many solid dispersions with different carriers, different solvents, or at a series of drug-to-carrier ratios, and compared their dissolution. The accumulative dissolution of docetaxel from poloxamer 188 was more excellent than that from PVP(k30) and glyceryl monostearate, and the dissolution of docetaxel from solid dispersion was markedly higher than that of pure docetaxel; meanwhile the increased dissolution was partly dependent on the ratios of docetaxel and poloxamer 188. The ethanol used to prepare solid dispersion is of more significant effect on the dissolution of docetaxel than that of acetone. The docetaxel/poloxamer 188 system was characterized by differential scanning calorimetry (DSC), X-ray diffractometry (XRD), and environmental scanning electron microscope (ESEM). The results of DSC, XRD, and ESEM analyses of docetaxel/poloxamer 188 system showed that there are intermolecular interactions between docetaxel and poloxamer, and the crystallinity of docetaxel disappeared. These results show that solid dispersion is a promising approach of developing docetaxel drug formulates.

Characterization and electrochemical properties of Ni(Si)/Ni5Si2 multiphase coatings prepared by HVOF spraying

NASA Astrophysics Data System (ADS)

Verdian, M. M.; Raeissi, K.; Salehi, M.

2012-11-01

Ni(Si)/Ni5Si2 powders were produced by mechanical alloying (MA) of Ni-25 at.% Si powder mixture. Then, the as-milled powders were sprayed onto copper substrate using high velocity oxy-fuel (HVOF) process. The phase composition and microstructure of the coatings were examined by X-ray diffractometry and scanning electron microscopy. Polarization tests and electrochemical impedance spectroscopy (EIS) measurements were also employed to study corrosion performance of the coatings in 3.5% NaCl solution. The results showed that although single phase Ni3Si was formed during annealing of Ni(Si)/Ni5Si2 powders, but, only Ni(Si) and Ni5Si2 are present in HVOF coatings and no new phase has been formed during spraying. The coatings had microhardness up to 746 HV0.05. Further investigations showed the corrosion performance of multiphase coatings in 3.5% NaCl solution was better than that of copper substrate. The phase transitions during MA, HVOF and annealing processes were discussed in association with Ni-Si phase diagram and nature of each process.

Review of Research Work on Ti-BASED Composite Coatings

NASA Astrophysics Data System (ADS)

Gabbitas, Brian; Salman, Asma; Zhang, Deliang; Cao, Peng

The service life of industrial components is limited predominantly by Chemical corrosion/mechanical wear. The project is concerned with the investigation of the capability of Ti(Al,O)/Al2O3 coatings to improve the service life of tool steel (H13) used for dies in aluminium high pressure die casting. This paper gives a general review on the research work conducted at the University of Waikato on producing and evaluating the titanium/alumina based composite coatings. The powder feedstocks for making the composite coatings were produced by high energy mechanical milling of a mixture of Al and TiO2 powders in two different molar ratios followed by a thermal reaction process. The feedstocks were then thermally sprayed using a high velocity air-fuel (HVAF) technique on H13 steel substrates to produce a Ti(Al,O)/Al2O3 composite coatings. The performance of the coating was assessed in terms of thermal shock resistance and reaction kinetics with molten aluminium. The composite powders and coatings were characterized using scanning electron microscopy (SEM), optical microscopy and X-ray diffractometry (XRD).

Novel Solid Encapsulation of Ethylene Gas Using Amorphous α-Cyclodextrin and the Release Characteristics.

PubMed

Ho, Binh T; Bhandari, Bhesh R

2016-05-04

This research investigated the encapsulation of ethylene gas into amorphous α-cyclodextrins (α-CDs) at low (LM) and high (HM) moisture contents at 1.0-1.5 MPa for 24-120 h and its controlled release characteristics at 11.2-52.9% relative humidity (RH) for 1-168 h. The inclusion complexes (ICs) were characterized using X-ray diffractometry (XRD), nuclear magnetic resonance spectroscopy (CP-MAS (13)C NMR), and scanning electron microscopy (SEM). Ethylene concentrations in the ICs were from 0.45 to 0.87 mol of ethylene/mol CD and from 0.42 to 0.54 mol of ethylene/mol CD for LM and HM α-CDs, respectively. Ethylene gas released from the encapsulated powder at higher rates with increasing RH. An analysis of release kinetics using Avrami's equation showed that the LM and HM amorphous α-CDs were not associated with significant differences in release constant k and parameter n for any given RH condition. NMR spectra showed the presence of the characteristic carbon-carbon double bond of ethylene gas in the encapsulated α-CD powder.

Preparation and Optimization of Amorphous Ursodeoxycholic Acid Nano-suspensions by Nanoprecipitation based on Acid-base Neutralization for Enhanced Dissolution.

PubMed

Xie, Yike; Chen, Zhongjian; Su, Rui; Li, Ye; Qi, Jianping; Wu, Wei; Lu, Yi

2017-01-01

Ursodeoxycholic acid, usually used to dissolve cholesterol gallstones in clinic, is a typical hydrophobic drug with poor oral bioavailability due to dissolution rate-limited performance. The objective of this study was to increase the dissolution of ursodeoxycholic acid by amorphous nanosuspensions. Nanoprecipitation based on acid-base neutralization was used to prepare the nanosuspensions with central composite design to optimize the formula. The nanosuspensions were characterized by particle size, morphology, crystallology and dissolution. The ursodeoxycholic acid nanosuspensions showed mean particle size around 380 nm with polydispersion index value about 0.25. Scanning electron microscope observed high coverage of HPMC-E50 onto the surface of the nanosuspensions. Differential scanning calorimetry and powder X-ray diffractometry revealed amorphous structure of the ursodeoxycholic acid nanosuspensions. A significant increase of dissolution in acidic media was achieved by the amorphous nanosuspensions compared with the physical mixture. It can be predicted that the amorphous nanosuspensions show great potential in improving the oral bioavailability of ursodeoxycholic acid. Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.

Photocatalytic degradation of an azo textile dye (C.I. Reactive Red 195 (3BF)) in aqueous solution over copper cobaltite nanocomposite coated on glass by Doctor Blade method

NASA Astrophysics Data System (ADS)

Habibi, Mohammad Hossein; Rezvani, Zoya

2015-08-01

The degradation of C.I. Reactive Red 195 (3BF) in aqueous solution using copper cobaltite nanocomposite coated on glass by Doctor Blade method was studied. Structural, optical and morphological properties of nanocomposite coatings were characterized by X-ray powder diffractometry (XRD), diffuse reflectance spectroscopy (DRS) and field emission scanning electron microscopy (FESEM). The nanoparticles exhibit a particle size of 31 nm, showing a good nanoscale crystalline morphology. The photocatalytic activity of copper cobaltite nanocomposite coated on glass was studied by performing the photocatalytic degradation of 3BF at different irradiation time. The effect of irradiation time on the degradation of 3BF was studied and the results showed that more than 85% of the 3BF was degraded in 45 min of irradiation. The pseudo-first-order kinetic models were used and the rate constants were evaluated with pseudo first order rate constants of 4.10 × 10-2 min-1. The main advantage of the photocatalyst coated on glass overcomes the difficulties in separation and recycle of photocatalyst suspensions.

Amino Acid Interaction with and Adsorption on Clays: FT-IR and Mössbauer Spectroscopy and X-ray Diffractometry Investigations

NASA Astrophysics Data System (ADS)

Benetoli, Luís O. B.; de Souza, Cláudio M. D.; da Silva, Klébson L.; de Souza, Ivan G.; de Santana, Henrique; Paesano, Andrea; da Costa, Antonio C. S.; Zaia, Cássia Thaïs B. V.; Zaia, Dimas A. M.

2007-12-01

In the present paper, the adsorption of amino acids (Ala, Met, Gln, Cys, Asp, Lys, His) on clays (bentonite, kaolinite) was studied at different pH (3.00, 6.00, 8.00). The amino acids were dissolved in seawater, which contains the major elements. There were two main findings in this study. First, amino acids with a charged R group (Asp, Lys, His) and Cys were adsorbed on clays more than Ala, Met and Gln (uncharged R groups). However, 74% of the amino acids in the proteins of modern organisms have uncharged R groups. These results raise some questions about the role of minerals in providing a prebiotic concentration mechanism for amino acids. Several mechanisms are also discussed that could produce peptide with a greater proportion of amino acids with uncharged R groups. Second, Cys could play an important role in prebiotic chemistry besides participating in the structure of peptides/proteins. The FT-IR spectra showed that the adsorption of amino acids on the clays occurs through the amine group. However, the Cys/clay interaction occurs through the sulfhydryl and amine groups. X-ray diffractometry showed that pH affects the bentonite interlayer, and at pH 3.00 the expansion of Cys/bentonite was greater than that of the samples of ethylene glycol/bentonite saturated with Mg. The Mössbauer spectrum for the sample with absorbed Cys showed a large increase (˜20%) in ferrous ions. This means that Cys was able to partially reduce iron present in bentonite. This result is similar to that which occurs with aconitase where the ferric ions are reduced to Fe 2.5.

Green synthesis palladium nanoparticles mediated by white tea (Camellia sinensis) extract with antioxidant, antibacterial, and antiproliferative activities toward the human leukemia (MOLT-4) cell line.

PubMed

Azizi, Susan; Mahdavi Shahri, Mahnaz; Rahman, Heshu Sulaiman; Rahim, Raha Abdul; Rasedee, Abdullah; Mohamad, Rosfarizan

2017-01-01

Among nanoparticles used for medical applications, palladium nanoparticles (PdNPs) are among the least investigated. This study was undertaken to develop PdNPs by green synthesis using white tea (W.tea; Camellia sinensis ) extract to produce the Pd@W.tea NPs. The Pd@W.tea NPs were characterized by UV-vis spectroscopy and X-ray diffractometry, and evaluated with transmission electron microscopy (TEM) and scanning electron microscopy (SEM). The Pd@W.tea NPs were spherical (size 6-18 nm) and contained phenols and flavonoids acquired from the W.tea extract. Pd@W.tea NPs has good 1-diphenyl-2-picrylhydrazyl (DPPH), OH, and NO-scavenging properties as well as antibacterial effects toward Staphylococcus epidermidis and Escherichia coli . MTT assay showed that Pd@W.tea NPs (IC 50 =0.006 μM) were more antiproliferative toward the human leukemia (MOLT-4) cells than the W.tea extract (IC 50 =0.894 μM), doxorubicin (IC 50 =2.133 μM), or cisplatin (IC 50 =0.013 μM), whereas they were relatively innocuous for normal human fibroblast (HDF-a) cells. The anticancer cell effects of Pd@W.tea NPs are mediated through the induction of apoptosis and G2/M cell-cycle arrest.

A Novel Microcharacterization Technique in the Measurement of Strain and Orientation Gradient in Advanced Materials

NASA Technical Reports Server (NTRS)

Garmestai, H.; Harris, K.; Lourenco, L.

1997-01-01

Representation of morphology and evolution of the microstructure during processing and their relation to properties requires proper experimental techniques. Residual strains, lattice distortion, and texture (micro-texture) at the interface and the matrix of a layered structure or a functionally gradient material and their variation are among parameters important in materials characterization but hard to measure with present experimental techniques. Current techniques available to measure changes in interred material parameters (residual stress, micro-texture, microplasticity) produce results which are either qualitative or unreliable. This problem becomes even more complicated in the case of a temperature variation. These parameters affect many of the mechanical properties of advanced materials including stress-strain relation, ductility, creep, and fatigue. A review of some novel experimental techniques using recent advances in electron microscopy is presented here to measure internal stress, (micro)texture, interracial strength and (sub)grain formation and realignment. Two of these techniques are combined in the chamber of an Environmental Scanning Electron Microscope to measure strain and orientation gradients in advanced materials. These techniques which include Backscattered Kikuchi Diffractometry (BKD) and Microscopic Strain Field Analysis are used to characterize metallic and intermetallic matrix composites and superplastic materials. These techniques are compared with the more conventional x-ray diffraction and indentation techniques.

Microwave assisted synthesis and characterisation of a zinc oxide/tobacco mosaic virus hybrid material. An active hybrid semiconductor in a field-effect transistor device.

PubMed

Sanctis, Shawn; Hoffmann, Rudolf C; Eiben, Sabine; Schneider, Jörg J

2015-01-01

Tobacco mosaic virus (TMV) has been employed as a robust functional template for the fabrication of a TMV/zinc oxide field effect transistor (FET). A microwave based approach, under mild conditions was employed to synthesize stable zinc oxide (ZnO) nanoparticles, employing a molecular precursor. Insightful studies of the decomposition of the precursor were done using NMR spectroscopy and material characterization of the hybrid material derived from the decomposition was achieved using dynamic light scattering (DLS), transmission electron microscopy (TEM), grazing incidence X-ray diffractometry (GI-XRD) and atomic force microscopy (AFM). TEM and DLS data confirm the formation of crystalline ZnO nanoparticles tethered on top of the virus template. GI-XRD investigations exhibit an orientated nature of the deposited ZnO film along the c-axis. FET devices fabricated using the zinc oxide mineralized virus template material demonstrates an operational transistor performance which was achieved without any high-temperature post-processing steps. Moreover, a further improvement in FET performance was observed by adjusting an optimal layer thickness of the deposited ZnO on top of the TMV. Such a bio-inorganic nanocomposite semiconductor material accessible using a mild and straightforward microwave processing technique could open up new future avenues within the field of bio-electronics.

Direct observation of the ferroelectric polarization in the layered perovskite Bi{sub 4}Ti{sub 3}O{sub 12}

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

Urushihara, Daisuke; Asaka, Toru, E-mail: asaka.toru@nitech.ac.jp; Frontier Research Institute for Materials Science, Nagoya Institute of Technology, Nagoya 466-8555

We investigated the crystal structure and ferroelectric domains of Bi{sub 4}Ti{sub 3}O{sub 12} (BTO) by means of transmission electron microscopy (TEM) and single-crystal X-ray diffractometry. From the extinction rule, we determined that the space group in the ferroelectric phase of BTO is P1a1 rather than B2cb and B1a1 which have been proposed previously. We successfully refined the crystal structure based on the space group P1a1. The 180° and 90° ferroelectric domain structures were observed by the [001]-zone dark-field TEM imaging. In the 180° domain structure, we determined that one component of the polarization vector is parallel to the a-axis. Anmore » annular bright-field scanning transmission electron microscopy (ABF-STEM) was performed for the direct observation of the crystal structures. The ABF-STEM images displayed the contrasts with respect to every atomic position in spite of the highly distorted structure of BTO. We could evaluate the tilting and distortion of the [TiO{sub 6}] octahedra relatively. Therefore, we directly observed the ferroelectric displacements of Bi and Ti ions.« less

Organic-Inorganic Hydrophobic Nanocomposite Film with a Core-Shell Structure

PubMed Central

Liu, Peng; Chen, Ying; Yu, Zhiwu

2016-01-01

A method to prepare novel organic-inorganic hydrophobic nanocomposite films was proposed by a site-specific polymerization process. The inorganic part, the core of the nanocomposite, is a ternary SiO2–Al2O3–TiO2 nanoparticles, which is grafted with methacryloxy propyl trimethoxyl silane (KH570), and wrapped by fluoride and siloxane polymers. The synthesized samples are characterized by transmission electron microscopy (TEM), Fourier transform infrared (FTIR) spectrscopy, X-ray diffractometry (XRD), contact angle meter (CA), and scanning electron microscope (SEM). The results indicate that the novel organic-inorganic hydrophobic nanocomposite with a core-shell structure was synthesized successfully. XRD analysis reveals the nanocomposite film has an amorphous structure, and FTIR analysis indicates the nanoparticles react with a silane coupling agent (methacryloxy propyl trimethoxyl silane KH570). Interestingly, the morphology of the nanoparticle film is influenced by the composition of the core. Further, comparing with the film synthesized by silica nanoparticles, the film formed from SiO2–Al2O3–TiO2 nanoparticles has higher hydrophobic performance, i.e., the contact angle is greater than 101.7°. In addition, the TEM analysis reveals that the crystal structure of the particles can be changed at high temperatures. PMID:28774141

Ergonomic Synthesis Suitable for Industrial Production of Silver-Festooned Zinc Oxide Nanorods

NASA Astrophysics Data System (ADS)

Khan, G. R.; Khan, R. A.

2015-07-01

For maximizing productivity, minimizing cost, time-boxing process and optimizing human effort, a single-step, cost-effective, ultra-fast and environmentally benign synthesis suitable for industrial production of nanocrystalline ZnO, and Ag-doped ZnO has been reported in this paper. The synthesis based on microwave-supported aqueous solution method used zinc acetate dehydrate and silver nitrate as precursors for fabrication of nanorods. The synthesized products were characterized by X-ray diffractometry (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Raman spectroscopy and UV-Vis-NIR spectroscopy. The undoped and Ag-doped ZnO nanorods crystallized in a hexagonal wurtzite structure having spindle-like morphology. The blue shift occurred at absorption edge of Ag-doped ZnO around 260 nm compared to 365 nm of bulk ZnO. The red shift occurred at Raman peak site of 434 cm-1 compared to characteristic wurtzite phase peak of ZnO (437 cm-1). The bandgap energies were found to be 3.10 eV, 3.11 eV and 3.18 eV for undoped, 1% Ag-doped, and 3% Ag-doped ZnO samples, respectively. The TEM results provided average particle sizes of 17 nm, 15 nm and 13 nm for undoped, and 1% and 3% Ag-doped ZnO samples, respectively.

A study of Bi-Pb-Sn-Cd-Sb penta-alloys rapidly quenched from melt

NASA Astrophysics Data System (ADS)

Kamal, M.; El-Bediwi, A. B.

2004-11-01

Optical microscopy, X-ray diffractometry, the double bridge method, the Vickers microhardness testing and dynamic resonance techniques have been used to investigate structure, electrical resistivity, hardness, internal friction and elastic modulus of quenched Bi-Pb-Sn-Cd-Sb penta-alloys. The properties of these penta-alloys are greatly affected by rapid quenching. The intermetallic compound chi(Pb-Bi) or Bi3Pb7 is obtained after rapid quenching using the melt-spinning technique, and this is in agreement with reports by other authors [Marshall, T.J., Mott, G. T. and Grieverson, M. H. (1975). Br. J. Radiol., 48, 924, Kamal, M., El-Bediwi, A. B. and Karman, M. B. (1998). Structure, mechanical properties and electrical resistivity of rapidly solidified Pb-Sn-Cd and Pb-Bi-Sn-Cd alloys. J. Mater. Sci.: Mater. Electron., 9, 425, Borromee-Gautier, C., Giessen, B. C. and Grrant, N. J. (1968). J. Chem. Phys., 48,1905, Moon, K.-W., Boettinger, W. J., Kanner, U. R., Handwerker, C. A. and Lee, D.-J. (2001). The effect of Pb contamination on the solidification behavior of Sn-Bi solders. J. Electron. Mater, 30, 45.]. The quenched Bi43.5Pb44.5Cd5Sn2Sb5 alloy has important properties for safety devices in fire detection and extinguishing systems.

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

Chen Long; Department of Chemistry, Huangshan University, Huangshan 245041; Post-Doctoral Scientific Research Workstation, HuangShan NOVEL Co. Ltd, Huangshan 245061

In this paper, biomimetic synthesis of aragonite superstructures using a low molecular weight organic-hexamethylenetetramine (HMT) as an additive in the presence of CO{sub 2} supplied by an ammonium carbonate ((NH{sub 4}){sub 2}CO{sub 3}) diffusion method at room temperature was studied. The products were characterized by scanning or transmission electron microscopy, Fourier transform infrared (FT-IR) spectroscopy, X-ray powder diffractometry, and selected area electron diffraction. The results showed the aragonite superstructures especially dumbbell-flower-like ones were obtained. The formation process of calcium carbonate (CaCO{sub 3}) in HMT aqueous solution was investigated, suggesting that the products transformed from calcite to vaterite primarily, and thenmore » changed into a mixture of aragonite and calcite with an increase of reaction time. The formation mechanism of CaCO{sub 3} in HMT solution was also discussed, revealing that aragonite might be controlled by HMT molecules and NH{sub 4}{sup +} ions together. - Graphical abstract: The well-defined aragonite hierarchical superstructures are formed using hexamethylenetetramine in aqueous solution. Highlights: > Aragonite superstructures are formed with hexamethylenetetramine at about 25 deg. C. > Dumbbell-flower-like aragonite produces when hexamethylenetetramine/Ca{sup 2+}=10:1. > CaCO{sub 3} formation in hexamethylenetetramine solution violates the Ostwald ripening. > Hexamethylenetetramine and NH{sub 4}{sup +} might control the growth of aragonite together.« less

Detecting element specific electrons from a single cobalt nanocluster with synchrotron x-ray scanning tunneling microscopy

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

Kersell, Heath; Shirato, Nozomi; Cummings, Marvin

We use a nanofabricated scanning tunneling microscope tip as a detector to investigate local X-ray induced tunneling and electron emission from a single cobalt nanocluster on a Au(111) surface. The tip-detector is positioned a few angstroms above the nanocluster, and ramping the incident X-ray energy across the Co photoabsorption K-edge enables the detection of element specific electrons. Atomic-scale spatial dependent changes in the X-ray absorption cross section are directly measured by taking the X-ray induced current as a function of X-ray energy. From the measured sample and tip currents, element specific X-ray induced current components can be separated and therebymore » the corresponding yields for the X-ray induced processes of the single cobalt nanocluster can be determined. The detection of element specific synchrotron X-ray induced electrons of a single nanocluster opens a new avenue for materials characterization on a one particle at-a-time basis.« less

Detecting element specific electrons from a single cobalt nanocluster with synchrotron x-ray scanning tunneling microscopy

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

Kersell, Heath; Shirato, Nozomi; Cummings, Marvin

Here, we use a nanofabricated scanning tunneling microscope tip as a detector to investigate local X-ray induced tunneling and electron emission from a single cobalt nanocluster on a Au(111) surface. The tip-detector is positioned a few angstroms above the nanocluster, and ramping the incident X-ray energy across the Co photoabsorption K-edge enables the detection of element specific electrons. Atomic-scale spatial dependent changes in the X-ray absorption cross section are directly measured by taking the X-ray induced current as a function of X-ray energy. From the measured sample and tip currents, element specific X-ray induced current components can be separated andmore » thereby the corresponding yields for the X-ray induced processes of the single cobalt nanocluster can be determined. The detection of element specific synchrotron X-ray induced electrons of a single nanocluster opens a new avenue for materials characterization on a one particle at-a-time basis.« less

Detecting element specific electrons from a single cobalt nanocluster with synchrotron x-ray scanning tunneling microscopy

DOE PAGES

Kersell, Heath; Shirato, Nozomi; Cummings, Marvin; ...

2017-09-05

Here, we use a nanofabricated scanning tunneling microscope tip as a detector to investigate local X-ray induced tunneling and electron emission from a single cobalt nanocluster on a Au(111) surface. The tip-detector is positioned a few angstroms above the nanocluster, and ramping the incident X-ray energy across the Co photoabsorption K-edge enables the detection of element specific electrons. Atomic-scale spatial dependent changes in the X-ray absorption cross section are directly measured by taking the X-ray induced current as a function of X-ray energy. From the measured sample and tip currents, element specific X-ray induced current components can be separated andmore » thereby the corresponding yields for the X-ray induced processes of the single cobalt nanocluster can be determined. The detection of element specific synchrotron X-ray induced electrons of a single nanocluster opens a new avenue for materials characterization on a one particle at-a-time basis.« less

Polymorphism of Alprazolam (Xanax): a review of its crystalline phases and identification, crystallographic characterization, and crystal structure of a new polymorph (form III).

PubMed

de Armas, Héctor Novoa; Peeters, Oswald M; Van den Mooter, Guy; Blaton, Norbert

2007-05-01

A new polymorphic form of Alprazolam (Xanax), 8-chloro-1-methyl-6-phenyl-4H-[1,2,4]triazolo-[4,3-alpha][1,4]benzodiazepine, C(17)H(13)ClN(4), has been investigated by means of X-ray powder diffraction (XRPD), single crystal X-ray diffraction, and differential scanning calorimetry (DSC). This polymorphic form (form III) was obtained during DSC experiments after the exothermic recrystallization of the melt of form I. The crystal unit cell dimensions for form III were determined from diffractometer methods. The monoclinic unit cell found for this polymorph using XRPD after indexing the powder diffractogram was confirmed by the cell parameters obtained from single crystal X-ray diffractometry on a crystal isolated from the DSC pans. The single crystal unit cell parameters are: a = 28.929(9), b = 13.844(8), c = 7.361(3) angstroms, beta = 92.82(3) degrees , V = 2944(2) angstroms(3), Z = 8, space group P2(1) (No.4), Dx = 1.393 Mg/m(3). The structure obtained from single crystal X-ray diffraction was used as initial model for Rietveld refinement on the powder diffraction data of form III. The temperature phase transformations of alprazolam were also studied using high temperature XRPD. A review of the different phases available in the Powder Diffraction File (PDF) database for this drug is described bringing some clarification and corrections. (c) 2007 Wiley-Liss, Inc. and the American Pharmacists Association.

An epistemology on the nature of polymers.

PubMed

Laridjani, Mortéza; Leboucher, Pierre

2014-01-01

Liquids have neither a periodic structure nor the completely random character of gases therefore the detailed study of their x-ray scattering diagram encounters many difficulties. The idea of periodic regularity in molecules of liquid polymers has been an attractive proposition for the simple interpretation of liquid polymer x-ray diagrams. The categorisation of polymer substances as being between a crystal phase with a perfect order and an amorphous disordered state is an over simplification of the complex reality. For obtaining structural information, during the early stages of the application of x-ray diffraction, a near crystalline model of the molecular arrangements in liquids was utilised. However, the results from these investigations led to just an approximation of the crystalline state. Our studies have analysed the real image of Fourier space of liquid polymers, for the first time, using anomalous diffractometry. The findings show the precise atomic structure of liquid polymers when transformed, by cooling, to solid polymers. We demonstrate that there is an intermediate ordered structure, characterised by the real full image of Fourier space. This prominent state of matter, an intermediate ordered structure, is defined by a regular unit cell with a five-fold symmetry. These structural atomic studies contribute to a more detailed understanding of the properties of polymers than the traditional studies of the degree of crystallinity.

An Epistemology on the Nature of Polymers

PubMed Central

Laridjani, Mortéza; Leboucher, Pierre

2014-01-01

Liquids have neither a periodic structure nor the completely random character of gases therefore the detailed study of their x-ray scattering diagram encounters many difficulties. The idea of periodic regularity in molecules of liquid polymers has been an attractive proposition for the simple interpretation of liquid polymer x-ray diagrams. The categorisation of polymer substances as being between a crystal phase with a perfect order and an amorphous disordered state is an over simplification of the complex reality. For obtaining structural information, during the early stages of the application of x-ray diffraction, a near crystalline model of the molecular arrangements in liquids was utilised. However, the results from these investigations led to just an approximation of the crystalline state. Our studies have analysed the real image of Fourier space of liquid polymers, for the first time, using anomalous diffractometry. The findings show the precise atomic structure of liquid polymers when transformed, by cooling, to solid polymers. We demonstrate that there is an intermediate ordered structure, characterised by the real full image of Fourier space. This prominent state of matter, an intermediate ordered structure, is defined by a regular unit cell with a five-fold symmetry. These structural atomic studies contribute to a more detailed understanding of the properties of polymers than the traditional studies of the degree of crystallinity. PMID:25329440

Complete p-type activation in vertical-gradient freeze GaAs co-implanted with gallium and carbon

NASA Astrophysics Data System (ADS)

Horng, S. T.; Goorsky, M. S.

1996-03-01

High-resolution triple-axis x-ray diffractometry and Hall-effect measurements were used to characterize damage evolution and electrical activation in gallium arsenide co-implanted with gallium and carbon ions. Complete p-type activation of GaAs co-implanted with 5×1014 Ga cm-2 and 5×1014 C cm-2 was achieved after rapid thermal annealing at 1100 °C for 10 s. X-ray diffuse scattering was found to increase after rapid thermal annealing at 600-900 °C due to the aggregation of implantation-induced point defects. In this annealing range, there was ˜10%-72% activation. After annealing at higher annealing temperatures, the diffuse scattered intensity decreased drastically; samples that had been annealed at 1000 °C (80% activated) and 1100 °C (˜100% activated) exhibited reciprocal space maps that were indicative of high crystallinity. The hole mobility was about 60 cm2/V s for all samples annealed at 800 °C and above, indicating that the crystal perfection influences dopant activation more strongly than it influences mobility. Since the high-temperature annealing simultaneously increases dopant activation and reduces x-ray diffuse scattering, we conclude that point defect complexes which form at lower annealing temperatures are responsible for both the diffuse scatter and the reduced activation.

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

Alves, L. M. S., E-mail: leandro-fisico@hotmail.com; Lima, B. S. de; Santos, C. A. M. dos

K{sub 0.05}MoO{sub 2} has been studied by x-ray and neutron diffractometry, electrical resistivity, magnetization, heat capacity, and thermal expansion measurements. The compound displays two phase transitions, a first-order phase transition near room temperature and a second-order transition near 54 K. Below the transition at 54 K, a weak magnetic anomaly is observed and the electrical resistivity is well described by a power-law temperature dependence with exponent near 0.5. The phase transitions in the K-doped MoO{sub 2} compound have been discussed for the first time using neutron diffraction, high resolution thermal expansion, and heat capacity measurements as a function of temperature.

Effect of thermal history on Mossbauer signature and hyperfine interaction parameters of copper ferrite

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

Modi, K. B., E-mail: kunalbmodi2003@yahoo.com; Raval, P. Y.; Dulera, S. V.

Two specimens of copper ferrite, CuFe{sub 2}O{sub 4}, have been synthesized by double sintering ceramic technique with different thermal history i.e. slow cooled and quenched. X-ray diffractometry has confirmed single phase fcc spinel structure for slow cooled sample while tetragonal distortion is present in quenched sample. Mossbauer spectral analysis for slow-cooled copper ferrite reveals super position of two Zeeman split sextets along with paramagnetic singlet in the centre position corresponds to delafossite (CuFeO{sub 2}) phase that is completely absent in quenched sample. The hyperfine interaction parameters are highly influenced by heat treatment employed.

The polymorphic and mesomorphic behavior of four esters of cholesterol.

NASA Technical Reports Server (NTRS)

Merritt, W. G.; Cole, G. D.; Walker, W. W.

1971-01-01

The techniques of differential scanning calorimetry, X-ray powder diffractometry, and positron annihilation have been used to study the polymorphic and mesomorphic behavior of the following esters of cholesterol: cholesteryl formate, cholesteryl butyrate, cholesteryl benzoate, and cholesteryl cinnamate. Each of these compounds exhibits a single mesophase of the cholesteric type. The solid phase formed from the melt for each ester was observed to be structurally different from the solid phase obtained from solution. Solvents from which the solution-grown samples were crystallized were as follows: cholesteryl formate and cholesteryl butyrate from acetone, cholesteryl benzoate from benzene, and cholesteryl cinnamate from 2-butanone.

Characterization and mechanical properties investigation of TiN-Ag films onto Ti-6Al-4V

NASA Astrophysics Data System (ADS)

Du, Dongxing; Liu, Daoxin; Zhang, Xiaohua; Tang, Jingang; Xiang, Dinggen

2016-03-01

To investigate their effect on fretting fatigue (FF) resistance of a Ti-6Al-4V alloy, hard solid lubricating composite films of TiN with varying silver contents (TiN-Ag) were deposited on a Ti-6Al-4V alloy using ion-assisted magnetron sputtering. The surface morphology and structure were analyzed by atomic force microscopy, X-ray diffractometry, X-ray photoelectron spectroscopy, and transmission electron microscopy. The hardness, bonding strength, and toughness of films were tested using a micro-hardness tester, scratch tester, and a repeated press-press test system that was manufactured in-house, respectively. The FF resistance of TiN-Ag composite films was studied using self-developed devices. The results show that the FF resistance of a titanium alloy can be improved by TiN-Ag composite films, which were fabricated using hard TiN coating doped with soft Ag. The FF life of Ag0.5, Ag2, Ag5, Ag10 and Ag20 composite films is 2.41, 3.18, 3.20, 2.94 and 2.87 times as great as that of the titanium alloy, respectively. This is because the composite films have the better toughness, friction lubrication, and high bonding strength. When the atomic fraction of Ag changes from 2% to 5%, the FF resistance of the composite films shows the best performance. This is attributed to the surface integrity of the composite film is sufficiently fine to prevent the initiation and early propagation of FF cracks.

[The "silica" component in the PM10 of an urban site].

PubMed

De Berardis, Barbara; Incocciati, Emma; Massera, S; Gargaro, G; Paoletti, L

2007-01-01

In vivo and in vitro toxicological studies have shown that the aged fracturated crystalline silica, which is a component of airborne particulate, exerts an important inflammatory action on airways. The evaluation of the concentration level of airborne crystalline silica in an urban area is an important research subject in order to determine the exposure levels of the general population. The aim was to study the seasonal trend of the quartz (the most common form of crystalline silica) concentration levels in the particulate inhalable faction (PM10) in the urban area of Rome. PM10, sampled by a cascade impactor, was analysed by scanning electron microscopy, equipped with a thin-window system for X-ray microanalysis (SEM/EDX) for qualitative analysis. Parallely the concentration levels of quartz in the particulate were determined by X-ray diffractometry (XRD) for quantitative analysis, using the NIOSH 7500 method (NIOSH, 1994). From September 2004 to October 2005 the abundance of silica particles, evaluated by SEM/EDX was in the range 1.6/10.4%, with a concentration level of free crystalline silica in the range 0.25/2.87 microg/mi. The equivalent diameter of silica particles ranged from 0.3 to 10.5 mircom, moreover, more than 87% of particles showed a diameter less than 2.5 microm. The correlations between SEM/EDX and XRD data seem to suggest that the airborne silica particles in the urban location studied consisted mostly of crystalline silica. Moreover, the data suggest the existence of a significant contribution of silica particles due to southwest wind carrying a fine dust from the Sahara desert to Mediterranean Europe.

THz-pump and X-ray-probe sources based on an electron linac

NASA Astrophysics Data System (ADS)

Setiniyaz, Sadiq; Park, Seong Hee; Kim, Hyun Woo; Vinokurov, Nikolay A.; Jang, Kyu-Ha; Lee, Kitae; Baek, In Hyung; Jeong, Young Uk

2017-11-01

We describe a compact THz-pump and X-ray-probe beamline, based on an electron linac, for ultrafast time-resolved diffraction applications. Two high-energy electron (γ > 50) bunches, 5 ns apart, impinge upon a single-foil or multifoil radiator and generate THz radiation and X-rays simultaneously. The THz pulse from the first bunch is synchronized to the X-ray beam of the second bunch by using an adjustable optical delay of a THz pulse. The peak power of THz radiation from the multifoil radiator is estimated to be 0.14 GW for a 200 pC well-optimized electron bunch. GEANT4 simulations show that a carbon foil with a thickness of 0.5-1.0 mm has the highest yield of 10-20 keV hard X-rays for a 25 MeV beam, which is approximately 103 photons/(keV pC-electrons) within a few degrees of the polar angle. A carbon multifoil radiator with 35 foils (25 μm thick each) can generate close to 103 hard X-rays/(keV pC-electrons) within a 2° acceptance angle. With 200 pC charge and a 100 Hz repetition rate, we can generate 107 X-rays per 1 keV energy bin per second or 105 X-rays per 1 keV energy bin per pulse. The longitudinal time profile of an X-ray pulse ranges from 400 to 600 fs depending on the acceptance angle. The broadening of the time duration of an X-ray pulse is observed owing to its diverging effect. A double-crystal monochromator will be used to select and transport the desired X-rays to the sample. The heating of the radiators by an electron beam is negligible because of the low beam current.

Miniature, low-power X-ray tube using a microchannel electron generator electron source

NASA Technical Reports Server (NTRS)

Elam, Wm. Timothy (Inventor); Kelliher, Warren C. (Inventor); Hershyn, William (Inventor); DeLong, David P. (Inventor)

2011-01-01

Embodiments of the invention provide a novel, low-power X-ray tube and X-ray generating system. Embodiments of the invention use a multichannel electron generator as the electron source, thereby increasing reliability and decreasing power consumption of the X-ray tube. Unlike tubes using a conventional filament that must be heated by a current power source, embodiments of the invention require only a voltage power source, use very little current, and have no cooling requirements. The microchannel electron generator comprises one or more microchannel plates (MCPs), Each MCP comprises a honeycomb assembly of a plurality of annular components, which may be stacked to increase electron intensity. The multichannel electron generator used enables directional control of electron flow. In addition, the multichannel electron generator used is more robust than conventional filaments, making the resulting X-ray tube very shock and vibration resistant.

Ultrafast Science Opportunities with Electron Microscopy

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

Durr, Hermann

X-rays and electrons are two of the most fundamental probes of matter. When the Linac Coherent Light Source (LCLS), the world’s first x-ray free electron laser, began operation in 2009, it transformed ultrafast science with the ability to generate laser-like x-ray pulses from the manipulation of relativistic electron beams. This document describes a similar future transformation. In Transmission Electron Microscopy, ultrafast relativistic (MeV energy) electron pulses can achieve unsurpassed spatial and temporal resolution. Ultrafast temporal resolution will be the next frontier in electron microscopy and can ideally complement ultrafast x-ray science done with free electron lasers. This document describes themore » Grand Challenge science opportunities in chemistry, material science, physics and biology that arise from an MeV ultrafast electron diffraction & microscopy facility, especially when coupled with linac-based intense THz and X-ray pump capabilities.« less

Compton spectra of atoms at high x-ray intensity

NASA Astrophysics Data System (ADS)

Son, Sang-Kil; Geffert, Otfried; Santra, Robin

2017-03-01

Compton scattering is the nonresonant inelastic scattering of an x-ray photon by an electron and has been used to probe the electron momentum distribution in gas-phase and condensed-matter samples. In the low x-ray intensity regime, Compton scattering from atoms dominantly comes from bound electrons in neutral atoms, neglecting contributions from bound electrons in ions and free (ionized) electrons. In contrast, in the high x-ray intensity regime, the sample experiences severe ionization via x-ray multiphoton multiple ionization dynamics. Thus, it becomes necessary to take into account all the contributions to the Compton scattering signal when atoms are exposed to high-intensity x-ray pulses provided by x-ray free-electron lasers (XFELs). In this paper, we investigate the Compton spectra of atoms at high x-ray intensity, using an extension of the integrated x-ray atomic physics toolkit, xatom. As the x-ray fluence increases, there is a significant contribution from ionized electrons to the Compton spectra, which gives rise to strong deviations from the Compton spectra of neutral atoms. The present study provides not only understanding of the fundamental XFEL-matter interaction but also crucial information for single-particle imaging experiments, where Compton scattering is no longer negligible. , which features invited work from the best early-career researchers working within the scope of J. Phys. B. This project is part of the Journal of Physics series’ 50th anniversary celebrations in 2017. Sang-Kil Son was selected by the Editorial Board of J. Phys. B as an Emerging Leader.

RF Phase Stability and Electron Beam Characterization for the PLEIADES Thomson X-Ray Source

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

Brown, W J; Hartemann, F V; Tremaine, A M

2002-10-16

We report on the performance of an S-band RF photocathode electron gun and accelerator for operation with the PLEIADES Thomson x-ray source at LLNL. To produce picosecond, high brightness x-ray pulses, picosecond timing, terahertz bandwidth diagnostics, and RF phase control are required. Planned optical, RF, x-ray and electron beam measurements to characterize the dependence of electron beam parameters and synchronization on RF phase stability are presented.

Millimeter, microwave, hard X-ray, and soft X-ray observations of energetic electron populations in solar flares

NASA Technical Reports Server (NTRS)

Kundu, M. R.; White, S. M.; Gopalswamy, N.; Lim, J.

1994-01-01

We present comparisons of multiwavelength data for a number of solar flares observed during the major campaign of 1991 June. The different wavelengths are diagnostics of energetic electrons in different energy ranges: soft X-rays are produced by electrons with energies typically below 10 keV, hard X-rays by electrons with energies in the range 10-200 keV, microwaves by electrons in the range 100 keV-1 MeV, and millimeter-wavelength emission by electrons with energies of 0.5 MeV and above. The flares in the 1991 June active period were remarkable in two ways: all have very high turnover frequencies in their microwave spectra, and very soft hard X-ray spectra. The sensitivity of the microwave and millimeter data permit us to study the more energetic (greater than 0.3 MeV) electrons even in small flares, where their high-energy bremsstrahlung is too weak for present detectors. The millimeter data show delays in the onset of emission with respect to the emissions associated with lower energy electrons and differences in time profiles, energy spectral indices incompatible with those implied by the hard X-ray data, and a range of variability of the peak flux in the impulsive phase when compared with the peak hard X-ray flux which is two orders of magnitude larger than the corresponding variability in the peak microwave flux. All these results suggest that the hard X-ray-emitting electrons and those at higher energies which produce millimeter emission must be regarded as separate populations. This has implications for the well-known 'number problem' found previously when comparing the numbers of non thermal electrons required to produce the hard X-ray and radio emissions.

Femtosecond profiling of shaped x-ray pulses

NASA Astrophysics Data System (ADS)

Hoffmann, M. C.; Grguraš, I.; Behrens, C.; Bostedt, C.; Bozek, J.; Bromberger, H.; Coffee, R.; Costello, J. T.; DiMauro, L. F.; Ding, Y.; Doumy, G.; Helml, W.; Ilchen, M.; Kienberger, R.; Lee, S.; Maier, A. R.; Mazza, T.; Meyer, M.; Messerschmidt, M.; Schorb, S.; Schweinberger, W.; Zhang, K.; Cavalieri, A. L.

2018-03-01

Arbitrary manipulation of the temporal and spectral properties of x-ray pulses at free-electron lasers would revolutionize many experimental applications. At the Linac Coherent Light Source at Stanford National Accelerator Laboratory, the momentum phase-space of the free-electron laser driving electron bunch can be tuned to emit a pair of x-ray pulses with independently variable photon energy and femtosecond delay. However, while accelerator parameters can easily be adjusted to tune the electron bunch phase-space, the final impact of these actuators on the x-ray pulse cannot be predicted with sufficient precision. Furthermore, shot-to-shot instabilities that distort the pulse shape unpredictably cannot be fully suppressed. Therefore, the ability to directly characterize the x-rays is essential to ensure precise and consistent control. In this work, we have generated x-ray pulse pairs via electron bunch shaping and characterized them on a single-shot basis with femtosecond resolution through time-resolved photoelectron streaking spectroscopy. This achievement completes an important step toward future x-ray pulse shaping techniques.

High-intensity double-pulse X-ray free-electron laser

DOE PAGES

Marinelli, A.; Ratner, D.; Lutman, A. A.; ...

2015-03-06

The X-ray free-electron laser has opened a new era for photon science, improving the X-ray brightness by ten orders of magnitude over previously available sources. Similar to an optical laser, the spectral and temporal structure of the radiation pulses can be tailored to the specific needs of many experiments by accurately manipulating the lasing medium, that is, the electron beam. Here we report the generation of mJ-level two-colour hard X-ray pulses of few femtoseconds duration with an XFEL driven by twin electron bunches at the Linac Coherent Light Source. This performance represents an improvement of over an order of magnitudemore » in peak power over state-of-the-art two-colour XFELs. The unprecedented intensity and temporal coherence of this new two-colour X-ray free-electron laser enable an entirely new set of scientific applications, ranging from X-ray pump/X-ray probe experiments to the imaging of complex biological samples with multiple wavelength anomalous dispersion.« less

Compton backscattered collimated x-ray source

DOEpatents

Ruth, R.D.; Huang, Z.

1998-10-20

A high-intensity, inexpensive and collimated x-ray source is disclosed for applications such as x-ray lithography is disclosed. An intense pulse from a high power laser, stored in a high-finesse resonator, repetitively collides nearly head-on with and Compton backscatters off a bunched electron beam, having relatively low energy and circulating in a compact storage ring. Both the laser and the electron beams are tightly focused and matched at the interaction region inside the optical resonator. The laser-electron interaction not only gives rise to x-rays at the desired wavelength, but also cools and stabilizes the electrons against intrabeam scattering and Coulomb repulsion with each other in the storage ring. This cooling provides a compact, intense bunch of electrons suitable for many applications. In particular, a sufficient amount of x-rays can be generated by this device to make it an excellent and flexible Compton backscattered x-ray (CBX) source for high throughput x-ray lithography and many other applications. 4 figs.

Compton backscattered collimated x-ray source

DOEpatents

Ruth, Ronald D.; Huang, Zhirong

1998-01-01

A high-intensity, inexpensive and collimated x-ray source for applications such as x-ray lithography is disclosed. An intense pulse from a high power laser, stored in a high-finesse resonator, repetitively collides nearly head-on with and Compton backscatters off a bunched electron beam, having relatively low energy and circulating in a compact storage ring. Both the laser and the electron beams are tightly focused and matched at the interaction region inside the optical resonator. The laser-electron interaction not only gives rise to x-rays at the desired wavelength, but also cools and stabilizes the electrons against intrabeam scattering and Coulomb repulsion with each other in the storage ring. This cooling provides a compact, intense bunch of electrons suitable for many applications. In particular, a sufficient amount of x-rays can be generated by this device to make it an excellent and flexible Compton backscattered x-ray (CBX) source for high throughput x-ray lithography and many other applications.

Compton backscattered collmated X-ray source

DOEpatents

Ruth, Ronald D.; Huang, Zhirong

2000-01-01

A high-intensity, inexpensive and collimated x-ray source for applications such as x-ray lithography is disclosed. An intense pulse from a high power laser, stored in a high-finesse resonator, repetitively collides nearly head-on with and Compton backscatters off a bunched electron beam, having relatively low energy and circulating in a compact storage ring. Both the laser and the electron beams are tightly focused and matched at the interaction region inside the optical resonator. The laser-electron interaction not only gives rise to x-rays at the desired wavelength, but also cools and stabilizes the electrons against intrabeam scattering and Coulomb repulsion with each other in the storage ring. This cooling provides a compact, intense bunch of electrons suitable for many applications. In particular, a sufficient amount of x-rays can be generated by this device to make it an excellent and flexible Compton backscattered x-ray (CBX) source for high throughput x-ray lithography and many other applications.

In Situ Identification of Mineral Resources with an X-Ray-Optical "Hands-Lens" Instrument

NASA Technical Reports Server (NTRS)

Marshall, J.; Koppel, L.; Bratton, C.; Metzger, E.; Hecht, M.

1999-01-01

The recognition of material resources on a planetary surface requires exploration strategies not dissimilar to those employed by early field geologists who searched for ore deposits primarily from surface clues. In order to determine the location of mineral ores or other materials, it will be necessary to characterize host terranes at regional or subregional scales. This requires geographically broad surveys in which statistically significant numbers of samples are rapidly scanned from a roving platform. To enable broad-scale, yet power-conservative planetary-surface exploration, we are developing an instrument that combines x-ray diffractometry (XRD), x-ray fluorescence spectrometry (XRF), and optical capabilities; the instrument can be deployed at the end of a rover's robotic arm, without the need for sample capture or preparation. The instrument provides XRD data for identification of mineral species and lithological types; diffractometry of minerals is conducted by ascertaining the characteristic lattice parameters or "d-spacings" of mineral compounds. D-spacings of 1.4 to 25 angstroms can be determined to include the large molecular structures of hydrated minerals such as clays. The XRF data will identify elements ranging from carbon (Atomic Number = 6) to elements as heavy as barium (Atomic Number = 56). While a sample is being x-rayed, the instrument simultaneously acquires an optical image of the sample surface at magnifications from lx to at least 50x (200x being feasible, depending on the sample surface). We believe that imaging the sample is extremely important as corroborative sample-identification data (the need for this capability having been illustrated by the experience of the Pathfinder rover). Very few geologists would rely on instrument data for sample identification without having seen the sample. Visual inspection provides critical recognition data such as texture, crystallinity, granularity, porosity, vesicularity, color, lustre, opacity, and so forth. These data can immediately distinguish sedimentary from igneous rocks, for example, and can thus eliminate geochemical or mineral ambiguities arising, say between arkose and granite. It would be important to know if the clay being analyzed was part of a uniform varve deposit laid down in a quiescent lake, or the matrix of a megabreccia diamictite deposited as a catastrophic impact ejecta blanket. The unique design of the instrument, which combines Debye-Scherrer geometry with elements of standard goniometry, negates the need for sample preparation of any kind, and thus negates the need for power-hungry and mechanically-complex sampling systems that would have to chip, crush, sieve, and mount the sample for x-ray analysis. Instead, the instrument is simply rested on the sample surface of interest (like a hand lens); the device can interrogate rough rock surfaces, coarse granular material, or fine rock flour. A breadboard version of the instrument has been deployed from the robotic arm of the Marsokhod rover in field trials at NASA Ames, where large vesicular boulders were x-rayed to demonstrate the functionality of the instrument design, and the ability of such a device to comply with constraints imposed by a roving platform. Currently under development is a flight prototype concept of this instrument that will weigh 0.3 kg, using about 4500 J of energy per sample analysis. It requires about 5 min. for XRD analysis, and about 30 min. for XRF interrogation. Its small mass and rugged design make it ideal for deployment on small rovers of the type currently envisaged for the exploration of Mars (e.g., Sojourner-scale platforms). The design utilizes a monolithic P-N junction photodiode pixel array for XRD, a Si PIN photodiode/avalanche photodiode system for XRF, and an endoscopic imaging camera system unobtrusively embedded between the detectors and the x-ray source (the endoscope with its board-mounted camera can be adapted for IR light in addition to visible wavelenths. A rugged, miniature (7 cu cm) x-ray source for the instrument has already been breadboarded.

In Situ Identification of Mineral Resources with an X-Ray-Optical "Hands-Lens" Instrument

NASA Astrophysics Data System (ADS)

Marshall, J.; Koppel, L.; Bratton, C.; Metzger, E.; Hecht, M.

1999-09-01

The recognition of material resources on a planetary surface requires exploration strategies not dissimilar to those employed by early field geologists who searched for ore deposits primarily from surface clues. In order to determine the location of mineral ores or other materials, it will be necessary to characterize host terranes at regional or subregional scales. This requires geographically broad surveys in which statistically significant numbers of samples are rapidly scanned from a roving platform. To enable broad-scale, yet power-conservative planetary-surface exploration, we are developing an instrument that combines x-ray diffractometry (XRD), x-ray fluorescence spectrometry (XRF), and optical capabilities; the instrument can be deployed at the end of a rover's robotic arm, without the need for sample capture or preparation. The instrument provides XRD data for identification of mineral species and lithological types; diffractometry of minerals is conducted by ascertaining the characteristic lattice parameters or "d-spacings" of mineral compounds. D-spacings of 1.4 to 25 angstroms can be determined to include the large molecular structures of hydrated minerals such as clays. The XRF data will identify elements ranging from carbon (Atomic Number = 6) to elements as heavy as barium (Atomic Number = 56). While a sample is being x-rayed, the instrument simultaneously acquires an optical image of the sample surface at magnifications from lx to at least 50x (200x being feasible, depending on the sample surface). We believe that imaging the sample is extremely important as corroborative sample-identification data (the need for this capability having been illustrated by the experience of the Pathfinder rover). Very few geologists would rely on instrument data for sample identification without having seen the sample. Visual inspection provides critical recognition data such as texture, crystallinity, granularity, porosity, vesicularity, color, lustre, opacity, and so forth. These data can immediately distinguish sedimentary from igneous rocks, for example, and can thus eliminate geochemical or mineral ambiguities arising, say between arkose and granite. It would be important to know if the clay being analyzed was part of a uniform varve deposit laid down in a quiescent lake, or the matrix of a megabreccia diamictite deposited as a catastrophic impact ejecta blanket. The unique design of the instrument, which combines Debye-Scherrer geometry with elements of standard goniometry, negates the need for sample preparation of any kind, and thus negates the need for power-hungry and mechanically-complex sampling systems that would have to chip, crush, sieve, and mount the sample for x-ray analysis. Instead, the instrument is simply rested on the sample surface of interest (like a hand lens); the device can interrogate rough rock surfaces, coarse granular material, or fine rock flour. A breadboard version of the instrument has been deployed from the robotic arm of the Marsokhod rover in field trials at NASA Ames, where large vesicular boulders were x-rayed to demonstrate the functionality of the instrument design, and the ability of such a device to comply with constraints imposed by a roving platform. Currently under development is a flight prototype concept of this instrument that will weigh 0.3 kg, using about 4500 J of energy per sample analysis. It requires about 5 min. for XRD analysis, and about 30 min. for XRF interrogation. Its small mass and rugged design make it ideal for deployment on small rovers of the type currently envisaged for the exploration of Mars (e.g., Sojourner-scale platforms). The design utilizes a monolithic P-N junction photodiode pixel array for XRD, a Si PIN photodiode/avalanche photodiode system for XRF, and an endoscopic imaging camera system unobtrusively embedded between the detectors and the x-ray source (the endoscope with its board-mounted camera can be adapted for IR light in addition to visible wavelenths. A rugged, miniature (7 cu cm) x-ray source for the instrument has already been breadboarded.

Generation of first hard X-ray pulse at Tsinghua Thomson Scattering X-ray Source.

PubMed

Du, Yingchao; Yan, Lixin; Hua, Jianfei; Du, Qiang; Zhang, Zhen; Li, Renkai; Qian, Houjun; Huang, Wenhui; Chen, Huaibi; Tang, Chuanxiang

2013-05-01

Tsinghua Thomson Scattering X-ray Source (TTX) is the first-of-its-kind dedicated hard X-ray source in China based on the Thomson scattering between a terawatt ultrashort laser and relativistic electron beams. In this paper, we report the experimental generation and characterization of the first hard X-ray pulses (51.7 keV) via head-on collision of an 800 nm laser and 46.7 MeV electron beams. The measured yield is 1.0 × 10(6) per pulse with an electron bunch charge of 200 pC and laser pulse energy of 300 mJ. The angular intensity distribution and energy spectra of the X-ray pulse are measured with an electron-multiplying charge-coupled device using a CsI scintillator and silicon attenuators. These measurements agree well with theoretical and simulation predictions. An imaging test using the X-ray pulse at the TTX is also presented.

Nonlinear X-Ray and Auger Spectroscopy at X-Ray Free-Electron Laser Sources

NASA Astrophysics Data System (ADS)

Rohringer, Nina

2015-05-01

X-ray free-electron lasers (XFELs) open the pathway to transfer non-linear spectroscopic techniques to the x-ray domain. A promising all x-ray pump probe technique is based on coherent stimulated electronic x-ray Raman scattering, which was recently demonstrated in atomic neon. By tuning the XFEL pulse to core-excited resonances, a few seed photons in the spectral tail of the XFEL pulse drive an avalanche of resonant inelastic x-ray scattering events, resulting in exponential amplification of the scattering signal by of 6-7 orders of magnitude. Analysis of the line profile of the emitted radiation permits to demonstrate the cross over from amplified spontaneous emission to coherent stimulated resonance scattering. In combination with statistical covariance mapping, a high-resolution spectrum of the resonant inelastic scattering process can be obtained, opening the path to coherent stimulated x-ray Raman spectroscopy. An extension of these ideas to molecules and a realistic feasibility study of stimulated electronic x-ray Raman scattering in CO will be presented. Challenges to realizing stimulated electronic x-ray Raman scattering at present-day XFEL sources will be discussed, corroborated by results of a recent experiment at the LCLS XFEL. Due to the small gain cross section in molecular targets, other nonlinear spectroscopic techniques such as nonlinear Auger spectroscopy could become a powerful alternative. Theory predictions of a novel pump probe technique based on resonant nonlinear Auger spectroscopic will be discussed and the method will be compared to stimulated x-ray Raman spectroscopy.

X-Ray Sum Frequency Diffraction for Direct Imaging of Ultrafast Electron Dynamics

NASA Astrophysics Data System (ADS)

Rouxel, Jérémy R.; Kowalewski, Markus; Bennett, Kochise; Mukamel, Shaul

2018-06-01

X-ray diffraction from molecules in the ground state produces an image of their charge density, and time-resolved x-ray diffraction can thus monitor the motion of the nuclei. However, the density change of excited valence electrons upon optical excitation can barely be monitored with regular diffraction techniques due to the overwhelming background contribution of the core electrons. We present a nonlinear x-ray technique made possible by novel free electron laser sources, which provides a spatial electron density image of valence electron excitations. The technique, sum frequency generation carried out with a visible pump and a broadband x-ray diffraction pulse, yields snapshots of the transition charge densities, which represent the electron density variations upon optical excitation. The technique is illustrated by ab initio simulations of transition charge density imaging for the optically induced electronic dynamics in a donor or acceptor substituted stilbene.

Seeing Atoms and Molecules in Action with an Electron 'Eye' | Berkeley Lab

Science.gov Websites

, also called "electron guns," that can drive advanced X-ray lasers known as "free form of X-ray light. Free-electron lasers have opened new frontiers in studying materials and chemistry that you can look at with an X-ray free-electron laser, but with an electron eye." He added, "

X-ray tube with magnetic electron steering

DOEpatents

Reed, Kim W.; Turman, Bobby N.; Kaye, Ronald J.; Schneider, Larry X.

2000-01-01

An X-ray tube uses a magnetic field to steer electrons. The magnetic field urges electrons toward the anode, increasing the proportion of electrons emitted from the cathode that reach desired portions of the anode and consequently contribute to X-ray production. The magnetic field also urges electrons reflected from the anode back to the anode, further increasing the efficiency of the tube.

High-pressure studies with x-rays using diamond anvil cells

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

Shen, Guoyin; Mao, Ho Kwang

2016-11-22

Pressure profoundly alters all states of matter. The symbiotic development of ultrahigh-pressure diamond anvil cells, to compress samples to sustainable multi-megabar pressures; and synchrotron x-ray techniques, to probe materials' properties in situ, has enabled the exploration of rich high-pressure (HP) science. In this article, we first introduce the essential concept of diamond anvil cell technology, together with recent developments and its integration with other extreme environments. We then provide an overview of the latest developments in HP synchrotron techniques, their applications, and current problems, followed by a discussion of HP scientific studies using x-rays in the key multidisciplinary fields. Thesemore » HP studies include: HP x-ray emission spectroscopy, which provides information on the filled electronic states of HP samples; HP x-ray Raman spectroscopy, which probes the HP chemical bonding changes of light elements; HP electronic inelastic x-ray scattering spectroscopy, which accesses high energy electronic phenomena, including electronic band structure, Fermi surface, excitons, plasmons, and their dispersions; HP resonant inelastic x-ray scattering spectroscopy, which probes shallow core excitations, multiplet structures, and spin-resolved electronic structure; HP nuclear resonant x-ray spectroscopy, which provides phonon densities of state and time-resolved Mössbauer information; HP x-ray imaging, which provides information on hierarchical structures, dynamic processes, and internal strains; HP x-ray diffraction, which determines the fundamental structures and densities of single-crystal, polycrystalline, nanocrystalline, and non-crystalline materials; and HP radial x-ray diffraction, which yields deviatoric, elastic and rheological information. Integrating these tools with hydrostatic or uniaxial pressure media, laser and resistive heating, and cryogenic cooling, has enabled investigations of the structural, vibrational, electronic, and magnetic properties of materials over a wide range of pressure-temperature conditions.« less

High-pressure studies with x-rays using diamond anvil cells

NASA Astrophysics Data System (ADS)

Shen, Guoyin; Mao, Ho Kwang

2017-01-01

Pressure profoundly alters all states of matter. The symbiotic development of ultrahigh-pressure diamond anvil cells, to compress samples to sustainable multi-megabar pressures; and synchrotron x-ray techniques, to probe materials’ properties in situ, has enabled the exploration of rich high-pressure (HP) science. In this article, we first introduce the essential concept of diamond anvil cell technology, together with recent developments and its integration with other extreme environments. We then provide an overview of the latest developments in HP synchrotron techniques, their applications, and current problems, followed by a discussion of HP scientific studies using x-rays in the key multidisciplinary fields. These HP studies include: HP x-ray emission spectroscopy, which provides information on the filled electronic states of HP samples; HP x-ray Raman spectroscopy, which probes the HP chemical bonding changes of light elements; HP electronic inelastic x-ray scattering spectroscopy, which accesses high energy electronic phenomena, including electronic band structure, Fermi surface, excitons, plasmons, and their dispersions; HP resonant inelastic x-ray scattering spectroscopy, which probes shallow core excitations, multiplet structures, and spin-resolved electronic structure; HP nuclear resonant x-ray spectroscopy, which provides phonon densities of state and time-resolved Mössbauer information; HP x-ray imaging, which provides information on hierarchical structures, dynamic processes, and internal strains; HP x-ray diffraction, which determines the fundamental structures and densities of single-crystal, polycrystalline, nanocrystalline, and non-crystalline materials; and HP radial x-ray diffraction, which yields deviatoric, elastic and rheological information. Integrating these tools with hydrostatic or uniaxial pressure media, laser and resistive heating, and cryogenic cooling, has enabled investigations of the structural, vibrational, electronic, and magnetic properties of materials over a wide range of pressure-temperature conditions.

Miniaturized, High-Speed, Modulated X-Ray Source

NASA Technical Reports Server (NTRS)

Gendreau, Keith; Arzoumanian, Zaven; Kenyon, Steve; Spartana, Nick

2013-01-01

A low-cost, miniature x-ray source has been developed that can be modulated in intensity from completely off to full intensity on nanosecond timescales. This modulated x-ray source (MXS) has no filaments and is extremely rugged. The energy level of the MXS is adjustable from 0 to more than 100 keV. It can be used as the core of many new devices, providing the first practical, arbitrarily time-variable source of x-rays. The high-speed switching capability and miniature size make possible many new technologies including x-ray-based communication, compact time-resolved x-ray diffraction, novel x-ray fluorescence instruments, and low- and precise-dose medical x-rays. To make x-rays, the usual method is to accelerate electrons into a target material held at a high potential. When the electrons stop in the target, x-rays are produced with a spectrum that is a function of the target material and the energy to which the electrons are accelerated. Most commonly, the electrons come from a hot filament. In the MXS, the electrons start off as optically driven photoelectrons. The modulation of the x-rays is then tied to the modulation of the light that drives the photoelectron source. Much of the recent development has consisted of creating a photoelectrically-driven electron source that is robust, low in cost, and offers high intensity. For robustness, metal photocathodes were adopted, including aluminum and magnesium. Ultraviolet light from 255- to 350-nm LEDs (light emitting diodes) stimulated the photoemissions from these photocathodes with an efficiency that is maximized at the low-wavelength end (255 nm) to a value of roughly 10(exp -4). The MXS units now have much higher brightness, are much smaller, and are made using a number of commercially available components, making them extremely inexpensive. In the latest MXS design, UV efficiency is addressed by using a high-gain electron multiplier. The photocathode is vapor-deposited onto the input cone of a Burle Magnum(TradeMark) multiplier. This system yields an extremely robust photon-driven electron source that can tolerate long, weeks or more, exposure to air with negligible degradation. The package is also small. When combined with the electron target, necessary vacuum fittings, and supporting components (but not including LED electronics or high-voltage sources), the entire modulated x-ray source weighs as little as 158 grams.

Processings of the Workshop on Electron Contamination in X-Ray Astronomy Experiments. [proceedings of conference on effects of extraterrestrial radiation

NASA Technical Reports Server (NTRS)

Holt, S. S. (Editor)

1974-01-01

The proceedings of a conference to investigate the effects of extraterrestrial radiation and particle contamination of X-ray astronomical data are presented. The subjects discussed include the following: (1) electrons at low altitudes which affect soft X-ray astronomy, (2) the geographical distribution of 100 keV electrons above the earth's atmosphere, (3) midlatitude electron precipitation, (4) particle background observed by X-ray detectors on board Copernicus satellite, and (5) a survey of trapped low energy electrons near the inner boundary of the inner radiation zone as determined by OSO-7.

Discovery of Diffuse Hard X-ray Emission associated with Jupiter

NASA Astrophysics Data System (ADS)

Ezoe, Y.; Miyoshi, Y.; Ishikawa, K.; Ohashi, T.; Terada, N.; Uchiyama, Y.; Negoro, H.

2009-12-01

Our discovery of diffuse hard (1-5 keV) X-ray emission around Jupiter is reported. Recent Chandra and XMM-Newton observations revealed several types of X-rays in the vicinity of Jupiter such as auroral and disk emission from Jupiter and faint diffuse X-rays from the Io Plasma Torus (see Bhardwaj et al. 2007 for review). To investigate possible diffuse hard X-ray emission around Jupiter with the highest sensitivity, we conducted data analysis of Suzaku XIS observations of Jupiter on Feb 2006. After removing satellite and planetary orbital motions, we detected a significant diffuse X-ray emission extending to ~6 x 3 arcmin with the 1-5 keV X-ray luminosity of ~3e15 erg/s. The emitting region very well coincided with the Jupiter's radiation belts. The 1-5 keV X-ray spectrum was represented by a simple power law model with a photon index of 1.4. Such a flat continuum strongly suggests non-thermal origin. Although such an emission can be originated from multiple background point sources, its possibility is quite low. We hence examined three mechanisms, assuming that the emission is truly diffuse: bremsstrahlung by keV electrons, synchrotron emission by TeV electrons, and inverse Compton scattering of solar photons by MeV electrons. The former two can be rejected because of the X-ray spectral shape and implausible existence of TeV electrons around Jupiter, respectively. The last possibility was found to be possible because tens MeV electrons, which have been confirmed in inner radiation belts (Bolton et al. 2002), can kick solar photons to the keV energy range and provide a simple power-law continuum. We estimated an average electron density from the X-ray luminosity assuming the oblate spheroid shaped emitting region with 8 x 8 x 4 Jovian radii. The necessary density was 0.02 1/cm3 for 50 MeV electrons. Hence, our results may suggest a new particle acceleration phenomenon around Jupiter.

Homogeneous and heterogenized iridium water oxidation catalysts

NASA Astrophysics Data System (ADS)

Macchioni, Alceo

2014-10-01

The development of an efficient catalyst for the oxidative splitting of water into molecular oxygen, protons and electrons is of key importance for producing solar fuels through artificial photosynthesis. We are facing the problem by means of a rational approach aimed at understanding how catalytic performance may be optimized by the knowledge of the reaction mechanism of water oxidation and the fate of the catalytic site under the inevitably harsh oxidative conditions. For the purposes of our study we selected iridium water oxidation catalysts, exhibiting remarkable performance (TOF > 5 s-1 and TON > 20000). In particular, we recently focused our attention on [Cp*Ir(N,O)X] (N,O = 2-pyridincarboxylate; X = Cl or NO3) and [IrCl(Hedta)]Na water oxidation catalysts. The former exhibited a remarkable TOF whereas the latter showed a very high TON. Furthermore, [IrCl(Hedta)]Na was heterogenized onto TiO2 taking advantage of the presence of a dandling -COOH functionality. The heterogenized catalyst maintained approximately the same catalytic activity of the homogeneous analogous with the advantage that could be reused many times. Mechanistic studies were performed in order to shed some light on the rate-determining step and the transformation of catalysts when exposed to "oxidative stress". It was found that the last oxidative step, preceding oxygen liberation, is the rate-determining step when a small excess of sacrificial oxidant is used. In addition, several intermediates of the oxidative transformation of the catalyst were intercepted and characterized by NMR, X-Ray diffractometry and ESI-MS.

Femtosecond profiling of shaped x-ray pulses

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

Hoffmann, M. C.; Grguras, I.; Behrens, C.

Arbitrary manipulation of the temporal and spectral properties of x-ray pulses at free-electron lasers would revolutionize many experimental applications. At the Linac Coherent Light Source at Stanford National Accelerator Laboratory, the momentum phase-space of the free-electron laser driving electron bunch can be tuned to emit a pair of x-ray pulses with independently variable photon energy and femtosecond delay. However, while accelerator parameters can easily be adjusted to tune the electron bunch phase-space, the final impact of these actuators on the x-ray pulse cannot be predicted with sufficient precision. Furthermore, shot-to-shot instabilities that distort the pulse shape unpredictably cannot be fullymore » suppressed. Therefore, the ability to directly characterize the x-rays is essential to ensure precise and consistent control. In this work, we have generated x-ray pulse pairs via electron bunch shaping and characterized them on a single-shot basis with femtosecond resolution through time-resolved photoelectron streaking spectroscopy. Furthermore, this achievement completes an important step toward future x-ray pulse shaping techniques.« less

Femtosecond profiling of shaped x-ray pulses

DOE PAGES

Hoffmann, M. C.; Grguras, I.; Behrens, C.; ...

2018-03-26

Arbitrary manipulation of the temporal and spectral properties of x-ray pulses at free-electron lasers would revolutionize many experimental applications. At the Linac Coherent Light Source at Stanford National Accelerator Laboratory, the momentum phase-space of the free-electron laser driving electron bunch can be tuned to emit a pair of x-ray pulses with independently variable photon energy and femtosecond delay. However, while accelerator parameters can easily be adjusted to tune the electron bunch phase-space, the final impact of these actuators on the x-ray pulse cannot be predicted with sufficient precision. Furthermore, shot-to-shot instabilities that distort the pulse shape unpredictably cannot be fullymore » suppressed. Therefore, the ability to directly characterize the x-rays is essential to ensure precise and consistent control. In this work, we have generated x-ray pulse pairs via electron bunch shaping and characterized them on a single-shot basis with femtosecond resolution through time-resolved photoelectron streaking spectroscopy. Furthermore, this achievement completes an important step toward future x-ray pulse shaping techniques.« less

Attosecond time-energy structure of X-ray free-electron laser pulses

NASA Astrophysics Data System (ADS)

Hartmann, N.; Hartmann, G.; Heider, R.; Wagner, M. S.; Ilchen, M.; Buck, J.; Lindahl, A. O.; Benko, C.; Grünert, J.; Krzywinski, J.; Liu, J.; Lutman, A. A.; Marinelli, A.; Maxwell, T.; Miahnahri, A. A.; Moeller, S. P.; Planas, M.; Robinson, J.; Kazansky, A. K.; Kabachnik, N. M.; Viefhaus, J.; Feurer, T.; Kienberger, R.; Coffee, R. N.; Helml, W.

2018-04-01

The time-energy information of ultrashort X-ray free-electron laser pulses generated by the Linac Coherent Light Source is measured with attosecond resolution via angular streaking of neon 1s photoelectrons. The X-ray pulses promote electrons from the neon core level into an ionization continuum, where they are dressed with the electric field of a circularly polarized infrared laser. This induces characteristic modulations of the resulting photoelectron energy and angular distribution. From these modulations we recover the single-shot attosecond intensity structure and chirp of arbitrary X-ray pulses based on self-amplified spontaneous emission, which have eluded direct measurement so far. We characterize individual attosecond pulses, including their instantaneous frequency, and identify double pulses with well-defined delays and spectral properties, thus paving the way for X-ray pump/X-ray probe attosecond free-electron laser science.

THz-pump and X-ray-probe sources based on an electron linac.

PubMed

Setiniyaz, Sadiq; Park, Seong Hee; Kim, Hyun Woo; Vinokurov, Nikolay A; Jang, Kyu-Ha; Lee, Kitae; Baek, In Hyung; Jeong, Young Uk

2017-11-01

We describe a compact THz-pump and X-ray-probe beamline, based on an electron linac, for ultrafast time-resolved diffraction applications. Two high-energy electron (γ > 50) bunches, 5 ns apart, impinge upon a single-foil or multifoil radiator and generate THz radiation and X-rays simultaneously. The THz pulse from the first bunch is synchronized to the X-ray beam of the second bunch by using an adjustable optical delay of a THz pulse. The peak power of THz radiation from the multifoil radiator is estimated to be 0.14 GW for a 200 pC well-optimized electron bunch. GEANT4 simulations show that a carbon foil with a thickness of 0.5-1.0 mm has the highest yield of 10-20 keV hard X-rays for a 25 MeV beam, which is approximately 10 3 photons/(keV pC-electrons) within a few degrees of the polar angle. A carbon multifoil radiator with 35 foils (25 μm thick each) can generate close to 10 3 hard X-rays/(keV pC-electrons) within a 2° acceptance angle. With 200 pC charge and a 100 Hz repetition rate, we can generate 10 7 X-rays per 1 keV energy bin per second or 10 5 X-rays per 1 keV energy bin per pulse. The longitudinal time profile of an X-ray pulse ranges from 400 to 600 fs depending on the acceptance angle. The broadening of the time duration of an X-ray pulse is observed owing to its diverging effect. A double-crystal monochromator will be used to select and transport the desired X-rays to the sample. The heating of the radiators by an electron beam is negligible because of the low beam current.

Growth and Electronic Structure of Heusler Compounds for Use in Electron Spin Based Devices

DTIC Science & Technology

2015-06-01

either Co– or MnSi– initiated films on c(4x4) GaAs. Studies using x - ray photoemission spectroscopy (XPS), STM/STS, and transmission electron microscopy...Co– or MnSi– initiated films on c(4x4) GaAs. Studies using x - ray photoemission spectroscopy (XPS), STM/STS, and transmission electron microscopy (TEM...diagram of the Palmstrøm lab in-situ growth and char- acterization setup, with 6 MBE growth chambers, 3 scanning probe microscopes, an x - ray

Long life electrodes for large-area x-ray generators

NASA Technical Reports Server (NTRS)

Rothe, Dietmar E. (Inventor)

1991-01-01

This invention is directed to rugged, reliable, and long-life electrodes for use in large-area, high-current-density electron gun and x-ray generators which are employed as contamination-free preionizers for high-energy pulsed gas lasers. The electron source at the cathode is a corona plasma formed at the interface between a conductor, or semiconductor, and a high-permittivity dielectric. Detailed descriptions are provided of a reliable cold plasma cathode, as well as an efficient liquid-cooled electron beam target (anode) and x-ray generator which concentrates the x-ray flux in the direction of an x-ray window.

X-ray spectra and electron structure of A15 compounds of transition metals

NASA Astrophysics Data System (ADS)

Kurmaev, E. Z.; Iarmoshenko, Iu. M.

1988-01-01

Results of an X-ray emission spectroscopy study of the electron structure of A15 compounds are reported. In particular, attention is given to the X-ray spectra of A15 compounds of the A3B type with transition and nontransition elements, effect of alloying on the formation of the electron structure of ternary phases, and effect of atomic ordering in the X-ray spectra of A15 compounds with changes in heat treament and concentration. The X-ray spectra of A15 compounds irradiated by fast neutrons are also examined.

Two types of electron events in solar flares

NASA Technical Reports Server (NTRS)

Daibog, E. I.; Kurt, V. G.; Logachev, Y. I.; Stolpovsky, V. G.

1985-01-01

The fluxes and spectra of the flare electrons measured on board Venera-I3 and I4 space probes are compared with the parameters of the hard (E sub x approximately 55 keV) and thermal X-ray bursts. The electron flux amplitude has been found to correlate with flare importance in the thermal X-ray range (r approximately 0.8). The following two types of flare events have been found in the electron component of SCR. The electron flux increase is accompanied by a hard X-ray burst and the electron spectrum index in the approximately 25 to 200 keV energy range is gamma approximately 2 to 3. The electron flux increase is not accompanied by a hard X-ray burst and the electron spectrum is softer (Delta gamma approximately 0.7 to 1.0).

On the properties of synchrotron-like X-ray emission from laser wakefield accelerated electron beams

NASA Astrophysics Data System (ADS)

McGuffey, C.; Schumaker, W.; Matsuoka, T.; Chvykov, V.; Dollar, F.; Kalintchenko, G.; Kneip, S.; Najmudin, Z.; Mangles, S. P. D.; Vargas, M.; Yanovsky, V.; Maksimchuk, A.; Thomas, A. G. R.; Krushelnick, K.

2018-04-01

The electric and magnetic fields responsible for electron acceleration in a Laser Wakefield Accelerator (LWFA) also cause electrons to radiate x-ray photons. Such x-ray pulses have several desirable properties including short duration and being well collimated with tunable high energy. We measure the scaling of this x-ray source experimentally up to laser powers greater than 100 TW. An increase in laser power allows electron trapping at a lower density as well as with an increased trapped charge. These effects resulted in an x-ray fluence that was measured to increase non-linearly with laser power. The fluence of x-rays was also compared with that produced from K-α emission resulting from a solid target interaction for the same energy laser pulse. The flux was shown to be comparable, but the LWFA x-rays had a significantly smaller source size. This indicates that such a source may be useful as a backlighter for probing high energy density plasmas with ultrafast temporal resolution.

THE X-RAY DETECTABILITY OF ELECTRON BEAMS ESCAPING FROM THE SUN

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

Saint-Hilaire, Pascal; Krucker, Saem; Christe, Steven

2009-05-01

We study the detectability and characterization of electron beams as they leave their acceleration site in the low corona toward interplanetary space through their nonthermal X-ray bremsstrahlung emission. We demonstrate that the largest interplanetary electron beams ({approx}>10{sup 35} electrons above 10 keV) can be detected in X-rays with current and future instrumentation, such as RHESSI or the X-Ray Telescope (XRT) onboard Hinode. We make a list of optimal observing conditions and beam characteristics. Amongst others, good imaging (as opposed to mere localization or detection in spatially integrated data) is required for proper characterization, putting the requirement on the number ofmore » escaping electrons (above 10 keV) to {approx}>3 x 10{sup 36} for RHESSI, {approx}>3 x 10{sup 35} for Hinode/XRT, and {approx}>10{sup 33} electrons for the FOXSI sounding rocket scheduled to fly in 2011. Moreover, we have found that simple modeling hints at the possibility that coronal soft X-ray jets could be the result of local heating by propagating electron beams.« less

The nanosphere iron mineral(s) in Mars soil

NASA Technical Reports Server (NTRS)

Banin, A.; Ben-Shlomo, T.; Margulies, L.; Blake, D. F.; Mancinelli, R. L.; Gehring, A. U.

1993-01-01

A series of surface-modified clays containing nanophase (np) iron/oxyhydroxides of extremely small particle sizes, with total iron contents as high as found in Mars soil, were prepared by iron deposition on the clay surface from ferrous chloride solution. Comprehensive studies of the iron mineralogy in these 'Mars-soil analogs' were conducted using chemical extractions, solubility analyses, pH and redox, x ray and electron diffractometry, electron microscopic imaging specific surface area and particle size determinations, differential thermal analyses, magnetic properties characterization, spectral reflectance, and Viking biology simulation experiments. The clay matrix and the procedure used for synthesis produced nanophase iron oxides containing a certain proportion of divalent iron, which slowly converts to more stable, fully oxidized iron minerals. The noncrystalline nature of the iron compounds precipitated on the surface of the clay was verified by their complete extractability in oxalate. Lepidocrocite (gamma-FeOOH) was detected by selected area electron diffraction. It is formed from a double iron Fe(II)/Fe(III) hydroxyl mineral such as 'green rust', or ferrosic hydroxide. Magnetic measurements suggested that lepidocrocite converted to the more stable meaghemite (gamma-Fe203) by mild heat treatment and then to nanophase hematite (aplha-Fe203) by extensive heat treatment. Their chemical reactivity offers a plausible mechanism for the somewhat puzzling observations of the Viking biology experiments. Their unique chemical reactivities are attributed to the combined catalytic effects of the iron oxide/oxyhydroxide and silicate phase surfaces. The mode of formation of these (nanophase) iron oxides on Mars is still unknown.

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

Liu, Zheng; Li, Zhilin; Institute of Carbon Fibers and Composites, Beijing University of Chemical Technology, Beijing 100029

Graphical abstract: The MWCNT/Ni-B catalyst has been successfully prepared by an electroless deposition process. The Ni-B nanoparticles on the supporter are amorphous and are well-distributed. The catalytic conversion towards hydrogenation of styrene shows excellent catalytic activity of the obtained materials. Highlights: Black-Right-Pointing-Pointer A two-step treatment of MWCNTs enabled the homogeneous growth of Ni-B nanoparticles. Black-Right-Pointing-Pointer Ni-B nanoparticles were amorphous with an average size of 60 nm. Black-Right-Pointing-Pointer There were electron transfer between Ni and B. Black-Right-Pointing-Pointer The catalyst had excellent catalytic activity towards hydrogenation of styrene. -- Abstract: Nickel-boron (Ni-B) nanoparticles supported on multi-walled carbon nanotubes (MWCNTs) were successfully synthesizedmore » through an electroless deposition process using the plating bath with sodium borohydride as a reducing agent. The structural and morphological analyses using field-emission scanning electron microscopy, X-ray diffractometry and high-resolution transmission electron microscopy have shown that the Ni-B nanoparticles deposited on the sidewalls of MWCNTs are fine spheres comprised of amorphous structure with the morphologically unique fine-structure like flowers, and homogenously dispersed with a narrow particle size distribution centered at around 60 nm diameter. The catalytic activity of MWCNT/Ni-B nanoparticles was evaluated with respect to hydrogenation of styrene. The hydrogenation catalyzed by MWCNT-supported Ni-B nanoparticles has been found to make styrene selectively converted into ethylbenzene. The highest conversion reaches 99.8% under proper reaction conditions, which demonstrates the high catalytic activity of MWCNT/Ni-B nanoparticles.« less

X-ray analysis of electron Bernstein wave heating in MST

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

Seltzman, A. H., E-mail: seltzman@wisc.edu; Anderson, J. K.; DuBois, A. M.

2016-11-15

A pulse height analyzing x-ray tomography system has been developed to detect x-rays from electron Bernstein wave heated electrons in the Madison symmetric torus reversed field pinch (RFP). Cadmium zinc telluride detectors are arranged in a parallel beam array with two orthogonal multi-chord detectors that may be used for tomography. In addition a repositionable 16 channel fan beam camera with a 55° field of view is used to augment data collected with the Hard X-ray array. The chord integrated signals identify target emission from RF heated electrons striking a limiter located 12° toroidally away from the RF injection port. Thismore » provides information on heated electron spectrum, transport, and diffusion. RF induced x-ray emission from absorption on harmonic electron cyclotron resonances in low current (<250 kA) RFP discharges has been observed.« less

Quantitative electron density characterization of soft tissue substitute plastic materials using grating-based x-ray phase-contrast imaging

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

Sarapata, A.; Chabior, M.; Zanette, I.

2014-10-15

Many scientific research areas rely on accurate electron density characterization of various materials. For instance in X-ray optics and radiation therapy, there is a need for a fast and reliable technique to quantitatively characterize samples for electron density. We present how a precise measurement of electron density can be performed using an X-ray phase-contrast grating interferometer in a radiographic mode of a homogenous sample in a controlled geometry. A batch of various plastic materials was characterized quantitatively and compared with calculated results. We found that the measured electron densities closely match theoretical values. The technique yields comparable results between amore » monochromatic and a polychromatic X-ray source. Measured electron densities can be further used to design dedicated X-ray phase contrast phantoms and the additional information on small angle scattering should be taken into account in order to exclude unsuitable materials.« less

High flux femtosecond x-ray emission from the electron-hose instability in laser wakefield accelerators

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

Dong, C. F.; Zhao, T. Z.; Behm, K.

Here, bright and ultrashort duration x-ray pulses can be produced by through betatron oscillations of electrons during laser wakefield acceleration (LWFA). Our experimental measurements using the Hercules laser system demonstrate a dramatic increase in x-ray flux for interaction distances beyond the depletion/dephasing lengths, where the initial electron bunch injected into the first wake bucket catches up with the laser pulse front and the laser pulse depletes. A transition from an LWFA regime to a beam-driven plasma wakefield acceleration regime consequently occurs. The drive electron bunch is susceptible to the electron-hose instability and rapidly develops large amplitude oscillations in its tail,more » which leads to greatly enhanced x-ray radiation emission. We measure the x-ray flux as a function of acceleration length using a variable length gas cell. 3D particle-in-cell simulations using a Monte Carlo synchrotron x-ray emission algorithm elucidate the time-dependent variations in the radiation emission processes.« less

High flux femtosecond x-ray emission from the electron-hose instability in laser wakefield accelerators

NASA Astrophysics Data System (ADS)

Dong, C. F.; Zhao, T. Z.; Behm, K.; Cummings, P. G.; Nees, J.; Maksimchuk, A.; Yanovsky, V.; Krushelnick, K.; Thomas, A. G. R.

2018-04-01

Bright and ultrashort duration x-ray pulses can be produced by through betatron oscillations of electrons during laser wakefield acceleration (LWFA). Our experimental measurements using the Hercules laser system demonstrate a dramatic increase in x-ray flux for interaction distances beyond the depletion/dephasing lengths, where the initial electron bunch injected into the first wake bucket catches up with the laser pulse front and the laser pulse depletes. A transition from an LWFA regime to a beam-driven plasma wakefield acceleration regime consequently occurs. The drive electron bunch is susceptible to the electron-hose instability and rapidly develops large amplitude oscillations in its tail, which leads to greatly enhanced x-ray radiation emission. We measure the x-ray flux as a function of acceleration length using a variable length gas cell. 3D particle-in-cell simulations using a Monte Carlo synchrotron x-ray emission algorithm elucidate the time-dependent variations in the radiation emission processes.

High flux femtosecond x-ray emission from the electron-hose instability in laser wakefield accelerators

DOE PAGES

Dong, C. F.; Zhao, T. Z.; Behm, K.; ...

2018-04-24

Here, bright and ultrashort duration x-ray pulses can be produced by through betatron oscillations of electrons during laser wakefield acceleration (LWFA). Our experimental measurements using the Hercules laser system demonstrate a dramatic increase in x-ray flux for interaction distances beyond the depletion/dephasing lengths, where the initial electron bunch injected into the first wake bucket catches up with the laser pulse front and the laser pulse depletes. A transition from an LWFA regime to a beam-driven plasma wakefield acceleration regime consequently occurs. The drive electron bunch is susceptible to the electron-hose instability and rapidly develops large amplitude oscillations in its tail,more » which leads to greatly enhanced x-ray radiation emission. We measure the x-ray flux as a function of acceleration length using a variable length gas cell. 3D particle-in-cell simulations using a Monte Carlo synchrotron x-ray emission algorithm elucidate the time-dependent variations in the radiation emission processes.« less

Probing solid catalysts under operating conditions: electrons or X-rays?

PubMed

Thomas, John Meurig; Hernandez-Garrido, Juan-Carlos

2009-01-01

Seeing is believing: In light of recent advances, the pros and cons of using electrons and X-rays for in situ studies of catalysts are analyzed: by using X-rays the structure of bound reactants at steady state are obtained from extended X-ray adsorption fine structure spectroscopy (EXAFS) data (see graph), thereby affording mechanistic insights.

Characterization of Synthetic and Natural Manganese Oxides as Martian Analogues

NASA Technical Reports Server (NTRS)

Fox, V. K.; Arvidson, R. E.; Jolliff, B. L.; Carpenter, P. K.; Catalano, J. G.; Hinkle, M. A. G.; Morris, R. V.

2015-01-01

Recent discoveries of highly concentrated manganese oxides in Gale Crater and on the rim of Endeavour Crater by the Mars Science Laboratory Curiosity and Mars Exploration Rover Opportunity, respectively, imply more highly oxidizing aqueous conditions than previously recognized. Manganese oxides are a significant environmental indicator about ancient aqueous conditions, provided the phases can be characterized reliably. Manganese oxides are typically fine-grained and poorly crystalline, making the mineral structures difficult to determine, and they generally have very low visible reflectance with few distinctive spectral features in the visible to near infrared, making them a challenge for interpretation from remote sensing data. Therefore, these recent discoveries motivate better characterization using methods available on Mars, particularly visible to near infrared (VNIR) spectroscopy, X-ray diffractometry (XRD), and compositional measurements. Both rovers have complementary instruments in this regard. Opportunity is equipped with its multispectral visible imager, Pancam, and an Alpha Particle X-ray Spectrometer (APXS), and Curiosity has the multispectral Mastcam, ChemCam (laser-induced breakdown spectroscopy and passive spectroscopy), and APXS for in situ characterization, and ChemMin (XRD) for collected samples.

Proteomic analysis of a rare urinary stone composed of calcium carbonate and calcium oxalate dihydrate: a case report.

PubMed

Kaneko, Kiyoko; Matsuta, Yosuke; Moriyama, Manabu; Yasuda, Makoto; Chishima, Noriharu; Yamaoka, Noriko; Fukuuchi, Tomoko; Miyazawa, Katsuhito; Suzuki, Koji

2014-03-01

The objective of the present study was to investigate the matrix protein of a rare urinary stone that contained calcium carbonate. A urinary stone was extracted from a 34-year-old male patient with metabolic alkalosis. After X-ray diffractometry and infrared analysis of the stone, proteomic analysis was carried out. The resulting mass spectra were evaluated with protein search software, and matrix proteins were identified. X-ray diffraction and infrared analysis confirmed that the stone contained calcium carbonate and calcium oxalate dihydrate. Of the identified 53 proteins, 24 have not been previously reported from calcium oxalate- or calcium phosphate-containing stones. The protease inhibitors and several proteins related to cell adhesion or the cytoskeleton were identified for the first time. We analyzed in detail a rare urinary stone composed of calcium carbonate and calcium oxalate dihydrate. Considering the formation of a calcium carbonate stone, the new identified proteins should play an important role on the urolithiasis process in alkaline condition. © 2013 The Japanese Urological Association.

Uncommon and Emissive {[Au2(C3H6NS2)2][Au(C3H6NS2)2]2(PF6)2} Mixed Au+ and Au3+ Pseudotetranuclear Crystalline Compound: Synthesis, Structural Characterization, and Optical Properties.

PubMed

Langaro, Ana P; Souza, Ana K R; Morassuti, Claudio Y; Lima, Sandro M; Casagrande, Gleison A; Deflon, Victor M; Nunes, Luiz A O; Da Cunha Andrade, Luis H

2016-11-23

An uncommon emissive pseudotetranuclear compound, {[Au 2 (C 3 H 6 NS 2 ) 2 ][Au(C 3 H 6 NS 2 ) 2 ] 2 (PF 6 ) 2 }, was synthesized and characterized in terms of its structure and optical properties. The synthesis produced a crystalline compound composed of four gold atoms with two different oxidation states (Au + and Au 3+ ) in the same crystalline structure. The title complex belonged to a triclinic crystalline system involving the centrosymmetric P1̅ space group. X-ray diffractometry and vibrational spectroscopy (infrared, Raman, and SERS) were used for structural characterization of the new crystal. The vibrational spectroscopy techniques supported the X-ray diffraction results and confirmed the presence of bonds including Au-Au and Au-S. Optical characterization performed using UV-vis spectroscopy showed that under ultraviolet excitation, the emissive crystalline complex presented characteristic broad luminescent bands centered at 420 and 670 nm.

Crystal structure and thermal expansion of a CsCe 2Cl 7 scintillator

DOE PAGES

Zhuravleva, M.; Lindsey, A.; Chakoumakos, B. C.; ...

2015-04-06

Here we used single-crystal X-ray diffraction data to determine crystal structure of CsCe 2Cl 7. It crystallizes in a P112 1/b space group with a = 19.352(1) Å, b = 19.352(1) Å, c = 14.838(1) Å, γ = 119.87(2) ° , and V = 4818.6(5) Å 3. Differential scanning calorimetry measurements combined with the structural evolution of CsCe 2Cl 7 via X-ray diffractometry over a temperature range from room temperature to the melting point indicates no obvious intermediate solid-solid phase transitions. The anisotropy in the average linear coefficient of thermal expansion of the a axis (21.3 10 -6/ °C) withmore » respect to the b and c axes (27.0 10 -6/ °C) was determined through lattice parameter refinement of the temperature dependent diffraction patterns. Lastly, these findings suggest that the reported cracking behavior during melt growth of CsCe 2Cl 7 bulk crystals using conventional Bridgman and Czochralski techniques may be largely attributed to the anisotropy in thermal expansion.« less

Behavior of pure gallium in water and various saline solutions.

PubMed

Horasawa, N; Nakajima, H; Takahashi, S; Okabe, T

1997-12-01

This study investigated the chemical stability of pure gallium in water and saline solutions in order to obtain fundamental knowledge about the corrosion mechanism of gallium-based alloys. A pure gallium plate (99.999%) was suspended in 50 mL of deionized water, 0.01%, 0.1% or 1% NaCl solution at 24 +/- 2 degrees C for 1, 7, or 28 days. The amounts of gallium released into the solutions were determined by atomic absorption spectrophotometry. The surfaces of the specimens were examined after immersion by x-ray diffractometry (XRD) and x-ray photoelectron spectroscopy (XPS). In the solutions containing 0.1% or more NaCl, the release of gallium ions into the solution was lowered when compared to deionized water after 28-day immersion. Gallium oxide monohydroxide was found by XRD on the specimens immersed in deionized water after 28-day immersion. XPS indicated the formation of gallium oxide/hydroxide on the specimens immersed in water or 0.01% NaCl solution. The chemical stability of pure solid gallium was strongly affected by the presence of Cl- ions in the aqueous solution.

Quantum theory for 1D X-ray free electron laser

DOE PAGES

Anisimov, Petr Mikhaylovich

2017-09-19

Classical 1D X-ray Free Electron Laser (X-ray FEL) theory has stood the test of time by guiding FEL design and development prior to any full-scale analysis. Future X-ray FELs and inverse-Compton sources, where photon recoil approaches an electron energy spread value, push the classical theory to its limits of applicability. After substantial efforts by the community to find what those limits are, there is no universally agreed upon quantum approach to design and development of future X-ray sources. We offer a new approach to formulate the quantum theory for 1D X-ray FELs that has an obvious connection to the classicalmore » theory, which allows for immediate transfer of knowledge between the two regimes. In conclusion, we exploit this connection in order to draw quantum mechanical conclusions about the quantum nature of electrons and generated radiation in terms of FEL variables.« less

Quantum theory for 1D X-ray free electron laser

NASA Astrophysics Data System (ADS)

Anisimov, Petr M.

2018-06-01

Classical 1D X-ray Free Electron Laser (X-ray FEL) theory has stood the test of time by guiding FEL design and development prior to any full-scale analysis. Future X-ray FELs and inverse-Compton sources, where photon recoil approaches an electron energy spread value, push the classical theory to its limits of applicability. After substantial efforts by the community to find what those limits are, there is no universally agreed upon quantum approach to design and development of future X-ray sources. We offer a new approach to formulate the quantum theory for 1D X-ray FELs that has an obvious connection to the classical theory, which allows for immediate transfer of knowledge between the two regimes. We exploit this connection in order to draw quantum mechanical conclusions about the quantum nature of electrons and generated radiation in terms of FEL variables.

X-ray diagnostic development for measurement of electron deposition to the SABRE anode

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

Lash, J.S.; Derzon, M.S.; Cuneo, M.E.

Extraction applied-B ion diodes are under development on the SABRE (6 MV, 250 kA) accelerator at Sandia. The authors are assessing this technology for the production of high brightness lithium ion beams for inertial confinement fusion. Electron loss physics is a focus of effort since electron sheath physics affects ion beam divergence, ion beam purity, and diode impedance. An x-ray slit-imaging diagnostic is under development for detection of x-rays produced during electron deposition to the anode. This diagnostic will aid in the correlation of electron deposition to ion production to better understand the ion diode physics. The x-ray detector consistsmore » of a filter pack, scintillator and optical fiber array that is streaked onto a CCD camera. Current orientation of the diagnostic provides spatial information across the anode radius at three different azimuths or at three different x-ray energy cuts. The observed x-ray emission spectrum can then be compared to current modeling efforts examining electron deposition to the anode.« less

Radiation of X-Rays Using Uniaxially Polarized LiNbO3 Single Crystal

NASA Astrophysics Data System (ADS)

Fukao, Shinji; Nakanishi, Yoshikazu; Mizoguchi, Tadahiro; Ito, Yoshiaki; Nakamura, Toru; Yoshikado, Shinzo

2009-03-01

X-rays are radiated due to the bremsstrahlung caused by the collision of electrons with a metal target placed opposite the negative electric surface of a crystal by changing the temperature of a LiNbO3 single crystal uniaxially polarized in the c-axis direction. It is suggested that both electric field intensity and electron density determine the intensity of X-ray radiation. Electrons are supplied by the ionization of residual gas in space, field emission from a case inside which a crystal is located, considered to be due to the high electric-field intensity formed by the surface charges on the crystal, and an external electron source, such as a thermionic source. In a high vacuum, it was found that the electrons supplied by electric-field emission mainly contribute to the radiation of X-rays. It was found that the integrated intensity of X-rays can be maximized by supplying electrons both external and by electric-field emission. Furthermore, the integrated intensity of the X-rays is stable for many repeated temperature changes.

Characterization of (Ba(0.5)Sr(0.5)) TiO3 Thin Films for Ku-Band Phase Shifters

NASA Technical Reports Server (NTRS)

Mueller, Carl H.; VanKeuls, Fredrick W.; Romanofsky, Robert R.; Miranda, Felix A.; Warner, Joseph D.; Canedy, Chadwick L.; Ramesh, Rammamoorthy

1999-01-01

The microstructural properties of (Ba(0.5)Sr(0.5)TiO3) (BSTO) thin films (300, 700, and 1400 nm thick) deposited on LaAlO3 (LAO) substrates were characterized using high-resolution x-ray diffractometry. Film crystallinity was the parameter that most directly influenced tunability, and we observed that a) the crystalline quality was highest in the thinnest film and progressively degraded with increasing film thickness; and b) strain at the film/substrate interface was completely relieved via dislocation formation. Paraelectric films such as BSTO offer an attractive means of incorporating low-cost phase shifter circuitry into beam-steerable reflectarray antennas.

Solid-state properties and crystallization behavior of PHA-739521 polymorphs.

PubMed

Sun, Changquan Calvin

2006-08-17

PHA-739521 is an experimental compound that exhibits polymorphism. The two anhydrous crystal forms, I and II, are characterized using powder X-ray diffractometry, thermal analyses, moisture sorption gravimetry. Both Forms I and II are non-hygroscopic and are stable to compaction pressure. The melting temperature is about 152 degrees C for Form I and 168 degrees C for Form II. Forms I and II are enantiotropically related where Form I is more stable below a transition temperature of approximately 70 degrees C. Crystallization behavior of this compound from solutions and during heating is also studied. Information obtained is used to design an appropriate crystallization process to successfully manufacture desired polymorph at large scale.

Possible role of Prussian blue nanoparticles in chemical evolution: interaction with ribose nucleotides

NASA Astrophysics Data System (ADS)

Sharma, Rachana; Iqubal, Md. Asif; Kamaluddin

2016-01-01

Ribonucleotides (RMPs) are the building blocks of genetic material consisting of a sugar group, a phosphate group and a nucleobase. Prussian blue (PB) is an ancient compound which is supposed to have formed under the conditions of primitive Earth. The interaction between nucleotides and mineral surfaces is of primary importance in the context of prebiotic chemistry. In the present work, the adsorption of RMPs on PB has been studied in the concentration range 0.4 × 10-4-3.0 × 10-4 M of RMPs at pH 7.5, T = 27°C and found to be 53.1, 41.7, 25.8 and 24.0% for adenosine 5'-monophosphate (5'-AMP), guanosine 5'-monophosphate, cytidine 5'-monophosphate and uridine 5'-monophosphate, respectively. Optimum conditions for the adsorption were studied as a function of concentration, time, amount of adsorbent and pH and data obtained were found to fit the Langmuir adsorption isotherm. Langmuir constants (K L and X m ) values were calculated. Fourier transform infrared spectroscopy, Raman spectroscopy, field-emission scanning electron microscopy and X-ray diffractometry techniques were used to investigate the interaction of RMPs on PB surface. Adsorption kinetics of 5'-AMP on PB has been found to be pseudo-second order. Results obtained from this study should prove valuable for a better understanding of the mechanism of RMP-PB interaction.

On the modulation of X ray fluxes in thunderstorms

NASA Technical Reports Server (NTRS)

Mccarthy, Michael P.; Parks, George K.

1992-01-01

The production of X-ray fluxes in thunderstorms has been attributed to bremsstrahlung. Assuming this, another question arises. How can a thunderstorm modulate the number density of electrons which are sufficiently energetic to produce X-rays? As a partial answer to this question, the effects of typical thunderstorm electric fields on a background population of energetic electrons, such as produced by cosmic ray secondaries and their decays or the decay of airborne radionuclides, are considered. The observed variation of X-ray flux is shown to be accounted for by a simple model involving typical electric field strengths. A necessary background electron number density is found from the model and is determined to be more than 2 orders of magnitude higher than that available from radon decay and a factor of 8 higher than that available from cosmic ray secondaries. The ionization enhancement due to energetic electrons and X-rays is discussed.

Femtosecond all-optical synchronization of an X-ray free-electron laser

DOE PAGES

Schulz, S.; Grguraš, I.; Behrens, C.; ...

2015-01-20

Many advanced applications of X-ray free-electron lasers require pulse durations and time resolutions of only a few femtoseconds. To generate these pulses and to apply them in time-resolved experiments, synchronization techniques that can simultaneously lock all independent components, including all accelerator modules and all external optical lasers, to better than the delivered free-electron laser pulse duration, are needed. Here we achieve all-optical synchronization at the soft X-ray free-electron laser FLASH and demonstrate facility-wide timing to better than 30 fs r.m.s. for 90 fs X-ray photon pulses. Crucially, our analysis indicates that the performance of this optical synchronization is limited primarilymore » by the free-electron laser pulse duration, and should naturally scale to the sub-10 femtosecond level with shorter X-ray pulses.« less

Time-dependent Schrödinger equation for molecular core-hole dynamics

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

Picón, A.

2017-02-01

X-ray spectroscopy is an important tool for the investigation of matter. X rays primarily interact with inner-shell electrons, creating core (inner-shell) holes that will decay on the time scale of attoseconds to a few femtoseconds through electron relaxations involving the emission of a photon or an electron. Furthermore, the advent of femtosecond x-ray pulses expands x-ray spectroscopy to the time domain and will eventually allow the control of core-hole population on time scales comparable to core-vacancy lifetimes. For both cases, a theoretical approach that accounts for the x-ray interaction while the electron relaxations occur is required. We describe a time-dependentmore » framework, based on solving the time-dependent Schrödinger equation, that is suitable for describing the induced electron and nuclear dynamics.« less

Femtosecond all-optical synchronization of an X-ray free-electron laser

PubMed Central

Schulz, S.; Grguraš, I.; Behrens, C.; Bromberger, H.; Costello, J. T.; Czwalinna, M. K.; Felber, M.; Hoffmann, M. C.; Ilchen, M.; Liu, H. Y.; Mazza, T.; Meyer, M.; Pfeiffer, S.; Prędki, P.; Schefer, S.; Schmidt, C.; Wegner, U.; Schlarb, H.; Cavalieri, A. L.

2015-01-01

Many advanced applications of X-ray free-electron lasers require pulse durations and time resolutions of only a few femtoseconds. To generate these pulses and to apply them in time-resolved experiments, synchronization techniques that can simultaneously lock all independent components, including all accelerator modules and all external optical lasers, to better than the delivered free-electron laser pulse duration, are needed. Here we achieve all-optical synchronization at the soft X-ray free-electron laser FLASH and demonstrate facility-wide timing to better than 30 fs r.m.s. for 90 fs X-ray photon pulses. Crucially, our analysis indicates that the performance of this optical synchronization is limited primarily by the free-electron laser pulse duration, and should naturally scale to the sub-10 femtosecond level with shorter X-ray pulses. PMID:25600823

Solid-state characterization of nevirapine.

PubMed

Sarkar, Mahua; Perumal, O P; Panchagnula, R

2008-09-01

The purpose of this investigation is to characterize nevirapine from commercial samples and samples crystallized from different solvents under various conditions. The solid-state behavior of nevirapine samples was investigated using a variety of complementary techniques such as microscopy (optical, polarized, hot stage microscopy), differential scanning calorimeter, thermogravimetric analysis, Fourier transform infrared spectroscopy and powder X-ray diffractometry. The commercial samples of nevirapine had the same polymorphic crystalline form with an anhedral crystal habit. Intrinsic dissolution of nevirapine was similar for both the commercial batches. Powder dissolution showed pH dependency, with maximum dissolution in acidic pH and there was no significant effect of particle size. The samples recrystallized from different solvent systems with varying polarity yielded different crystal habits. Stirring and degrees of supersaturation influenced the size and shape of the crystals. The recrystallized samples did not produce any new polymorphic form, but weak solvates with varying crystal habit were produced. Recrystallized samples showed differences in the x-ray diffractograms. However, all the samples had the same internal crystal lattice as revealed from their similar melting points and heat of fusion. The intrinsic dissolution rate of recrystallized samples was lower than the commercial sample. It was found that the compression pressure resulted in desolvation and partial conversion of the crystal form. After compression, the recrystallized samples showed similar x-ray diffractograms to the commercial sample. Amorphous form showed slightly higher aqueous solubility than the commercial crystalline form.

Using DTSA-II to simulate and interpret energy dispersive spectra from particles.

PubMed

Ritchie, Nicholas W M

2010-06-01

A high quality X-ray spectrum image of a 3.3 mum diameter sphere of K411 glass resting on a copper substrate was collected at 25 keV. The same sample configuration was modeled using the NISTMonte Monte Carlo simulation of electron and X-ray transport as is integrated into the quantitative X-ray microanalysis software package DTSA-II. The distribution of measured and simulated X-ray intensity compare favorably for all the major lines present in the spectra. The simulation is further examined to investigate the influence of angle-of-incidence, sample thickness, and sample diameter on the generated and measured X-ray intensity. The distribution of generated X-rays is seen to deviate significantly from a naive model which assumes that the distribution of generated X-rays is similar to bulk within the volume they share in common. It is demonstrated that the angle at which the electron beam strikes the sample has nonnegligible consequences. It is also demonstrated that within the volume that the bulk and particle share in common that electrons, which have exited and later reentered the particle volume, generate a significant fraction of the X-rays. Any general model of X-ray generation in particles must take into account the lateral spread of the scattered electron beam.

Two-colour hard X-ray free-electron laser with wide tunability.

PubMed

Hara, Toru; Inubushi, Yuichi; Katayama, Tetsuo; Sato, Takahiro; Tanaka, Hitoshi; Tanaka, Takashi; Togashi, Tadashi; Togawa, Kazuaki; Tono, Kensuke; Yabashi, Makina; Ishikawa, Tetsuya

2013-01-01

Ultrabrilliant, femtosecond X-ray pulses from X-ray free-electron lasers (XFELs) have promoted the investigation of exotic interactions between intense X-rays and matters, and the observation of minute targets with high spatio-temporal resolution. Although a single X-ray beam has been utilized for these experiments, the use of multiple beams with flexible and optimum beam parameters should drastically enhance the capability and potentiality of XFELs. Here we show a new light source of a two-colour double-pulse (TCDP) XFEL in hard X-rays using variable-gap undulators, which realizes a large and flexible wavelength separation of more than 30% with an ultraprecisely controlled time interval in the attosecond regime. Together with sub-10-fs pulse duration and multi-gigawatt peak powers, the TCDP scheme enables us to elucidate X-ray-induced ultrafast transitions of electronic states and structures, which will significantly contribute to the advancement of ultrafast chemistry, plasma and astronomical physics, and quantum X-ray optics.

Macromolecular structures probed by combining single-shot free-electron laser diffraction with synchrotron coherent X-ray imaging.

PubMed

Gallagher-Jones, Marcus; Bessho, Yoshitaka; Kim, Sunam; Park, Jaehyun; Kim, Sangsoo; Nam, Daewoong; Kim, Chan; Kim, Yoonhee; Noh, Do Young; Miyashita, Osamu; Tama, Florence; Joti, Yasumasa; Kameshima, Takashi; Hatsui, Takaki; Tono, Kensuke; Kohmura, Yoshiki; Yabashi, Makina; Hasnain, S Samar; Ishikawa, Tetsuya; Song, Changyong

2014-05-02

Nanostructures formed from biological macromolecular complexes utilizing the self-assembly properties of smaller building blocks such as DNA and RNA hold promise for many applications, including sensing and drug delivery. New tools are required for their structural characterization. Intense, femtosecond X-ray pulses from X-ray free-electron lasers enable single-shot imaging allowing for instantaneous views of nanostructures at ambient temperatures. When combined judiciously with synchrotron X-rays of a complimentary nature, suitable for observing steady-state features, it is possible to perform ab initio structural investigation. Here we demonstrate a successful combination of femtosecond X-ray single-shot diffraction with an X-ray free-electron laser and coherent diffraction imaging with synchrotron X-rays to provide an insight into the nanostructure formation of a biological macromolecular complex: RNA interference microsponges. This newly introduced multimodal analysis with coherent X-rays can be applied to unveil nano-scale structural motifs from functional nanomaterials or biological nanocomplexes, without requiring a priori knowledge.

Sonochemical synthesis of highly crystalline photocatalyst for industrial applications.

PubMed

Noman, Muhammad Tayyab; Militky, Jiri; Wiener, Jakub; Saskova, Jana; Ashraf, Muhammad Azeem; Jamshaid, Hafsa; Azeem, Musaddaq

2018-02-01

Highly photo active pure anatase form of TiO 2 nanoparticles with average particle size 4nm have been successfully synthesized by ultrasonic acoustic method (UAM). The effects of process variables i.e. precursors concentration and sonication time were investigated based on central composite design and response surface methodology. The characteristics of the resulting nanoparticles (RNP) were analyzed by scanning electron microscopy, dynamic light scattering, transmission electron microscopy, X-ray diffractometry and Raman spectroscopy. Photocatalytic experiments were performed with methylene blue dye which is considered as model organic pollutant in textile industry. A comparative analysis between the RNP and commercially available Degussa P25 for photocatalytic performance against dye removal efficiency was performed. The rapid removal of methylene blue in case of RNP indicates their higher photocatalytic activity than P25. Maximum dye removal efficiency 98.45% was achieved with optimal conditions i.e. TTIP conc. 10mL, EG conc. 4mL and sonication time 1h. Interestingly, no significant difference was found in the photocatalytic performance of RNP after calcination. Moreover, self-cleaning efficiency of RNP deposited on cotton was evaluated in RGB color space. The obtained results indicate the significant impact of ultrasonic irradiations on the photocatalytic performance of pure anatase form than any other hybrid type of TiO 2 nanoparticles. Copyright © 2017 Elsevier B.V. All rights reserved.

Spectroellipsometric studies of sol-gel derived Sr0.6Ba0.4Nb2O6 films

NASA Astrophysics Data System (ADS)

Ho, Melanie M. T.; Tang, T. B.; Mak, C. L.; Pang, G. K. H.; Chan, K. Y.; Wong, K. H.

2006-10-01

Sr0.6Ba0.4Nb2O6 (SBN) films have been fabricated on (001)Si substrates by a sol-gel technique. The annealing process was carried out in air at various temperatures ranging from 200to700°C. Studies using x-ray diffractometry, high resolution transmission electron microscopy, and scanning electron microscopy showed that polycrystalline films, with a grain size of about 100nm, were obtained only for annealing temperatures ⩾600°C. The optical properties of these sol-gel derived SBN films were studied by spectroscopic ellipsometry (SE). In the analysis of the measured SE spectra, a triple-layer Lorentz model has been developed and used to deduce the optical properties of the SBN films. Our systematic SE measurements revealed that the refractive indices of the SBN films increase with the annealing temperature. This increase is more pronounced at around the crystallization temperature, i.e., between 500 and 600°C. The extinction coefficients of the films also exhibit a similar trend, showing a zero value for amorphous films and larger values for films annealed at above 600°C. Our results demonstrate that while crystallization helps to raise the refractive index of the film due to film densification, it also promotes scattering by grain boundary, resulting in a larger extinction coefficient.

Water treatment with exceptional virus inactivation using activated carbon modified with silver (Ag) and copper oxide (CuO) nanoparticles.

PubMed

Shimabuku, Quelen Letícia; Arakawa, Flávia Sayuri; Fernandes Silva, Marcela; Ferri Coldebella, Priscila; Ueda-Nakamura, Tânia; Fagundes-Klen, Márcia Regina; Bergamasco, Rosangela

2017-08-01

Continuous flow experiments (450 mL min -1 ) were performed in household filter in order to investigate the removal and/or inactivation of T4 bacteriophage, using granular activated carbon (GAC) modified with silver and/or copper oxide nanoparticles at different concentrations. GAC and modified GAC were characterized by X-ray diffractometry, specific surface area, pore size and volume, pore average diameter, scanning electron microscopy, transmission electron microscopy, zeta potential and atomic absorption spectroscopy. The antiviral activity of the produced porous media was evaluated by passing suspensions of T4 bacteriophage (∼10 5  UFP/mL) through filters. The filtered water was analyzed for the presence of the bacteriophage and the release of silver and copper oxide. The porous media containing silver and copper oxide nanoparticles showed high inactivation capacity, even reaching reductions higher than 3 log. GAC6 (GAC/Ag0.5%Cu1.0%) was effective in the bacteriophage inactivation, reaching 5.53 log reduction. The levels of silver and copper released in filtered water were below the recommended limits (100 ppb for silver and 1000 ppb for copper) in drinking water. From this study, it is possible to conclude that activated carbon modified with silver and copper oxide nanoparticles can be used as a filter for virus removal in the treatment of drinking water.

The X-ray Detectability of Electron Beams Escaping from the Sun

NASA Astrophysics Data System (ADS)

Saint-Hilaire, Pascal; Krucker, Säm; Christe, Steven; Lin, Robert P.

2009-05-01

We study the detectability and characterization of electron beams as they leave their acceleration site in the low corona toward interplanetary space through their nonthermal X-ray bremsstrahlung emission. We demonstrate that the largest interplanetary electron beams (gsim1035 electrons above 10 keV) can be detected in X-rays with current and future instrumentation, such as RHESSI or the X-Ray Telescope (XRT) onboard Hinode. We make a list of optimal observing conditions and beam characteristics. Amongst others, good imaging (as opposed to mere localization or detection in spatially integrated data) is required for proper characterization, putting the requirement on the number of escaping electrons (above 10 keV) to gsim3 × 1036 for RHESSI, gsim3 × 1035 for Hinode/XRT, and gsim1033 electrons for the FOXSI sounding rocket scheduled to fly in 2011. Moreover, we have found that simple modeling hints at the possibility that coronal soft X-ray jets could be the result of local heating by propagating electron beams.

Towards simultaneous measurements of electronic and structural properties in ultra-fast x-ray free electron laser absorption spectroscopy experiments

NASA Astrophysics Data System (ADS)

Gaudin, J.; Fourment, C.; Cho, B. I.; Engelhorn, K.; Galtier, E.; Harmand, M.; Leguay, P. M.; Lee, H. J.; Nagler, B.; Nakatsutsumi, M.; Ozkan, C.; Störmer, M.; Toleikis, S.; Tschentscher, Th; Heimann, P. A.; Dorchies, F.

2014-04-01

The rapidly growing ultrafast science with X-ray lasers unveils atomic scale processes with unprecedented time resolution bringing the so called ``molecular movie'' within reach. X-ray absorption spectroscopy is one of the most powerful x-ray techniques providing both local atomic order and electronic structure when coupled with ad-hoc theory. Collecting absorption spectra within few x-ray pulses is possible only in a dispersive setup. We demonstrate ultrafast time-resolved measurements of the LIII-edge x-ray absorption near-edge spectra of irreversibly laser excited Molybdenum using an average of only few x-ray pulses with a signal to noise ratio limited only by the saturation level of the detector. The simplicity of the experimental set-up makes this technique versatile and applicable for a wide range of pump-probe experiments, particularly in the case of non-reversible processes.

Towards simultaneous measurements of electronic and structural properties in ultra-fast x-ray free electron laser absorption spectroscopy experiments

PubMed Central

Gaudin, J.; Fourment, C.; Cho, B. I.; Engelhorn, K.; Galtier, E.; Harmand, M.; Leguay, P. M.; Lee, H. J.; Nagler, B.; Nakatsutsumi, M.; Ozkan, C.; Störmer, M.; Toleikis, S.; Tschentscher, Th; Heimann, P. A.; Dorchies, F.

2014-01-01

The rapidly growing ultrafast science with X-ray lasers unveils atomic scale processes with unprecedented time resolution bringing the so called “molecular movie” within reach. X-ray absorption spectroscopy is one of the most powerful x-ray techniques providing both local atomic order and electronic structure when coupled with ad-hoc theory. Collecting absorption spectra within few x-ray pulses is possible only in a dispersive setup. We demonstrate ultrafast time-resolved measurements of the LIII-edge x-ray absorption near-edge spectra of irreversibly laser excited Molybdenum using an average of only few x-ray pulses with a signal to noise ratio limited only by the saturation level of the detector. The simplicity of the experimental set-up makes this technique versatile and applicable for a wide range of pump-probe experiments, particularly in the case of non-reversible processes. PMID:24740172

Towards simultaneous measurements of electronic and structural properties in ultra-fast x-ray free electron laser absorption spectroscopy experiments

DOE PAGES

Gaudin, J.; Fourment, C.; Cho, B. I.; ...

2014-04-17

The rapidly growing ultrafast science with X-ray lasers unveils atomic scale processes with unprecedented time resolution bringing the so called “molecular movie” within reach. X-ray absorption spectroscopy is one of the most powerful x-ray techniques providing both local atomic order and electronic structure when coupled with ad-hoc theory. Collecting absorption spectra within few x-ray pulses is possible only in a dispersive setup. We demonstrate ultrafast time-resolved measurements of the LIII-edge x-ray absorption near-edge spectra of irreversibly laser excited Molybdenum using an average of only few x-ray pulses with a signal to noise ratio limited only by the saturation level ofmore » the detector. The simplicity of the experimental set-up makes this technique versatile and applicable for a wide range of pump-probe experiments, particularly in the case of non-reversible processes.« less

Combining experiment and optical simulation in coherent X-ray nanobeam characterization of Si/SiGe semiconductor heterostructures

DOE PAGES

Tilka, J. A.; Park, J.; Ahn, Y.; ...

2016-07-06

Here, the highly coherent and tightly focused x-ray beams produced by hard x-ray light sources enable the nanoscale characterization of the structure of electronic materials but are accompanied by significant challenges in the interpretation of diffraction and scattering patterns. X-ray nanobeams exhibit optical coherence combined with a large angular divergence introduced by the x-ray focusing optics. The scattering of nanofocused x-ray beams from intricate semiconductor heterostructures produces a complex distribution of scattered intensity. We report here an extension of coherent xray optical simulations of convergent x-ray beam diffraction patterns to arbitrary x-ray incident angles to allow the nanobeam diffraction patternsmore » of complex heterostructures to be simulated faithfully. These methods are used to extract the misorientation of lattice planes and the strain of individual layers from synchrotron x-ray nanobeam diffraction patterns of Si/SiGe heterostructures relevant to applications in quantum electronic devices. The systematic interpretation of nanobeam diffraction patterns from semiconductor heterostructures presents a new opportunity in characterizing and ultimately designing electronic materials.« less

One-Step Synthesis of Silver Nanoparticles on Polydopamine-Coated Sericin/Polyvinyl Alcohol Composite Films for Potential Antimicrobial Applications.

PubMed

Cai, Rui; Tao, Gang; He, Huawei; Song, Kai; Zuo, Hua; Jiang, Wenchao; Wang, Yejing

2017-04-30

Silk sericin has great potential as a biomaterial for biomedical applications due to its good hydrophilicity, reactivity, and biodegradability. To develop multifunctional sericin materials for potential antibacterial application, a one-step synthesis method for preparing silver nanoparticles (AgNPs) modified on polydopamine-coated sericin/polyvinyl alcohol (PVA) composite films was developed. Polydopamine (PDA) acted as both metal ion chelating and reducing agent to synthesize AgNPs in situ on the sericin/PVA composite film. Scanning electron microscopy and energy dispersive spectroscopy analysis revealed that polydopamine could effectively facilitate the high-density growth of AgNPs as a 3-D matrix. X-ray diffractometry studies suggested the synthesized AgNPs formed good face-centered cubic crystalline structures. Contact angle measurement and mechanical test indicated AgNPs modified PDA-sericin/PVA composite film had good hydrophilicity and mechanical property. The bacterial growth curve and inhibition zone assays showed the AgNPs modified PDA-sericin/PVA composite film had long-term antibacterial activities. This work develops a new method for the preparation of AgNPs modified PDA-sericin/PVA film with good hydrophilicity, mechanical performance and antibacterial activities for the potential antimicrobial application in biomedicine.

Molecular inclusion complex of curcumin-β-cyclodextrin nanoparticle to enhance curcumin skin permeability from hydrophilic matrix gel.

PubMed

Rachmawati, Heni; Edityaningrum, Citra Ariani; Mauludin, Rachmat

2013-12-01

Curcumin (CUR) has various pharmacological effects, but its extensive first-pass metabolism and short elimination half-life limit its bioavailability. Therefore, transdermal application has become a potential alternative to delivery CUR. To increase CUR solubility for the development of a transparent homogenous gel and also enhance the permeation rate of CUR into the skin, β-cyclodextrin-curcumin nanoparticle complex (BCD-CUR-N) was developed. CUR encapsulation efficiency was increased by raising the percentage of CUR to BCD up to 20%. The mean particle size of the best CUR loading formula was 156 nm. All evaluation data using infrared spectroscopy, Raman spectroscopy, powder X-ray diffractometry, differential thermal analysis and scanning electron microscopy confirmed the successful formation of the inclusion complex. BCD-CUR-N increased the CUR dissolution rate of 10-fold (p < 0.01). In addition, the improvement of CUR permeability acrossed skin model tissue was observed in gel containing the BCD-CUR-N and was about 1.8-fold when compared with the free CUR gel (p < 0.01). Overall, CUR in the form of the BCD-CUR-N improved the solubility further on the penetration of CUR.

Dissolution enhancement of tadalafil by liquisolid technique.

PubMed

Lu, Mei; Xing, Haonan; Yang, Tianzhi; Yu, Jiankun; Yang, Zhen; Sun, Yanping; Ding, Pingtian

2017-02-01

This study aimed to enhance the dissolution of tadalafil, a poorly water-soluble drug by applying liquisolid technique. The effects of two critical formulation variables, namely drug concentration (17.5% and 35%, w/w) and excipients ratio (10, 15 and 20) on dissolution rates were investigated. Pre-compression tests, including particle size distribution, flowability determination, Fourier transform infrared (FT-IR), differential scanning calorimetry (DSC), X-ray diffractometry (XRD) and scanning electron microscopy (SEM), were carried out to investigate the mechanism of dissolution enhancement. Tadalafil liquisolid tablets were prepared and their quality control tests, dissolution study, contact angle measurement, Raman mapping, and storage stability test were performed. The results suggested that all the liquisolid tablets exhibited significantly higher dissolution rates than the conventional tablets and pure tadalafil. FT-IR spectrum reflected no drug-excipient interactions. DSC and XRD studies indicated reduction in crystallinity of tadalafil, which was further confirmed by SEM and Raman mapping outcomes. The contact angle measurement demonstrated obvious increase in wetting property. Taken together, the reduction of particle size and crystallinity, and the improvement of wettability were the main mechanisms for the enhanced dissolution rate. No significant changes were observed in drug crystallinity and dissolution behavior after storage based on XRD, SEM and dissolution results.

Growth of ferroelectric Ba{sub 0.8}Sr{sub 0.2}TiO{sub 3} epitaxial films by ultraviolet pulsed laser irradiation of chemical solution derived precursor layers

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

Queraltó, A.; Pérez del Pino, A., E-mail: aperez@icmab.es; Mata, M. de la

2015-06-29

Highly crystalline epitaxial Ba{sub 0.8}Sr{sub 0.2}TiO{sub 3} (BST) thin-films are grown on (001)-oriented LaNiO{sub 3}-buffered LaAlO{sub 3} substrates by pulsed laser irradiation of solution derived barium-zirconium-titanium precursor layers using a UV Nd:YAG laser source at atmospheric conditions. The structural analyses of the obtained films, studied by X-ray diffractometry and transmission electron microscopy, demonstrate that laser processing allows the growth of tens of nm-thick BST epitaxial films with crystalline structure similar to that of films obtained through conventional thermal annealing methods. However, the fast pulsed nature of the laser employed leads to crystallization kinetic evolution orders of magnitude faster than inmore » thermal treatments. The combination of specific photothermal and photochemical mechanisms is the main responsible for the ultrafast epitaxial laser-induced crystallization. Piezoresponse microscopy measurements demonstrate equivalent ferroelectric behavior in laser and thermally annealed films, being the piezoelectric constant ∼25 pm V{sup −1}.« less

Synthesis and surface properties of submicron barium sulfate particles

NASA Astrophysics Data System (ADS)

Zhang, Ming; Zhang, Bao; Li, Xinhai; Yin, Zhoulan; Guo, Xueyi

2011-10-01

Barium sulfate particles were synthesized in the presence of EDTA at room temperature. X-ray diffractometry (XRD), Fourier transform infrared resonance (FTIR) and scanning electron microscopy (SEM) were used to characterize the structure and morphology of BaSO 4 particles. The effect of the preparation parameters on the particle size distribution and morphology was investigated. The conditional formation constants of Ba-EDTA at different pH values were calculated. The results show that the size and morphology of BaSO 4 particles can be effectively controlled by adding EDTA in the precipitation process. Among all the operation conditions, the pH value has significant effect on the particle size. The obtained barium sulfate particles are spherical and well dispersed at pH = 9-10. Zeta potentials of BaSO 4 were measured at different pH. The isoelectric point (IEP) of barium sulfate colloid appears at pH 6.92. The model of the solid-solution interface at a particle of BaSO 4 was presented. The FTIR result indicates that the surface of the prepared BaSO 4 absorbs the functional groups of EDTA, which lower the IEP of the barium sulfate particles.

Effect of Ca addition on the damping capacity of Mg-Al-Zn casting alloys

NASA Astrophysics Data System (ADS)

Jun, Joong-Hwan; Moon, Jung-Hyun

2015-07-01

The influences of Ca addition on the microstructures and damping capacities of AZ91-(0˜2)%Ca casting alloys were investigated, on the basis of the results of X-ray diffractometry, optical microscopy, scanning electron microscopy and vibration tests in a single cantilever mode. The amount of intermetallic compounds decreased with increasing Ca content up to 0.5%, above which it increased; the average cell size showed the opposite tendency. All alloys exhibited similar damping levels in the strain-amplitude independent region. Considering the very low solubility of Ca in the matrix, and that most of the Ca elements are consumed by the formation of the Al2Ca phase and incorporation into the Mg17Al12 phase, this would be ascribed to the almost identical concentrations of Ca solutes distributed in the matrix. In the strain-amplitude dependent region, however, the AZ91-0.5%Ca alloy possessed the maximum damping capacity. From the viewpoint of microstructural evolution with Ca addition, the number density of compound particles is considered to be the principal factor affecting the damping behavior in the strain-amplitude dependent region.

Formation and characterization of calcium orthophosphates in the presence of two different acidic macromolecules

NASA Astrophysics Data System (ADS)

Pelin, Irina M.; Maier, Vasilica; Suflet, Dana M.; Popescu, Irina; Darie-Nita, Raluca N.; Aflori, Magdalena; Butnaru, Maria

2017-10-01

The synthetic nanocrystalline calcium orthophosphates have a notable bioactivity due to the chemical similarity with biological apatite from calcified tissues. In mineralized tissues, the highly ordered structures come from organized assemblies of biomacromolecules and inorganic nanoparticles. One of the purposes of this work was to study the effect of two types of acidic macromolecules: atelocollagen and phosphorylated curdlan onto calcium orthophosphates formation after 30 days of maturation at 2 ± 2 °C. The resulted samples after a long aging time, either calcium orthophosphates or composites, were first investigated by FT-IR spectroscopy and X-ray diffractometry and the results indicated that precipitated hydroxyapatite with low crystallinity was obtained when the synthesis was performed in the presence of phosphorylated curdlan. The macromolecules influenced the morphology of the particles as shown by scanning and transmission electron microscopy. The presence of macromolecules as demonstrated by thermal investigation also influenced the rheological properties of the samples. The second purpose of the work was to evaluate the cytotoxicity of the samples using the MTT assay, and the results revealed very good cells viability. The preliminary results are encouraging regarding the use of these materials for further tests in order to develop injectable bone substitutes.

Microstructure and corrosion resistance of TC2 Ti alloy by laser cladding with Ti/TiC/TiB2 powders

NASA Astrophysics Data System (ADS)

Diao, Yunhua; Zhang, Kemin

2015-10-01

In the present work, a TiC/TiB2 composite coating was produced onto a TC2 Ti alloy by laser cladding with Ti/TiC/TiB2 powders. The surface microstructure, phase components and compositions were characterized with methods of optical microscopy (OM), scanning electron microscopy (SEM), X-ray diffractometry (XRD), and energy dispersive spectrometry (EDS). The cladding layer is consisted of Ti, TiC and TiB2. And the surface microhardness was measured. After laser cladding, a maximum hardness of 1100 HV is achieved in the laser cladding surface layer, which is more three times higher than that of the TC2 substrate (∼300 HV). Due to the formation of TiC and TiB2 intermetallic compounds in the alloyed region and grain refinement, the microhardness of coating is higher than TC2 Ti alloy. In this paper, the corrosion property of matrix material and treated samples were both measured in NaCl (3.5 wt%) aqueous solution. From the result we can see that the laser cladding specimens' corrosion property is clearly becoming better than that of the substrate.

Structural and optical properties of low temperature grown AlN films on sapphire using helicon sputtering system

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

Chen, Meei-Ru; Chen, Hou-Guang; Kao, Hui-Ling, E-mail: hlkao@cycu.edu.tw

2015-05-15

AlN thin films have been deposited directly on c-plane sapphire substrates at low temperatures by a helicon sputtering system. The structural quality of AlN epitaxial films was characterized by x-ray diffractometry and transmission electron microscopy. The films exhibit smooth surface with root-mean-square roughness as small as 0.7 nm evaluated by atomic force microscope. The optical transmittance spectra show a steep absorption edge at the wavelength of 200 nm and a high transmittance of over 80% in the visible range. The band-edge transition (6.30 eV) of AlN film was observed in the cathodoluminescence spectrum recorded at 11 K. The spectral response of metal–semiconductor–metal photodetectors constructedmore » with AlN/sapphire reveals the peak responsivity at 200 nm and a UV/visible rejection ratio of about two orders of magnitude. The results of this low temperature deposition suggest the feasibility of the epitaxial growth of AlN on sapphire substrates and the incorporation of the AlN films in the surface acoustic wave devices and the optical devices at deep ultraviolet region.« less

Structural characterization and bioavailability of ternary nanoparticles consisting of amylose, α-linoleic acid and β-lactoglobulin complexed with naringin.

PubMed

Feng, Tao; Wang, Ke; Liu, Fangfang; Ye, Ran; Zhu, Xiao; Zhuang, Haining; Xu, Zhimin

2017-06-01

Naringin is a bioflavonoid that is rich in citrus plants and possesses enormous health benefits. However, the use of naringin as a nutraceutical is significantly limited by its low bioavailability. In this study, a novel water-soluble ternary nanoparticle material consisting of amylose, α-linoleic acid and β-lactoglobulin was developed to encapsulate naringin to improve its bioavailability. The physicochemical characteristics of the ternary nanoparticle-naringin inclusion complex were analysed by ultraviolet-visible spectroscopy (UV), Fourier transform infrared spectroscopy (FT-IR), differential scanning calorimetry (DSC), high-resolution transmission electron microscopy (TEM), X-ray diffractometry (XRD) and particle size distribution. The results confirmed the formation of the ternary nanoparticle-naringin inclusion complex. The encapsulation efficiency (EE) and loading content (LC) of the ternary nanoparticle-naringin inclusion complex were 78.73±4.17% and 14.51±3.43%, respectively. In addition, the results of the ternary nanoparticle-naringin inclusion complex in simulated gastric fluid (SGF) and simulated intestinal fluid (SIF) demonstrated that naringin can be gradually released from the complex. In conclusion, ternary nanoparticles are considered promising carriers to effectively improve the bioavailability of naringin. Copyright © 2017 Elsevier B.V. All rights reserved.

Surface improvement and biocompatibility of TiAl 24Nb 10 intermetallic alloy using rf plasma nitriding

NASA Astrophysics Data System (ADS)

Abd El-Rahman, A. M.; Maitz, M. F.; Kassem, M. A.; El-Hossary, F. M.; Prokert, F.; Reuther, H.; Pham, M. T.; Richter, E.

2007-09-01

The present work describes the surface improvement and biocompatibility of TiAl 24Nb 10 intermetallic alloy using rf plasma nitriding. The nitriding process was carried out at different plasma power from 400 W to 650 W where the other plasma conditions were fixed. Grazing incidence X-ray diffractometry (GIXRD), Auger electron spectroscopy (AES), tribometer and a nanohardness tester were employed to characterize the nitrided layer. Further potentiodynamic polarization method was used to describe the corrosion behavior of the un-nitrided and nitrided alloy. It has been found that the Vickers hardness (HV) and corrosion resistance values of the nitrided layers increase with increasing plasma power while the wear rates of the nitrided layers reduce by two orders of magnitude as compared to those of the un-nitrided layer. This improvement in surface properties of the intermetallic alloy is due to formation of a thin modified layer which is composed of titanium nitride in the alloy surface. Moreover, all modified layers were tested for their sustainability as a biocompatible material. Concerning the application area of biocompatibility, the present treated alloy show good surface properties especially for the nitrided alloy at low plasma power of 400 W.

LiMn2O4–yBryNanoparticles Synthesized by a Room Temperature Solid-State Coordination Method

PubMed Central

2009-01-01

LiMn2O4–yBrynanoparticles were synthesized successfully for the first time by a room temperature solid-state coordination method. X-ray diffractometry patterns indicated that the LiMn2O4–yBrypowders were well-crystallized pure spinel phase. Transmission electron microscopy images showed that the LiMn2O4–yBrypowders consisted of small and uniform nanosized particles. Synthesis conditions such as the calcination temperature and the content of Br−were investigated to optimize the ideal condition for preparing LiMn2O4–yBrywith the best electrochemical performances. The optimized synthesis condition was found in this work; the calcination temperature is 800 °C and the content of Br−is 0.05. The initial discharge capacity of LiMn2O3.95Br0.05obtained from the optimized synthesis condition was 134 mAh/g, which is far higher than that of pure LiMn2O4, indicating introduction of Br−in LiMn2O4is quite effective in improving the initial discharge capacity. PMID:20628635

Synthesis and characterization of ferrite-semiconductor nano composite for photocatalytic degradation of aqueous nitrobenzene solution

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

Modi, K. B.; Kathad, C. R.; Raval, P. Y.

2016-05-06

Nanoparticles of semiconductor TiO{sub 2}, zinc ferrite (ZnFe{sub 2}O{sub 4}) and ZnFe{sub 2}O{sub 4}-TiO{sub 2} composite, were synthesized by auto combustion route. Subsequent characterization of synthesized photocatalysts was carried out by X-ray powder diffractometry, transmission electron microscopy, UV-Vis-Diffuse Reflectance Spectroscopy to study the structural and textural properties. The specific surface area, pore diameter and pore volume of synthesized materials were investigated by N{sub 2} adsorption analysis while the presence of TiO{sub 2} in the composite material was verified by infrared spectral analysis. The photocatalytic activity of synthesized photocatalysts was evaluated by degradation of nitrobenzene (NB) in aqueous medium under irradiationmore » of ultraviolet light. The result revealed that 77, 73 and 70% of NB was degraded using TiO{sub 2}, ZnFe{sub 2}O{sub 4} and ZnFe{sub 2}O{sub 4}-TiO{sub 2} photocatalysts after 4h in the presence of UV irradiation. The composite photocatalyst was found easy to separate from the treated solution.« less

Photocatalytic degradation of an azo textile dye (C.I. Reactive Red 195 (3BF)) in aqueous solution over copper cobaltite nanocomposite coated on glass by Doctor Blade method.

PubMed

Habibi, Mohammad Hossein; Rezvani, Zoya

2015-08-05

The degradation of C.I. Reactive Red 195 (3BF) in aqueous solution using copper cobaltite nanocomposite coated on glass by Doctor Blade method was studied. Structural, optical and morphological properties of nanocomposite coatings were characterized by X-ray powder diffractometry (XRD), diffuse reflectance spectroscopy (DRS) and field emission scanning electron microscopy (FESEM). The nanoparticles exhibit a particle size of 31 nm, showing a good nanoscale crystalline morphology. The photocatalytic activity of copper cobaltite nanocomposite coated on glass was studied by performing the photocatalytic degradation of 3BF at different irradiation time. The effect of irradiation time on the degradation of 3BF was studied and the results showed that more than 85% of the 3BF was degraded in 45 min of irradiation. The pseudo-first-order kinetic models were used and the rate constants were evaluated with pseudo first order rate constants of 4.10 × 10(-2) min(-1). The main advantage of the photocatalyst coated on glass overcomes the difficulties in separation and recycle of photocatalyst suspensions. Copyright © 2015 Elsevier B.V. All rights reserved.

Piroxicam/2-hydroxypropyl-beta-cyclodextrin inclusion complex prepared by a new fluid-bed coating technique.

PubMed

Zhang, Xingwang; Wu, Danni; Lai, Jie; Lu, Yi; Yin, Zongning; Wu, Wei

2009-02-01

This work was aimed at investigating the feasibility of fluid-bed coating as a new method to prepare cyclodextrin inclusion complex. The inclusion complex of the model drug piroxicam (PIX) and 2-hydroxypropyl-beta-cyclodextrin (HPCD) in aqueous ethanol solution was sprayed and deposited onto the surface of the pellet substrate upon removal of the solvent. The coating process was fluent with high coating efficiency. Scanning electron microscopy revealed a coarse pellet surface, and a loosely packed coating structure. Significantly enhanced dissolution, over 90% at 5 min, was observed at stoichiometric PIX/HPCD molar ratio (1/1) and at a ratio with excessive HPCD (1/2). Differential scanning calorimetry and powder X-ray diffractometry confirmed absence of crystallinity of PIX at PIX/HPCD molar ratio of 1/1 and 1/2. Fourier transform-infrared spectrometry and Raman spectrometry revealed interaction between PIX and HPCD adding evidence on inclusion of PIX moieties into HPCD cavities. Solid-state (13)C NMR spectrometry indicated possible inclusion of PIX through the pyridine ring. It is concluded that fluid-bed coating has potential to be used as a new technique to prepare cyclodextrin inclusion complex.

Diffusive transport of energetic electrons in the solar corona: X-ray and radio diagnostics

NASA Astrophysics Data System (ADS)

Musset, S.; Kontar, E. P.; Vilmer, N.

2018-02-01

Context. Imaging spectroscopy in X-rays with RHESSI provides the possibility to investigate the spatial evolution of X-ray emitting electron distribution and therefore, to study transport effects on energetic electrons during solar flares. Aims: We study the energy dependence of the scattering mean free path of energetic electrons in the solar corona. Methods: We used imaging spectroscopy with RHESSI to study the evolution of energetic electrons distribution in various parts of the magnetic loop during the 2004 May 21 flare. We compared these observations with the radio observations of the gyrosynchrotron radiation of the same flare and with the predictions of a diffusive transport model. Results: X-ray analysis shows a trapping of energetic electrons in the corona and a spectral hardening of the energetic electron distribution between the top of the loop and the footpoints. Coronal trapping of electrons is stronger for radio-emitting electrons than for X-ray-emitting electrons. These observations can be explained by a diffusive transport model. Conclusions: We show that the combination of X-ray and radio diagnostics is a powerful tool to study electron transport in the solar corona in different energy domains. We show that the diffusive transport model can explain our observations, and in the range 25-500 keV, the scattering mean free path of electrons decreases with electron energy. We can estimate for the first time the scattering mean free path dependence on energy in the corona.

Liquid sample delivery techniques for serial femtosecond crystallography

PubMed Central

Weierstall, Uwe

2014-01-01

X-ray free-electron lasers overcome the problem of radiation damage in protein crystallography and allow structure determination from micro- and nanocrystals at room temperature. To ensure that consecutive X-ray pulses do not probe previously exposed crystals, the sample needs to be replaced with the X-ray repetition rate, which ranges from 120 Hz at warm linac-based free-electron lasers to 1 MHz at superconducting linacs. Liquid injectors are therefore an essential part of a serial femtosecond crystallography experiment at an X-ray free-electron laser. Here, we compare different techniques of injecting microcrystals in solution into the pulsed X-ray beam in vacuum. Sample waste due to mismatch of the liquid flow rate to the X-ray repetition rate can be addressed through various techniques. PMID:24914163

Upgrading pyrolytic residue from waste tires to commercial carbon black.

PubMed

Zhang, Xue; Li, Hengxiang; Cao, Qing; Jin, Li'e; Wang, Fumeng

2018-05-01

The managing and recycling of waste tires has become a worldwide environmental challenge. Among the different disposal methods for waste tires, pyrolysis is regarded as a promising route. How to effectively enhance the added value of pyrolytic residue (PR) from waste tires is a matter of great concern. In this study, the PRs were treated with hydrochloric and hydrofluoric acids in turn under ultrasonic waves. The removal efficiency for the ash and sulfur was investigated. The pyrolytic carbon black (PCB) obtained after treating PR with acids was analyzed by X-ray fluorescence spectrophotometry, Fourier transform infrared spectrometry, X-ray diffractometry, laser Raman spectrometry, scanning electron microscopy, thermogravimetric (TG) analysis, and physisorption apparatus. The properties of PCB were compared with those of commercial carbon black (CCB) N326 and N339. Results showed PRs from waste tires were mainly composed of carbon, sulfur, and ash. The carbon in PCB was mainly from the CCB added during tire manufacture rather than from the pyrolysis of pure rubbers. The removal percentages for the ash and sulfur of PR are 98.33% (from 13.98 wt % down to 0.24 wt %) and 70.16% (from 1.81 wt % down to 0.54 wt %), respectively, in the entire process. The ash was mainly composed of metal oxides, sulfides, and silica. The surface properties, porosity, and morphology of the PCB were all close to those of N326. Therefore, PCB will be a potential alternative of N326 and reused in tire manufacture. This route successfully upgrades PR from waste tires to the high value-added CCB and greatly increases the overall efficiency of the waste tire pyrolysis industry.

Cu-TiO2 nanorods with enhanced ultraviolet- and visible-light photoactivity for bisphenol A degradation.

PubMed

Chiang, Li-Fen; Doong, Ruey-An

2014-07-30

In this study, the microwave-assisted sol-gel method and chemical reduction were used to synthesize Cu-TiO2 nanorod composites for enhanced photocatalytic degradation of bisphenol A (BPA) in the presence of UV and visible lights. The electron microscopic images showed that the Cu nanoparticles at 4.5±0.1nm were well-deposited onto the surface of TiO2 nanorods after chemical reduction of Cu ions by NaBH4. The X-ray diffractometry patterns and X-ray photoelectron spectroscopic results indicated that Cu species on the Cu-TiO2 nanorods were mainly the mixture of Cu2O and Cu(0). The Cu-TiO2 nanorods showed excellent photocatalytic activity toward BPA photodegradation under the irradiation of UV and visible lights. The pseudo-first-order rate constant (kobs) for BPA photodegradation by 7wt% Cu-TiO2 nanorods were 18.4 and 3.8 times higher than those of as-synthesized TiO2 nanorods and Degussa P25 TiO2, respectively, under the UV light irradiation. In addition, the kobs for BPA photodegradation by 7wt% Cu-TiO2 nanorods increased by a factor of 5.8 when compared with that of Degussa P25 TiO2 under the irradiation of 460±40nm visible light. Results obtained in this study clearly demonstrate the feasibility of using one-dimensional Cu-TiO2 nanorods for photocatalytic degradation of BPA and other pharmaceutical and personal care products in water and wastewater treatment plants. Copyright © 2014 Elsevier B.V. All rights reserved.

First Evidence of Epithermal Gold Occurrences in the SE Afar Rift, Republic of Djibouti

NASA Astrophysics Data System (ADS)

Moussa, Nima; Fouquet, Yves; Caminiti, Antoine Marie; Le Gall, Bernard; Rolet, Joel; Bohn, Marcel; Etoubleau, Joel; Delacourt, Christophe; Jalludin, Mohamed

2010-05-01

The Republic of Djibouti, located at the SE part of the Afar volcanic Triangle, is characterized by intense tectonic and bimodal volcanic activity, and is emplaced over an earlier magmatic rift system, as old as 25-30 Ma. Each magmatic event is accompanied by hydrothermal activity. Few works have been so far published on hydrothermal mineralization in the Afar area. Mineralization generally occur as veins and are mainly associated with acidic volcanic intrusions along the fractures at the edges of grabens established during the last 4 Ma. Eighty samples from hydrothermal quartz ± carbonate veins and breccias were studied on 9 different sites representative of 4 main volcanic events ranging in age from early Miocene up to Present. Gold was found in excess of 200 ppb in 30% of the samples. Mineralogical analyses based on optical reflected light microscopy, X-Ray diffractometry, X-Ray fluorescence, inductively coupled plasma mass spectroscopy and electron microprobe, led us to identify two types of gold mineralization (i) native gold, electrum, hessite and sulfides (chalcopyrite, pyrite, bornite, ± sphalerite, and galena) in massive quartz breccias and banded chalcedony, (ii) gold, electrum, hematite, magnetite, trace minerals (argentite) and adularia in banded chalcedony. Another group without gold is characterized by quartz, pyrite ± goethite. Secondary minerals are characterized by goethite, native silver and native copper. Arsenic is enriched in pyrite in samples with a high gold content. The bimodal volcanism, the occurrence of adularia, the native gold and electrum in banded silica veins, are classically observed in neutral epithermal systems. The discovery of this type of mineralization in a recent-active continental rift system supplies new insights about hydrothermal processes associated with volcanic activity in a spreading context. Keywords: Republic of Djibouti, Afar Triangle, Hydrothermal, Epithermal system, Gold

Electronic structure and optical properties of CdSxSe1-x solid solution nanostructures from X-ray absorption near edge structure, X-ray excited optical luminescence, and density functional theory investigations

NASA Astrophysics Data System (ADS)

Murphy, M. W.; Yiu, Y. M.; Ward, M. J.; Liu, L.; Hu, Y.; Zapien, J. A.; Liu, Yingkai; Sham, T. K.

2014-11-01

The electronic structure and optical properties of a series of iso-electronic and iso-structural CdSxSe1-x solid solution nanostructures have been investigated using X-ray absorption near edge structure, extended X-ray absorption fine structure, and X-ray excited optical luminescence at various absorption edges of Cd, S, and Se. It is found that the system exhibits compositions, with variable local structure in-between that of CdS and CdSe accompanied by tunable optical band gap between that of CdS and CdSe. Theoretical calculation using density functional theory has been carried out to elucidate the observations. It is also found that luminescence induced by X-ray excitation shows new optical channels not observed previously with laser excitation. The implications of these observations are discussed.

Energetic electrons, hard x-ray emission and MHD activity studies in the IR-T1 tokamak.

PubMed

Agah, K Mikaili; Ghoranneviss, M; Elahi, A Salar

2015-01-01

Determinations of plasma parameters as well as the Magnetohydrodynamics (MHD) activity, energetic electrons energy and energy confinement time are essential for future fusion reactors experiments and optimized operation. Also some of the plasma information can be deduced from these parameters, such as plasma equilibrium, stability, and MHD instabilities. In this contribution we investigated the relation between energetic electrons, hard x-ray emission and MHD activity in the IR-T1 Tokamak. For this purpose we used the magnetic diagnostics and a hard x-ray spectroscopy in IR-T1 tokamak. A hard x-ray emission is produced by collision of the runaway electrons with the plasma particles or limiters. The mean energy was calculated from the slope of the energy spectrum of hard x-ray photons.

Systematic design and three-dimensional simulation of X-ray FEL oscillator for Shanghai Coherent Light Facility

NASA Astrophysics Data System (ADS)

Li, Kai; Deng, Haixiao

2018-07-01

The Shanghai Coherent Light Facility (SCLF) is a quasi-continuous wave hard X-ray free electron laser facility, which is currently under construction. Due to the high repetition rate and high-quality electron beams, it is straightforward to consider X-ray free electron laser oscillator (XFELO) operation for the SCLF. In this paper, the main processes for XFELO design, and parameter optimization of the undulator, X-ray cavity, and electron beam are described. A three-dimensional X-ray crystal Bragg diffraction code, named BRIGHT, was introduced for the first time, which can be combined with the GENESIS and OPC codes for the numerical simulations of the XFELO. The performance of the XFELO of the SCLF is investigated and optimized by theoretical analysis and numerical simulation.

Development of a simulation method for dynamics of electrons ejected from DNA molecules irradiated with X-rays.

PubMed

Kai, Takeshi; Higuchi, Mariko; Fujii, Kentaro; Watanabe, Ritsuko; Yokoya, Akinari

2012-12-01

To develop a method for simulating the dynamics of the photoelectrons and Auger electrons ejected from DNA molecules irradiated with pulsed monochromatic X-rays. A 30-base-pair (bp) DNA molecule was used as the target model, and the X-rays were assumed to have a Gaussian-shaped time distribution. Photoionization and Auger decay were considered as the atomic processes. The atoms from which the photoelectrons or Auger electrons were emitted were specified in the DNA molecule (or DNA ion) using the Monte Carlo method, and the trajectory of each electron in the electric field formed around the positively charged DNA molecule was calculated with a Newtonian equation. The kinetics of the electrons produced by irradiation with X-rays at an intensity ranging from 1 × 10(12) to 1 × 10(16) photons/mm(2) and energies of 380 eV (below the carbon K-edge), 435 eV (above the nitrogen K-edge), and 560 eV (above the oxygen K-edge) were evaluated. It was found that at an X-ray intensity of 1 × 10(14) photons/mm(2) or less, all the produced electrons escaped from the target. However, above an X-ray intensity of 1 × 10(15) photons/mm(2) and an energy of 560 eV, some photoelectrons that were ejected from the oxygen atoms were trapped near the target DNA. A simulation method for studying the trajectories of electrons ejected from a 30-bp DNA molecule irradiated with pulsed monochromatic X-rays has been developed. The present results show that electron dynamics are strongly dependent on the charged density induced in DNA by pulsed X-ray irradiation.

A vacuum-sealed compact x-ray tube based on focused carbon nanotube field-emission electrons

NASA Astrophysics Data System (ADS)

Jeong, Jin-Woo; Kim, Jae-Woo; Kang, Jun-Tae; Choi, Sungyoul; Ahn, Seungjoon; Song, Yoon-Ho

2013-03-01

We report on a fully vacuum-sealed compact x-ray tube based on focused carbon nanotube (CNT) field-emission electrons for various radiography applications. The specially designed two-step brazing process enabled us to accomplish a good vacuum level for the stable and reliable operation of the x-ray tube without any active vacuum pump. Also, the integrated focusing electrodes in the field-emission electron gun focused electron beams from the CNT emitters onto the anode target effectively, giving a small focal spot of around 0.3 mm with a large current of above 50 mA. The active-current control through the cathode electrode of the x-ray tube led a fast digital modulation of x-ray dose with a low voltage of below 5 V. The fabricated compact x-ray tube showed a stable and reliable operation, indicating good maintenance of a vacuum level of below 5 × 10-6 Torr and the possibility of field-emission x-ray tubes in a stand-alone device without an active pumping system.

Design and characterization of electron beam focusing for X-ray generation in novel medical imaging architecturea

PubMed Central

Bogdan Neculaes, V.; Zou, Yun; Zavodszky, Peter; Inzinna, Louis; Zhang, Xi; Conway, Kenneth; Caiafa, Antonio; Frutschy, Kristopher; Waters, William; De Man, Bruno

2014-01-01

A novel electron beam focusing scheme for medical X-ray sources is described in this paper. Most vacuum based medical X-ray sources today employ a tungsten filament operated in temperature limited regime, with electrostatic focusing tabs for limited range beam optics. This paper presents the electron beam optics designed for the first distributed X-ray source in the world for Computed Tomography (CT) applications. This distributed source includes 32 electron beamlets in a common vacuum chamber, with 32 circular dispenser cathodes operated in space charge limited regime, where the initial circular beam is transformed into an elliptical beam before being collected at the anode. The electron beam optics designed and validated here are at the heart of the first Inverse Geometry CT system, with potential benefits in terms of improved image quality and dramatic X-ray dose reduction for the patient. PMID:24826066

Table-top laser-driven ultrashort electron and X-ray source: the CIBER-X source project

NASA Astrophysics Data System (ADS)

Girardeau-Montaut, Jean-Pierre; Kiraly, Bélà; Girardeau-Montaut, Claire; Leboutet, Hubert

2000-09-01

We report on the development of a new laser-driven table-top ultrashort electron and X-ray source, also called the CIBER-X source . X-ray pulses are produced by a three-step process which consists of the photoelectron emission from a thin metallic photocathode illuminated by 16 ps duration laser pulses at 213 nm. The e-gun is a standard Pierce diode electrode type, in which electrons are accelerated by a cw electric field of ˜11 MV/m up to a hole made in the anode. The photoinjector produces a train of 70-80 keV electron pulses of ˜0.5 nC and 20 A peak current at a repetition rate of 10 Hz. The electrons are then transported outside the diode along a path of 20 cm length, and are focused onto a target of thullium by magnetic fields produced by two electromagnetic coils. X-rays are then produced by the impact of electrons on the target. Simulations of geometrical, electromagnetic fields and energetic characteristics of the complete source were performed previously with the assistance of the code PIXEL1 also developed at the laboratory. Finally, experimental electron and X-ray performances of the CIBER-X source as well as its application to very low dose imagery are presented and discussed. source Compacte d' Impulsions Brèves d' Electrons et de Rayons X

The gamma-ray emitting region of the jet in Cyg X-3

NASA Astrophysics Data System (ADS)

Zdziarski, Andrzej A.; Sikora, Marek; Dubus, Guillaume; Yuan, Feng; Cerutti, Benoit; Ogorzałek, Anna

2012-04-01

We study models of the γ-ray emission of Cyg X-3 observed by Fermi. We calculate the average X-ray spectrum during the γ-ray active periods. Then, we calculate spectra from Compton scattering of a photon beam into a given direction by isotropic relativistic electrons with a power-law distribution, both based on the Klein-Nishina cross-section and in the Thomson limit. Applying the results to scattering of stellar blackbody radiation in the inner jet of Cyg X-3, we find that a low-energy break in the electron distribution at a Lorentz factor of ˜300-103 is required by the shape of the observed X-ray/γ-ray spectrum in order to avoid overproducing the observed X-ray flux. The electrons giving rise to the observed γ-rays are efficiently cooled by Compton scattering, and the power-law index of the acceleration process is ≃2.5-3. The bulk Lorentz factor of the jet and the kinetic power before the dissipation region depend on the fraction of the dissipation power supplied to the electrons; if it is ≃1/2, the Lorentz factor is ˜2.5, and the kinetic power is ˜1038 erg s-1, which represents a firm lower limit on the jet power, and is comparable to the bolometric luminosity of Cyg X-3. Most of the power supplied to the electrons is radiated. The broad-band spectrum constrains the synchrotron and self-Compton emission from the γ-ray emitting electrons, which requires the magnetic field to be relatively weak, with the magnetic energy density ≲ a few times 10-3 of that in the electrons. The actual value of the magnetic field strength can be inferred from a future simultaneous measurement of the infrared and γ-ray fluxes.

Resonantly Enhanced Betatron Hard X-rays from Ionization Injected Electrons in a Laser Plasma Accelerator

PubMed Central

Huang, K.; Li, Y. F.; Li, D. Z.; Chen, L. M.; Tao, M. Z.; Ma, Y.; Zhao, J. R.; Li, M. H.; Chen, M.; Mirzaie, M.; Hafz, N.; Sokollik, T.; Sheng, Z. M.; Zhang, J.

2016-01-01

Ultrafast betatron x-ray emission from electron oscillations in laser wakefield acceleration (LWFA) has been widely investigated as a promising source. Betatron x-rays are usually produced via self-injected electron beams, which are not controllable and are not optimized for x-ray yields. Here, we present a new method for bright hard x-ray emission via ionization injection from the K-shell electrons of nitrogen into the accelerating bucket. A total photon yield of 8 × 108/shot and 108 photons with energy greater than 110 keV is obtained. The yield is 10 times higher than that achieved with self-injection mode in helium under similar laser parameters. The simulation suggests that ionization-injected electrons are quickly accelerated to the driving laser region and are subsequently driven into betatron resonance. The present scheme enables the single-stage betatron radiation from LWFA to be extended to bright γ-ray radiation, which is beyond the capability of 3rd generation synchrotrons. PMID:27273170

X-ray generator

DOEpatents

Dawson, John M.

1976-01-01

Apparatus and method for producing coherent secondary x-rays that are controlled as to direction by illuminating a mixture of high z and low z gases with an intense burst of primary x-rays. The primary x-rays are produced with a laser activated plasma, and these x-rays strip off the electrons of the high z atoms in the lasing medium, while the low z atoms retain their electrons. The neutral atoms transfer electrons to highly excited states of the highly striped high z ions giving an inverted population which produces the desired coherent x-rays. In one embodiment, a laser, light beam provides a laser spark that produces the intense burst of coherent x-rays that illuminates the mixture of high z and low z gases, whereby the high z atoms are stripped while the low z ones are not, giving the desired mixture of highly ionized and neutral atoms. To this end, the laser spark is produced by injecting a laser light beam, or a plurality of beams, into a first gas in a cylindrical container having an adjacent second gas layer co-axial therewith, the laser producing a plasma and the intense primary x-rays in the first gas, and the second gas containing the high and low atomic number elements for receiving the primary x-rays, whereupon the secondary x-rays are produced therein by stripping desired ions in a neutral gas and transfer of electrons to highly excited states of the stripped ions from the unionized atoms. Means for magnetically confining and stabilizing the plasma are disclosed for controlling the direction of the x-rays.

Studies on solar hard X-Rays and gamma-rays: Compton backscatter, anisotropy, polarization and evidence for two phases of acceleration. Ph.D. Thesis - Maryland Univ.

NASA Technical Reports Server (NTRS)

Bai, T.

1977-01-01

Observations of solar X-rays and gamma-rays from large flares show that the hard X-ray spectrum extends into the gamma ray region, where a flattening in the spectrum of the continuum emission is observed above about 1 MeV. This emission is believed to be due to bremsstrahlung. In addition to electron-proton collisions, at energies greater than approximately 500 keV, bremsstrahlung due to electron-electron collisions becomes significant. Bremsstrahlung production was calculated for a variety of electron spectra extending from the nonrelativistic region to relativistic energies and electron-electron bremsstrahlung is taken into account. By comparing these calculations with data, it is shown that the flattening in the spectrum of the continuum emission can be best explained by an electron spectrum consisting of two distinctive components. This evidence, together with information on the X-ray and gamma ray time profiles, implied the existence of two phases of acceleration. The first phase accelerates electrons mainly up to about several hundred keV; the second phase accelerates a small fraction of the electrons accelerated in the first phase to relativistic energies and accelerates protons to tens and hundreds of MeV.

Visualizing the non-equilibrium dynamics of photoinduced intramolecular electron transfer with femtosecond X-ray pulses

PubMed Central

Canton, Sophie E.; Kjær, Kasper S.; Vankó, György; van Driel, Tim B.; Adachi, Shin-ichi; Bordage, Amélie; Bressler, Christian; Chabera, Pavel; Christensen, Morten; Dohn, Asmus O.; Galler, Andreas; Gawelda, Wojciech; Gosztola, David; Haldrup, Kristoffer; Harlang, Tobias; Liu, Yizhu; Møller, Klaus B.; Németh, Zoltán; Nozawa, Shunsuke; Pápai, Mátyás; Sato, Tokushi; Sato, Takahiro; Suarez-Alcantara, Karina; Togashi, Tadashi; Tono, Kensuke; Uhlig, Jens; Vithanage, Dimali A.; Wärnmark, Kenneth; Yabashi, Makina; Zhang, Jianxin; Sundström, Villy; Nielsen, Martin M.

2015-01-01

Ultrafast photoinduced electron transfer preceding energy equilibration still poses many experimental and conceptual challenges to the optimization of photoconversion since an atomic-scale description has so far been beyond reach. Here we combine femtosecond transient optical absorption spectroscopy with ultrafast X-ray emission spectroscopy and diffuse X-ray scattering at the SACLA facility to track the non-equilibrated electronic and structural dynamics within a bimetallic donor–acceptor complex that contains an optically dark centre. Exploiting the 100-fold increase in temporal resolution as compared with storage ring facilities, these measurements constitute the first X-ray-based visualization of a non-equilibrated intramolecular electron transfer process over large interatomic distances. Experimental and theoretical results establish that mediation through electronically excited molecular states is a key mechanistic feature. The present study demonstrates the extensive potential of femtosecond X-ray techniques as diagnostics of non-adiabatic electron transfer processes in synthetic and biological systems, and some directions for future studies, are outlined. PMID:25727920

Visualizing the non-equilibrium dynamics of photoinduced intramolecular electron transfer with femtosecond X-ray pulses

DOE PAGES

Canton, Sophie E.; Kjær, Kasper S.; Vankó, György; ...

2015-03-02

Ultrafast photoinduced electron transfer preceding energy equilibration still poses many experimental and conceptual challenges to the optimization of photoconversion since an atomic-scale description has so far been beyond reach. Here we combine femtosecond transient optical absorption spectroscopy with ultrafast X-ray emission spectroscopy and diffuse X-ray scattering at the SACLA facility to track the non-equilibrated electronic and structural dynamics within a bimetallic donor–acceptor complex that contains an optically dark centre. Exploiting the 100-fold increase in temporal resolution as compared with storage ring facilities, these measurements constitute the first X-ray-based visualization of a non-equilibrated intramolecular electron transfer process over large interatomic distances.more » Thus experimental and theoretical results establish that mediation through electronically excited molecular states is a key mechanistic feature. The present study demonstrates the extensive potential of femtosecond X-ray techniques as diagnostics of non-adiabatic electron transfer processes in synthetic and biological systems, and some directions for future studies, are outlined.« less

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

Fukao, Shinji; Nakanishi, Yoshikazu; Mizoguchi, Tadahiro

X-rays are radiated due to the bremsstrahlung caused by the collision of electrons with a metal target placed opposite the negative electric surface of a crystal by changing the temperature of a LiNbO{sub 3} single crystal uniaxially polarized in the c-axis direction. It is suggested that both electric field intensity and electron density determine the intensity of X-ray radiation. Electrons are supplied by the ionization of residual gas in space, field emission from a case inside which a crystal is located, considered to be due to the high electric-field intensity formed by the surface charges on the crystal, and anmore » external electron source, such as a thermionic source. In a high vacuum, it was found that the electrons supplied by electric-field emission mainly contribute to the radiation of X-rays. It was found that the integrated intensity of X-rays can be maximized by supplying electrons both external and by electric-field emission. Furthermore, the integrated intensity of the X-rays is stable for many repeated temperature changes.« less

Symposium N: Materials and Devices for Thermal-to-Electric Energy Conversion

DTIC Science & Technology

2010-08-24

X - ray diffraction, transmission electron microscopy, scanning electron microscopy, and dynamic light scattering. Thermal conductivity measurements...SEM), X - ray diffraction (XRD) measurements as well as Raman spectroscopy. The results from these techniques indicate a clear modification...was examined by using scanning electron microscope (SEM; HITACHI S-4500 model) attached with an energy dispersive x - ray spectroscopy. The electrical

Trajectories of high energy electrons in a plasma focus

NASA Technical Reports Server (NTRS)

Harries, W. L.; Lee, J. H.; Mcfarland, D. R.

1978-01-01

Measurements are made of high-energy electron trajectories in a plasma focus as functions of position, time, energy, and angle of emission. The spatial resolution of the X-ray emission shows that low-energy X-rays are emitted from the anode surface. It is also suggested that the highest energy X-rays originate from a small region on the axis. The so-called shadow technique shows that the electron beam is perpendicular to the anode surface. Polar diagrams of medium and high-energy X-rays agree with the bremsstrahlung emission from a relativistic electron beam, the current of which is several 100 A.

Thomson-backscattered x rays from laser-accelerated electrons.

PubMed

Schwoerer, H; Liesfeld, B; Schlenvoigt, H-P; Amthor, K-U; Sauerbrey, R

2006-01-13

We present the first observation of Thomson-backscattered light from laser-accelerated electrons. In a compact, all-optical setup, the "photon collider," a high-intensity laser pulse is focused into a pulsed He gas jet and accelerates electrons to relativistic energies. A counterpropagating laser probe pulse is scattered from these high-energy electrons, and the backscattered x-ray photons are spectrally analyzed. This experiment demonstrates a novel source of directed ultrashort x-ray pulses and additionally allows for time-resolved spectroscopy of the laser acceleration of electrons.

Electron beams in solar flares

NASA Technical Reports Server (NTRS)

Aschwanden, Markus J.; Dennis, Brian R.; Benz, Arnold O.

1994-01-01

A list of publications resulting from this program includes 'The Timing of Electron Beam Signatures in Hard X-Ray and Radio: Solar Flare Observations by BATSE/Compton Gamma-Ray Observatory and PHOENIX'; 'Coherent-Phase or Random-Phase Acceleration of Electron Beams in Solar Flares'; 'Particle Acceleration in Flares'; 'Chromospheric Evaporation and Decimetric Radio Emission in Solar Flares'; 'Sequences of Correlated Hard X-Ray and Type 3 Bursts During Solar Flares'; and 'Solar Electron Beams Detected in Hard X-Rays and Radiowaves.' Abstracts and reprints of each are attached to this report.

Comparison of structural and magnetic properties of Zn{sub x}Mg{sub 1.5-x}Mn{sub 0.5}FeO{sub 4} and MgAl{sub x}Cr{sub x}Fe{sub 2-2x}O{sub 4} spinel oxides

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

Thummer, K. P., E-mail: kpthummer@yahoo.co.in; Tanna, A. R., E-mail: ashish.tanna@rku.ac.in; Joshi, H. H.

2016-05-23

The spinel oxides Zn{sub x}Mg{sub 1.5-x}Mn{sub 0.5}FeO{sub 4} (x = 0.0 to 0.6) and MgAl{sub x}Cr{sub x}Fe{sub 2-2x}O{sub 4} (x = 0.0 to 0.6) abbreviated as ZMMFO and MACFO respectively, were synthesized by standard ceramic processing. The compositional purity of all the specimens was checked by EDAX technique. The X-ray diffractometry was employed to determine the lattice constants and distribution of cations in the interstitial voids. The initial decrease of cell edge parameter (a) for ZMMFO up to x = 0.2 and thereafter expected rise in the ‘a’ and the initial slower rate of reduction in the lattice constant formore » MACFO are explained as basic of cation occupancy. The magnetic ordering in both systems is explained by invoking statistical canting models. The compositional variation of magneton number (n{sub B}) for ZMMFO could be very well explained by Localized canting of spin (LCS) model while Random canting of spin (RCS) model was used for MACFO system.« less

Comparative analysis of strain fields in layers of step-graded metamorphic buffers of various designs

NASA Astrophysics Data System (ADS)

Aleshin, A. N.; Bugaev, A. S.; Ruban, O. A.; Tabachkova, N. Yu.; Shchetinin, I. V.

2017-10-01

Spatial distribution of residual elastic strain in the layers of two step-graded metamophic buffers of various designs, grown by molecular beam epitaxy from ternary InxAl1-xAs solutions on GaAs(001) substrates, is obtained using reciprocal space mapping by three-axis X-ray diffractometry and the linear theory of elasticity. The difference in the design of the buffers enabled the formation of a dislocation-free layer with different thickness in each of the heterostructures, which was the main basis of this study. It is shown that, in spite of the different design of graded metamorphic buffers, the nature of strain fields in them is the same, and the residual elastic strains in the final elements of both buffers adjusted for the effect of work hardening subject to the same phenomenological law, which describes the strain relief process in single-layer heterostructures.

Generation of High Brightness X-rays with the PLEIADES Thomson X-ray Source

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

Brown, W J; Anderson, S G; Barty, C P J

2003-05-28

The use of short laser pulses to generate high peak intensity, ultra-short x-ray pulses enables exciting new experimental capabilities, such as femtosecond pump-probe experiments used to temporally resolve material structural dynamics on atomic time scales. PLEIADES (Picosecond Laser Electron InterAction for Dynamic Evaluation of Structures) is a next generation Thomson scattering x-ray source being developed at Lawrence Livermore National Laboratory (LLNL). Ultra-fast picosecond x-rays (10-200 keV) are generated by colliding an energetic electron beam (20-100 MeV) with a high intensity, sub-ps, 800 nm laser pulse. The peak brightness of the source is expected to exceed 10{sup 20} photons/s/0.1% bandwidth/mm2/mrad2. Simulationsmore » of the electron beam production, transport, and final focus are presented. Electron beam measurements, including emittance and final focus spot size are also presented and compared to simulation results. Measurements of x-ray production are also reported and compared to theoretical calculations.« less

Laboratory Measurements of X-Ray Emissions From Centimeter-Long Streamer Corona Discharges

NASA Astrophysics Data System (ADS)

da Silva, C. L.; Millan, R. M.; McGaw, D. G.; Yu, C. T.; Putter, A. S.; LaBelle, J.; Dwyer, J.

2017-11-01

We provide extensive evidence that runaway electron acceleration and subsequent bremsstrahlung X-ray emission are a common feature in negative electrical discharges with voltages as low as 100 kV, indicating that all negative lightning could potentially produce runaway electrons. Centimeter long streamer corona discharges produce bursts of X-ray radiation, emitted by a source highly compact in space and time, leading to photon pileup. Median photon burst energies vary between 33 and 96 keV in 100 kV discharges. Statistical analysis of 5,000+ discharges shows that X-rays are observed in as many as 60% of the triggers, depending on the configuration. X-ray detection is more frequent when streamers are not followed by a spark, the detector is oriented perpendicular to the gap, and a thicker anode is used. In an 8-cm-long gap, X-rays are produced when runaway electrons hit the anode, and the electron acceleration is not necessarily correlated with streamer collisions.

Fresh-slice multicolour X-ray free-electron lasers

DOE PAGES

Lutman, Alberto A.; Maxwell, Timothy J.; MacArthur, James P.; ...

2016-10-24

X-ray free-electron lasers (XFELs) provide femtosecond X-ray pulses with a narrow energy bandwidth and unprecedented brightness. Ultrafast physical and chemical dynamics, initiated with a site-specific X-ray pulse, can be explored using XFELs with a second ultrashort X-ray probe pulse. However, existing double-pulse schemes are complicated, difficult to customize or provide only low-intensity pulses. Here we present the novel fresh-slice technique for multicolour pulse production, wherein different temporal slices of an electron bunch lase to saturation in separate undulator sections. This method combines electron bunch tailoring from a passive wakefield device with trajectory control to provide multicolour pulses. The fresh-slice schememore » outperforms existing techniques at soft X-ray wavelengths. It produces femtosecond pulses with a power of tens of gigawatts and flexible colour separation. The pulse delay can be varied from temporal overlap to almost one picosecond. As a result, we also demonstrate the first three-colour XFEL and variably polarized two-colour pulses.« less

High resolution energy-angle correlation measurement of hard x rays from laser-Thomson backscattering.

PubMed

Jochmann, A; Irman, A; Bussmann, M; Couperus, J P; Cowan, T E; Debus, A D; Kuntzsch, M; Ledingham, K W D; Lehnert, U; Sauerbrey, R; Schlenvoigt, H P; Seipt, D; Stöhlker, Th; Thorn, D B; Trotsenko, S; Wagner, A; Schramm, U

2013-09-13

Thomson backscattering of intense laser pulses from relativistic electrons not only allows for the generation of bright x-ray pulses but also for the investigation of the complex particle dynamics at the interaction point. For this purpose a complete spectral characterization of a Thomson source powered by a compact linear electron accelerator is performed with unprecedented angular and energy resolution. A rigorous statistical analysis comparing experimental data to 3D simulations enables, e.g., the extraction of the angular distribution of electrons with 1.5% accuracy and, in total, provides predictive capability for the future high brightness hard x-ray source PHOENIX (photon electron collider for narrow bandwidth intense x rays) and potential gamma-ray sources.

Synthesis and Characterization of Cu- and Co-Doped Bi4V2O11 for Intermediate-Temperature Solid Oxide Fuel Cell Electrolytes by Carbonate Coprecipitation

NASA Astrophysics Data System (ADS)

Lee, Jin Goo; Yoon, Hyon Hee

2011-01-01

Bi2MexV1-xO5.5-3x/2 (Me = Cu; 0≤x≤0.2) powders were prepared by the ammonium carbonate coprecipitation method. The starting salts were bismuth nitrate, copper nitrate, cobalt nitrate, and vanadium sulphate. The thermal decomposition of Bi2MexV1-xO5.5-3x/2 precursors was completed at about 500 °C. The crystallite structure, surface morphology, and ionic conductivity of the prepared powders and pellets were examined using X-ray diffractometry, field emission scanning electron microscopy, and an impedance analyzer, respectively. The average particle sizes of the Bi2Cu0.1V0.9O5.35 and Bi2Co0.1V0.9O5.35 powders were 10-50 nm. The tetragonal structure (γ-phase) appeared at sintering temperatures higher than 700 °C and the peak intensity increased at higher sintering temperatures. The ionic conductivities of the Bi2Cu0.1V0.9O5.35 and Bi2Co0.1V0.9O5.35 pellets sintered at 800 °C showed the highest values of 6.8×10-2 S cm-1 at 700 °C and 9.1×10-2 S cm-1 at 700 °C, respectively. The optimum concentration of the Cu and Co dopants in Bi2MexV1-xO5.5-3x/2 was determined to be 0.1. The results of this study demonstrated that the ammonium carbonate coprecipitation process could be used as an economical method for the preparation of Bi2MexV1-xO5.5-3x/2 electrolytes for intermediate-temperature solid oxide fuel cells.

X-ray emissions from centimeter-long streamer corona discharges

NASA Astrophysics Data System (ADS)

da Silva, C. L.; Millan, R. M.; McGaw, D. G.; Yu, C. T.; Putter, A. S.; Labelle, J. W.; Dwyer, J. R.

2017-12-01

In this work we provide extensive evidence that runaway electron acceleration and subsequent bremsstrahlung X-ray emission are a common feature in electrical discharges of negative polarity. They can be easily detected at voltages as low as 100 kV, indicating that all negative lightning could potentially produce runaway electrons. We show that centimeter-long streamer corona discharges produce bursts of X-ray radiation that are emitted by a source that is highly compact in space and time. Therefore, the emitted X-ray photons arrive together at the detector and pile up. Median burst energies vary between 33-96% of the total 100 keV available electrostatic energy that an electron can acquire in the gap. We present detailed statistical analysis of 5000+ discharges, showing that X-rays are observed in as many as 60% of the triggers, depending on the configuration. X-ray detection is more frequent when: the streamer corona discharge is not followed by a spark, the detector is oriented perpendicular to the gap, and a thicker anode is used. We show that for an 8-cm-long gap, X-rays are produced when runaway electrons hit the anode, and that the runaway electron acceleration is not correlated with streamer collisions, as inferred in meter-long discharges. The described experiment is a promising way for measuring the runaway electron distribution very close to the source and its dependence on the applied voltage.

A new endstation at the Swiss Light Source for ultraviolet photoelectron spectroscopy, X-ray photoelectron spectroscopy, and X-ray absorption spectroscopy measurements of liquid solutions.

PubMed

Brown, Matthew A; Redondo, Amaia Beloqui; Jordan, Inga; Duyckaerts, Nicolas; Lee, Ming-Tao; Ammann, Markus; Nolting, Frithjof; Kleibert, Armin; Huthwelker, Thomas; Müächler, Jean-Pierre; Birrer, Mario; Honegger, Juri; Wetter, Reto; Wörner, Hans Jakob; van Bokhoven, Jeroen A

2013-07-01

A new liquid microjet endstation designed for ultraviolet (UPS) and X-ray (XPS) photoelectron, and partial electron yield X-ray absorption (XAS) spectroscopies at the Swiss Light Source is presented. The new endstation, which is based on a Scienta HiPP-2 R4000 electron spectrometer, is the first liquid microjet endstation capable of operating in vacuum and in ambient pressures up to the equilibrium vapor pressure of liquid water at room temperature. In addition, the Scienta HiPP-2 R4000 energy analyzer of this new endstation allows for XPS measurements up to 7000 eV electron kinetic energy that will enable electronic structure measurements of bulk solutions and buried interfaces from liquid microjet samples. The endstation is designed to operate at the soft X-ray SIM beamline and at the tender X-ray Phoenix beamline. The endstation can also be operated using a Scienta 5 K ultraviolet helium lamp for dedicated UPS measurements at the vapor-liquid interface using either He I or He II α lines. The design concept, first results from UPS, soft X-ray XPS, and partial electron yield XAS measurements, and an outlook to the potential of this endstation are presented.

X-ray free-electron laser oscillator with nuclear-resonant cavity stabilization and quantum-optical applications

DOE PAGES

Adams, Bernhard W.; Kim, Kwang -Je

2016-08-09

Here, x-ray free-electron-laser oscillators with nuclear-resonant cavity stabilization (NRS-XFELO) hold the promise for providing x-rays with unprecedented coherence properties that will enable interesting quantum-optical and metrological applications. Among these are atom optics with x-ray-based optical elements providing high momentum transfer, or a frequency standard far surpassing the best state-of the-art atomic clocks.

Modification and benchmarking of MCNP for low-energy tungsten spectra.

PubMed

Mercier, J R; Kopp, D T; McDavid, W D; Dove, S B; Lancaster, J L; Tucker, D M

2000-12-01

The MCNP Monte Carlo radiation transport code was modified for diagnostic medical physics applications. In particular, the modified code was thoroughly benchmarked for the production of polychromatic tungsten x-ray spectra in the 30-150 kV range. Validating the modified code for coupled electron-photon transport with benchmark spectra was supplemented with independent electron-only and photon-only transport benchmarks. Major revisions to the code included the proper treatment of characteristic K x-ray production and scoring, new impact ionization cross sections, and new bremsstrahlung cross sections. Minor revisions included updated photon cross sections, electron-electron bremsstrahlung production, and K x-ray yield. The modified MCNP code is benchmarked to electron backscatter factors, x-ray spectra production, and primary and scatter photon transport.

Density gradient free electron collisionally excited x-ray laser

DOEpatents

Campbell, E.M.; Rosen, M.D.

1984-11-29

An operational x-ray laser is provided that amplifies 3p-3s transition x-ray radiation along an approximately linear path. The x-ray laser is driven by a high power optical laser. The driving line focused optical laser beam illuminates a free-standing thin foil that may be associated with a substrate for improved structural integrity. This illumination produces a generally cylindrically shaped plasma having an essentially uniform electron density and temperature, that exists over a long period of time, and provides the x-ray laser gain medium. The x-ray laser may be driven by more than one optical laser beam. The x-ray laser has been successfully demonstrated to function in a series of experimental tests.

Status of the eROSITA Telescope testing and calibrating the x-ray mirror assemblies

NASA Astrophysics Data System (ADS)

Burwitz, Vadim; Predehl, Peter; Bräuninger, Heinrich; Burkert, Wolfgang; Dennerl, Konrad; Eder, Josef; Friedrich, Peter; Fürmetz, Maria; Grisoni, Gabriele; Hartner, Gisela; Marioni, Fabio; Menz, Benedikt; Pfeffermann, Elmar; Valsecchi, Giuseppe

2013-09-01

The eROSITA X-ray observatory that will be launched on board the Russian Spectrum-RG mission comprises seven X-ray telescopes, each with its own mirror assembly (mirror module + X-ray baffle), electron deflector, filter wheel, and CCD camera with its control electronics. The completed flight mirror modules are undergoing many thorough X-ray tests at the PANTHER X-ray test facility after delivery, after being mated with the X-ray baffle, and again after both the vibration and thermal-vacuum tests. A description of the work done with mirror modules/assemblies and the test results obtained will be reported here. We report also on the environmental tests that have been performed on the eROSITA telescope qualification model.

LABORATORY MEASUREMENTS COMPELLINGLY SUPPORT A CHARGE-EXCHANGE MECHANISM FOR THE “DARK MATTER” ∼3.5 keV X-Ray LINE

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

Shah, Chintan; Dobrodey, Stepan; Bernitt, Sven

2016-12-10

The reported observations of an unidentified X-ray line feature at ∼3.5 keV have driven a lively discussion about its possible dark matter origin. Motivated by this, we have measured the K-shell X-ray spectra of highly ionized bare sulfur ions following charge exchange with gaseous molecules in an electron beam ion trap, as a source of or a contributor to this X-ray line. We produced S{sup 16+} and S{sup 15+} ions and let them capture electrons in collision with those molecules with the electron beam turned off while recording X-ray spectra. We observed a charge-exchange-induced X-ray feature at the Lyman seriesmore » limit (3.47 ± 0.06 keV). The inferred X-ray energy is in full agreement with the reported astrophysical observations and supports the novel scenario proposed by Gu et al.« less

Radiation damage free ghost diffraction with atomic resolution

DOE PAGES

Li, Zheng; Medvedev, Nikita; Chapman, Henry N.; ...

2017-12-21

The x-ray free electron lasers can enable diffractive structural determination of protein nanocrystals and single molecules that are too small and radiation-sensitive for conventional x-ray diffraction. However the electronic form factor may be modified during the ultrashort x-ray pulse due to photoionization and electron cascade caused by the intense x-ray pulse. For general x-ray imaging techniques, the minimization of the effects of radiation damage is of major concern to ensure reliable reconstruction of molecular structure. Here in this paper, we show that radiation damage free diffraction can be achieved with atomic spatial resolution by using x-ray parametric down-conversion and ghostmore » diffraction with entangled photons of x-ray and optical frequencies. We show that the formation of the diffraction patterns satisfies a condition analogous to the Bragg equation, with a resolution that can be as fine as the crystal lattice length scale of several Ångstrom. Since the samples are illuminated by low energy optical photons, they can be free of radiation damage.« less

Radiation damage free ghost diffraction with atomic resolution

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

Li, Zheng; Medvedev, Nikita; Chapman, Henry N.

The x-ray free electron lasers can enable diffractive structural determination of protein nanocrystals and single molecules that are too small and radiation-sensitive for conventional x-ray diffraction. However the electronic form factor may be modified during the ultrashort x-ray pulse due to photoionization and electron cascade caused by the intense x-ray pulse. For general x-ray imaging techniques, the minimization of the effects of radiation damage is of major concern to ensure reliable reconstruction of molecular structure. Here in this paper, we show that radiation damage free diffraction can be achieved with atomic spatial resolution by using x-ray parametric down-conversion and ghostmore » diffraction with entangled photons of x-ray and optical frequencies. We show that the formation of the diffraction patterns satisfies a condition analogous to the Bragg equation, with a resolution that can be as fine as the crystal lattice length scale of several Ångstrom. Since the samples are illuminated by low energy optical photons, they can be free of radiation damage.« less

Development of a low-energy x-ray camera for the imaging of secondary electron bremsstrahlung x-ray emitted during proton irradiation for range estimation.

PubMed

Ando, Koki; Yamaguchi, Mitsutaka; Yamamoto, Seiichi; Toshito, Toshiyuki; Kawachi, Naoki

2017-06-21

Imaging of secondary electron bremsstrahlung x-ray emitted during proton irradiation is a possible method for measurement of the proton beam distribution in phantom. However, it is not clear that the method is used for range estimation of protons. For this purpose, we developed a low-energy x-ray camera and conducted imaging of the bremsstrahlung x-ray produced during irradiation of proton beams. We used a 20 mm  ×  20 mm  ×  1 mm finely grooved GAGG scintillator that was optically coupled to a one-inch square high quantum efficiency (HQE)-type position-sensitive photomultiplier tube to form an imaging detector. The imaging detector was encased in a 2 cm-thick tungsten container, and a pinhole collimator was attached to its camera head. After performance of the camera was evaluated, secondary electron bremsstrahlung x-ray imaging was conducted during irradiation of the proton beams for three different proton energies, and the results were compared with Monte Carlo simulation as well as calculated value. The system spatial resolution and sensitivity of the developed x-ray camera with 1.5 mm-diameter pinhole collimator were estimated to be 32 mm FWHM and 5.2  ×  10 -7 for ~35 keV x-ray photons at 100 cm from the collimator surface, respectively. We could image the proton beam tracks by measuring the secondary electron bremsstrahlung x-ray during irradiation of the proton beams, and the ranges for different proton energies could be estimated from the images. The measured ranges from the images were well matched with the Monte Carlo simulation, and slightly smaller than the calculated values. We confirmed that the imaging of the secondary electron bremsstrahlung x-ray emitted during proton irradiation with the developed x-ray camera has the potential to be a new tool for proton range estimations.

Electronic structure and soft-X-ray-induced photoreduction studies of iron-based magnetic polyoxometalates of type {(M)M5}12Fe(III)30 (M = Mo(VI), W(VI)).

PubMed

Kuepper, Karsten; Derks, Christine; Taubitz, Christian; Prinz, Manuel; Joly, Loïc; Kappler, Jean-Paul; Postnikov, Andrei; Yang, Wanli; Kuznetsova, Tatyana V; Wiedwald, Ulf; Ziemann, Paul; Neumann, Manfred

2013-06-14

Giant Keplerate-type molecules with a {Mo72Fe30} core show a number of very interesting properties, making them particularly promising for various applications. So far, only limited data on the electronic structure of these molecules from X-ray spectra and electronic structure calculations have been available. Here we present a combined electronic and magnetic structure study of three Keplerate-type nanospheres--two with a {Mo72Fe30} core and one with a {W72Fe30} core by means of X-ray absorption spectroscopy, X-ray magnetic circular dichroism (XMCD), SQUID magnetometry, and complementary theoretical approaches. Furthermore, we present detailed studies of the Fe(3+)-to-Fe(2+) photoreduction process, which is induced under soft X-ray radiation in these molecules. We observe that the photoreduction rate greatly depends on the ligand structure surrounding the Fe ions, with negatively charged ligands leading to a dramatically reduced photoreduction rate. This opens the possibility of tailoring such polyoxometalates by X-ray spectroscopic studies and also for potential applications in the field of X-ray induced photochemistry.

Nonlinear effects in propagation of radiation of X-ray free-electron lasers

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

Nosik, V. L., E-mail: v-nosik@yandex.ru, E-mail: nosik@ns.crys.ras.ru

2016-05-15

Nonlinear effects accompanying the propagation of high-intensity beams of X-ray free-electron lasers are considered. It is shown that the X-ray wave field in the crystal significantly changes due to the formation of “hollow” atomic shells as a result of the photoelectric effect.

An investigation on some of the tumor treatment cases using x-rays and electron beams

NASA Astrophysics Data System (ADS)

Ucar, Burcu; Yigitoglu, Ibrahim; Arslan Kabalay, Ipek; Altiparmak, Duygu; Kilicaslan, Sinem

2015-07-01

In this work, we discussed some of the applications which X-rays and electron beam used in radiotherapy for tumor treatments. This study has been performed at Radiation Oncology Department, Medicine Faculty in Gaziosmanpasa University by using the VARIAN CLINICA DHX linear accelerator which is operated in the range of 6 MeV - 15 MeV. Processes for the treatments that X-rays used for pancreas, bladder and prostate tumors and the processes that the electron beam used for some of the derm tumors are studied. Effects of X-rays and electron beams to treatments process are examined and the obtained results are presented comparatively.

Energetics of impulsive solar flares: Correlating BATSE hard x-ray bursts and the solar atmosphere's soft x-ray response

NASA Technical Reports Server (NTRS)

Newton, Elizabeth

1996-01-01

This investigation has involved the correlation of BATSE-observed solar hard X-ray emission with the characteristics of soft X-ray emitting plasma observed by the Yohkoh Bragg Crystal Spectrometers. The goal was to test the hypothesis that localized electron beam heating is the dominant energy transport mechanism in impulsive flares, as formulated in the thick-target electron-heated model of Brown.

Two-dimensional time-resolved ultra-high speed imaging of K-alpha emission from short-pulse-laser interactions to observe electron recirculation

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

Nagel, S. R.; Chen, H.; Park, J.

Time resolved x-ray images with 7 ps resolution are recorded on relativistic short-pulse laser-plasma experiments using the dilation x-ray imager, a high-speed x-ray framing camera, sensitive to x-rays in the range of ≈1-17 keV. Furthermore, this capability enables a series of 2D x-ray images to be recorded at picosecond scales, which allows for the investigation of fast electron transport within the target with unprecedented temporal resolution. With an increase in the Kα-emission spot size over time we found that targets were thinner than the recirculation limit and is absent for thicker targets. Together with the observed polarization dependence of themore » spot size increase, this indicates that electron recirculation is relevant for the x-ray production in thin targets.« less

Two-dimensional time-resolved ultra-high speed imaging of K-alpha emission from short-pulse-laser interactions to observe electron recirculation

DOE PAGES

Nagel, S. R.; Chen, H.; Park, J.; ...

2017-04-04

Time resolved x-ray images with 7 ps resolution are recorded on relativistic short-pulse laser-plasma experiments using the dilation x-ray imager, a high-speed x-ray framing camera, sensitive to x-rays in the range of ≈1-17 keV. Furthermore, this capability enables a series of 2D x-ray images to be recorded at picosecond scales, which allows for the investigation of fast electron transport within the target with unprecedented temporal resolution. With an increase in the Kα-emission spot size over time we found that targets were thinner than the recirculation limit and is absent for thicker targets. Together with the observed polarization dependence of themore » spot size increase, this indicates that electron recirculation is relevant for the x-ray production in thin targets.« less

Establishing nonlinearity thresholds with ultraintense X-ray pulses

NASA Astrophysics Data System (ADS)

Szlachetko, Jakub; Hoszowska, Joanna; Dousse, Jean-Claude; Nachtegaal, Maarten; Błachucki, Wojciech; Kayser, Yves; Sà, Jacinto; Messerschmidt, Marc; Boutet, Sebastien; Williams, Garth J.; David, Christian; Smolentsev, Grigory; van Bokhoven, Jeroen A.; Patterson, Bruce D.; Penfold, Thomas J.; Knopp, Gregor; Pajek, Marek; Abela, Rafael; Milne, Christopher J.

2016-09-01

X-ray techniques have evolved over decades to become highly refined tools for a broad range of investigations. Importantly, these approaches rely on X-ray measurements that depend linearly on the number of incident X-ray photons. The advent of X-ray free electron lasers (XFELs) is opening the ability to reach extremely high photon numbers within ultrashort X-ray pulse durations and is leading to a paradigm shift in our ability to explore nonlinear X-ray signals. However, the enormous increase in X-ray peak power is a double-edged sword with new and exciting methods being developed but at the same time well-established techniques proving unreliable. Consequently, accurate knowledge about the threshold for nonlinear X-ray signals is essential. Herein we report an X-ray spectroscopic study that reveals important details on the thresholds for nonlinear X-ray interactions. By varying both the incident X-ray intensity and photon energy, we establish the regimes at which the simplest nonlinear process, two-photon X-ray absorption (TPA), can be observed. From these measurements we can extract the probability of this process as a function of photon energy and confirm both the nature and sub-femtosecond lifetime of the virtual intermediate electronic state.

X-Ray Data Booklet

Science.gov Websites

X-RAY DATA BOOKLET Center for X-ray Optics and Advanced Light Source Lawrence Berkeley National Laboratory Introduction X-Ray Properties of Elements Electron Binding Energies X-Ray Energy Emission Energies Table of X-Ray Properties Synchrotron Radiation Characteristics of Synchrotron Radiation History of X

High Energy Electron Detectors on Sphinx

NASA Astrophysics Data System (ADS)

Thompson, J. R.; Porte, A.; Zucchini, F.; Calamy, H.; Auriel, G.; Coleman, P. L.; Bayol, F.; Lalle, B.; Krishnan, M.; Wilson, K.

2008-11-01

Z-pinch plasma radiation sources are used to dose test objects with K-shell (˜1-4keV) x-rays. The implosion physics can produce high energy electrons (> 50keV), which could distort interpretation of the soft x-ray effects. We describe the design and implementation of a diagnostic suite to characterize the electron environment of Al wire and Ar gas puff z-pinches on Sphinx. The design used ITS calculations to model detector response to both soft x-rays and electrons and help set upper bounds to the spurious electron flux. Strategies to discriminate between the known soft x-ray emission and the suspected electron flux will be discussed. H.Calamy et al, ``Use of microsecond current prepulse for dramatic improvements of wire array Z-pinch implosion,'' Phys Plasmas 15, 012701 (2008) J.A.Halbleib et al, ``ITS: the integrated TIGER series of electron/photon transport codes-Version 3.0,'' IEEE Trans on Nuclear Sci, 39, 1025 (1992)

Prediction and observation of tin and silver plasmas with index of refraction greater than one in the soft x-ray range.

PubMed

Filevich, Jorge; Grava, Jonathan; Purvis, Mike; Marconi, Mario C; Rocca, Jorge J; Nilsen, Joseph; Dunn, James; Johnson, Walter R

2006-07-01

We present the calculated prediction and the experimental confirmation that doubly ionized Ag and Sn plasmas can have an index of refraction greater than one for soft x-ray wavelengths. Interferometry experiments conducted using a capillary discharge soft x-ray laser operating at a wavelength of confirm that in few times ionized laser-created plasmas of these elements the anomalous dispersion from bound electrons can dominate the free electron contribution, making the index of refraction greater than one. The results confirm that bound electrons can strongly influence the index of refraction of numerous plasmas over a broad range of soft x-ray wavelengths confirming recent observations. The understanding of index of refraction at short wavelengths will become even more essential during the next decade as x-ray free electron lasers will become available to probe a wider variety of plasmas at higher densities and shorter wavelengths.

Real Time Spectroscopic Ellipsometry Analysis of First Stage CuIn1-xGaxSe₂ Growth: Indium-Gallium Selenide Co-Evaporation.

PubMed

Pradhan, Puja; Aryal, Puruswottam; Attygalle, Dinesh; Ibdah, Abdel-Rahman; Koirala, Prakash; Li, Jian; Bhandari, Khagendra P; Liyanage, Geethika K; Ellingson, Randy J; Heben, Michael J; Marsillac, Sylvain; Collins, Robert W; Podraza, Nikolas J

2018-01-16

Real time spectroscopic ellipsometry (RTSE) has been applied for in-situ monitoring of the first stage of copper indium-gallium diselenide (CIGS) thin film deposition by the three-stage co-evaporation process used for fabrication of high efficiency thin film photovoltaic (PV) devices. The first stage entails the growth of indium-gallium selenide (In 1- x Ga x )₂Se₃ (IGS) on a substrate of Mo-coated soda lime glass maintained at a temperature of 400 °C. This is a critical stage of CIGS deposition because a large fraction of the final film thickness is deposited, and as a result precise compositional control is desired in order to achieve the optimum performance of the resulting CIGS solar cell. RTSE is sensitive to monolayer level film growth processes and can provide accurate measurements of bulk and surface roughness layer thicknesses. These in turn enable accurate measurements of the bulk layer optical response in the form of the complex dielectric function ε = ε₁ - iε₂, spectra. Here, RTSE has been used to obtain the (ε₁, ε₂) spectra at the measurement temperature of 400 °C for IGS thin films of different Ga contents ( x ) deduced from different ranges of accumulated bulk layer thickness during the deposition process. Applying an analytical expression in common for each of the (ε₁, ε₂) spectra of these IGS films, oscillator parameters have been obtained in the best fits and these parameters in turn have been fitted with polynomials in x . From the resulting database of polynomial coefficients, the (ε₁, ε₂) spectra can be generated for any composition of IGS from the single parameter, x . The results have served as an RTSE fingerprint for IGS composition and have provided further structural information beyond simply thicknesses, for example information related to film density and grain size. The deduced IGS structural evolution and the (ε₁, ε₂) spectra have been interpreted as well in relation to observations from scanning electron microscopy, X-ray diffractometry and energy-dispersive X-ray spectroscopy profiling analyses. Overall the structural, optical and compositional analysis possible by RTSE has assisted in understanding the growth and properties of three stage CIGS absorbers for solar cells and shows future promise for enhancing cell performance through monitoring and control.

Implications of X-Ray Observations for Electron Acceleration and Propagation in Solar Flares

NASA Technical Reports Server (NTRS)

Holman, G. D.; Aschwanden, M. J.; Aurass, H.; Battaglia, M.; Grigis, P. C.; Kontar, E. P.; Liu, W.; Saint-Hilaire, P.; Zharkova, V. V.

2011-01-01

High-energy X-rays and gamma-rays from solar flares were discovered just over fifty years ago. Since that time, the standard for the interpretation of spatially integrated flare X-ray spectra at energies above several tens of keV has been the collisional thick-target model. After the launch of the Reuven Ramaty High Energy Solar Spectroscopic Imager (RHESSI) in early 2002, X-ray spectra and images have been of sufficient quality to allow a greater focus on the energetic electrons responsible for the X-ray emission, including their origin and their interactions with the flare plasma and magnetic field. The result has been new insights into the flaring process, as well as more quantitative models for both electron acceleration and propagation, and for the flare environment with which the electrons interact. In this article we review our current understanding of electron acceleration, energy loss, and propagation in flares. Implications of these new results for the collisional thick-target model, for general flare models, and for future flare studies are discussed.

Growth of indium gallium arsenide thin film on silicon substrate by MOCVD technique

NASA Astrophysics Data System (ADS)

Chowdhury, Sisir; Das, Anish; Banerji, Pallab

2018-05-01

Indium gallium arsenide (InGaAs) thin film with indium phosphide (InP) buffer has been grown on p-type silicon (100) by Metal Organic Chemical Vapor Deposition (MOCVD) technique. To get a lattice matched substrate an Indium Phosphide buffer thin film is deposited onto Si substrate prior to InGaAs growth. The grown films have been investigated by UV-Vis-NIR reflectance spectroscopy. The band gap energy of the grown InGaAs thin films determined to be 0.82 eV from reflectance spectrum and the films are found to have same thickness for growth between 600 °C and 650 °C. Crystalline quality of the grown films has been studied by grazing incidence X-ray diffractometry (GIXRD).

Degradation of 4-Chlorophenol Under Sunlight Using ZnO Nanoparticles as Catalysts

NASA Astrophysics Data System (ADS)

Rajar, Kausar; Sirajuddin; Balouch, Aamna; Bhanger, M. I.; Sherazi, Tufail H.; Kumar, Raj

2018-03-01

Herein we demonstrate a simplistic microwave assisted chemical precipitation approach regarding the synthesis of zinc oxide nanoparticles. As-prepared ZnO nanoparticles (NPs) were characterized by UV-visible spectroscopy, Fourier transform infra-red spectroscopy, atomic force microscopy and x-ray diffractometry and scrutinized as photo-catalysts for degradation of 4-chlorophenol (4-CP) under sunlight. The study substantiated that 98.5% of 4-CP was degraded within 20 min in the absence of initiator like H2O2 which reflects an outstanding prospective use for ZnO NPs as photo-catalysts. The nanocatalysts were recycled four times and still showed catalytic efficiency up to 95.5% for degradation of 4-CP in the specified 20 min.

Optical Fourier diffractometry applied to degraded bone structure recognition

NASA Astrophysics Data System (ADS)

Galas, Jacek; Godwod, Krzysztof; Szawdyn, Jacek; Sawicki, Andrzej

1993-09-01

Image processing and recognition methods are useful in many fields. This paper presents the hybrid optical and digital method applied to recognition of pathological changes in bones involved by metabolic bone diseases. The trabecular bone structure, registered by x ray on the photographic film, is analyzed in the new type of computer controlled diffractometer. The set of image parameters, extracted from diffractogram, is evaluated by statistical analysis. The synthetic image descriptors in discriminant space, constructed on the base of 3 training groups of images (control, osteoporosis, and osteomalacia groups) by discriminant analysis, allow us to recognize bone samples with degraded bone structure and to recognize the disease. About 89% of the images were classified correctly. This method after optimization process will be verified in medical investigations.

Removal of р-nitrophenol from aqueous solution by magnetically modified activated carbon

NASA Astrophysics Data System (ADS)

Han, Shuai; Zhao, Feng; Sun, Jian; Wang, Bin; Wei, Rongyan; Yan, Shiqiang

2013-09-01

Activated carbon was modified with γ-Fe2O3 nanoparticles, using the chemical co-precipitation technique and the carboxylic acid vapor treatment technique. Two magnetic composites were characterized and compared by Fourier Transform Infrared spectroscopy, X-ray diffractometry, vibrating sample magnetometry and nitrogen adsorption-desorption. Then the two materials were used to remove p-nitrophenol in water. The equilibrium data revealed that the Langmuir isotherm was better in fitting the experiment result than the Freundlich isotherm, and the sorption capacity of the nanocomposite made by the chemical co-precipitation technique was higher than that of the other one. We suggest that the chemical co-precipitation technique is a more efficient and practical method to produce magnetically modified activated carbon.

Lattice distortion and strain relaxation in epitaxial thin films of multiferroic TbMnO3 probed by X-ray diffractometry and micro-Raman spectroscopy

NASA Astrophysics Data System (ADS)

Hu, Y.; Stender, D.; Medarde, M.; Lippert, T.; Wokaun, A.; Schneider, C. W.

2013-08-01

A detailed structural XRD analysis of (1 1 0)-oriented TbMnO3 thin films grown on (1 1 0)-YAlO3 substrates shows the co-existence of a strained and relaxed "sublayer" within the films due to strain relaxation during epitaxial growth by pulsed laser deposition. The substrate-film lattice mismatch yields a compressive strain anisotropy along the two in-plane directions, i.e. [1 -1 0] and [0 0 1] and a monoclinic distortion. A further manifestation of the growth-induced strain is the hardening of Raman active modes as a result of changed atomic motions along the [1 -1 0] and [0 0 1] directions.

A new nanospray drying method for the preparation of nicergoline pure nanoparticles

NASA Astrophysics Data System (ADS)

Martena, Valentina; Censi, Roberta; Hoti, Ela; Malaj, Ledjan; Di Martino, Piera

2012-06-01

Three different batches of pure nanoparticles (NPs) of nicergoline (NIC) were prepared by spray drying a water:ethanol solution by a new Nano Spray Dryer Büchi B-90. Spherical pure NPs were obtained, and several analytical techniques such as differential scanning calorimetry and X-ray powder diffractometry permitted to assess their amorphous character. A comparison of the solubility, intrinsic dissolution, and drug release of original particles and pure amorphous NPs were determined, revealing an interesting improvement of biopharmaceutical properties of amorphous NPs, due to both amorphous properties and nanosize dimensions. Since in a previous work, the high-thermodynamic stability of amorphous NIC was demonstrated, this study is addressed toward the formulation of NIC as pure amorphous NPs.

Laboratory-size three-dimensional x-ray microscope with Wolter type I mirror optics and an electron-impact water window x-ray source

NASA Astrophysics Data System (ADS)

Ohsuka, Shinji; Ohba, Akira; Onoda, Shinobu; Nakamoto, Katsuhiro; Nakano, Tomoyasu; Miyoshi, Motosuke; Soda, Keita; Hamakubo, Takao

2014-09-01

We constructed a laboratory-size three-dimensional water window x-ray microscope that combines wide-field transmission x-ray microscopy with tomographic reconstruction techniques, and observed bio-medical samples to evaluate its applicability to life science research fields. It consists of a condenser and an objective grazing incidence Wolter type I mirror, an electron-impact type oxygen Kα x-ray source, and a back-illuminated CCD for x-ray imaging. A spatial resolution limit of around 1.0 line pairs per micrometer was obtained for two-dimensional transmission images, and 1-μm scale three-dimensional fine structures were resolved.

Mechanical design of thin-film diamond crystal mounting apparatus for coherence preservation hard x-ray optics

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

Shu, Deming, E-mail: shu@aps.anl.gov; Shvyd’ko, Yuri V.; Stoupin, Stanislav

2016-07-27

A new thin-film diamond crystal mounting apparatus has been designed at the Advanced Photon Source (APS) for coherence preservation hard x-ray optics with optimized thermal contact and minimized crystal strain. This novel mechanical design can be applied to new development in the field of: x-ray optics cavities for hard x-ray free-electron laser oscillators (XFELOs), self-seeding monochromators for hard x-ray free-electron laser (XFEL) with high average thermal loading, high heat load diamond crystal monochromators and beam-sharing/beam-split-and-delay devices for XFEL facilities and future upgraded high-brightness coherent x-ray source in the MBA lattice configuration at the APS.

Laboratory-size three-dimensional x-ray microscope with Wolter type I mirror optics and an electron-impact water window x-ray source.

PubMed

Ohsuka, Shinji; Ohba, Akira; Onoda, Shinobu; Nakamoto, Katsuhiro; Nakano, Tomoyasu; Miyoshi, Motosuke; Soda, Keita; Hamakubo, Takao

2014-09-01

We constructed a laboratory-size three-dimensional water window x-ray microscope that combines wide-field transmission x-ray microscopy with tomographic reconstruction techniques, and observed bio-medical samples to evaluate its applicability to life science research fields. It consists of a condenser and an objective grazing incidence Wolter type I mirror, an electron-impact type oxygen Kα x-ray source, and a back-illuminated CCD for x-ray imaging. A spatial resolution limit of around 1.0 line pairs per micrometer was obtained for two-dimensional transmission images, and 1-μm scale three-dimensional fine structures were resolved.

The Effects of Low- and High-Energy Cutoffs on Solar Flare Microwave and Hard X-Ray Spectra

NASA Technical Reports Server (NTRS)

Holman, G. D.; Oegerle, William (Technical Monitor)

2002-01-01

Microwave and hard x-ray spectra provide crucial information about energetic electrons and their environment in solar flares. These spectra are becoming better determined with the Owens Valley Solar Array (OVSA) and the recent launch of the Ramaty High Energy Solar Spectroscopic Imager (RHESSI). The proposed Frequency Agile Solar Radiotelescope (FASR) promises even greater advances in radio observations of solar flares. Both microwave and hard x-ray spectra are sensitive to cutoffs in the electron distribution function. The determination of the high-energy cutoff from these spectra establishes the highest electron energies produced by the acceleration mechanism, while determination of the low-energy cutoff is crucial to establishing the total energy in accelerated electrons. This paper will show computations of the effects of both high- and low-energy cutoffs on microwave and hard x-ray spectra. The optically thick portion of a microwave spectrum is enhanced and smoothed by a low-energy cutoff, while a hard x-ray spectrum is flattened below the cutoff energy. A high-energy cutoff steepens the microwave spectrum and increases the wavelength at which the spectrum peaks, while the hard x-ray spectrum begins to steepen at photon energies roughly an order of magnitude below the electron cutoff energy. This work discusses how flare microwave and hard x-ray spectra can be analyzed together to determine these electron cutoff energies. This work is supported in part by the NASA Sun-Earth Connection Program.

Creation of X-Ray Transparency of Matter by Stimulated Elastic Forward Scattering.

PubMed

Stöhr, J; Scherz, A

2015-09-04

X-ray absorption by matter has long been described by the famous Beer-Lambert law. Here, we show how this fundamental law needs to be modified for high-intensity coherent x-ray pulses, now available at x-ray free electron lasers, due to the onset of stimulated elastic forward scattering. We present an analytical expression for the modified polarization-dependent Beer-Lambert law for the case of resonant core-to-valence electronic transitions and incident transform limited x-ray pulses. Upon transmission through a solid, the resonant absorption and dichroic contrasts are found to vanish with increasing x-ray intensity, with the stimulation threshold lowered by orders of magnitude through a resonant superradiantlike effect. Our results have broad implications for the study of matter with x-ray lasers.

Creation of X-Ray Transparency of Matter by Stimulated Elastic Forward Scattering

NASA Astrophysics Data System (ADS)

Stöhr, J.; Scherz, A.

2015-09-01

X-ray absorption by matter has long been described by the famous Beer-Lambert law. Here, we show how this fundamental law needs to be modified for high-intensity coherent x-ray pulses, now available at x-ray free electron lasers, due to the onset of stimulated elastic forward scattering. We present an analytical expression for the modified polarization-dependent Beer-Lambert law for the case of resonant core-to-valence electronic transitions and incident transform limited x-ray pulses. Upon transmission through a solid, the resonant absorption and dichroic contrasts are found to vanish with increasing x-ray intensity, with the stimulation threshold lowered by orders of magnitude through a resonant superradiantlike effect. Our results have broad implications for the study of matter with x-ray lasers.

Density gradient free electron collisionally excited X-ray laser

DOEpatents

Campbell, Edward M.; Rosen, Mordecai D.

1989-01-01

An operational X-ray laser (30) is provided that amplifies 3p-3s transition X-ray radiation along an approximately linear path. The X-ray laser (30) is driven by a high power optical laser. The driving line focused optical laser beam (32) illuminates a free-standing thin foil (34) that may be associated with a substrate (36) for improved structural integrity. This illumination produces a generally cylindrically shaped plasma having an essentially uniform electron density and temperature, that exists over a long period of time, and provides the X-ray laser gain medium. The X-ray laser (30) may be driven by more than one optical laser beam (32, 44). The X-ray laser (30) has been successfully demonstrated to function in a series of experimental tests.

High sensitive X-ray films to detect electron showers in 100 GeV region

NASA Technical Reports Server (NTRS)

Taira, T.; Shirai, T.; Tateyama, N.; Torii, S.; Nishimura, J.; Fujii, M.; Yoshida, A.; Aizu, H.; Nomura, Y.; Kazuno, M.

1985-01-01

Nonscreen type X-ray films were used in emulsion chamber experiments to detect high energy showers in cosmic rays. Ranges of the detection threshold is from about 1 to 2 TeV depending on the exposure conditions. Different types of X-ray films and sheets i.e. high sensitive screen type X-ray films and luminescence sheets were tested. The threshold of the shower detection is found to be about 200 GeV, which is much lower than that of nonscreen type X-ray films. These films are useful to detect showers in the medium energy range, a few hundred GeV, of the cosmic ray electrons.

Polymeric and Molecular Materials for Advanced Organic Electronics

DTIC Science & Technology

2014-10-20

x - ray reflectivity, grazing incidence x - ray scattering, cyclic voltam- metry...6). ix These materials are characterized by AFM, conducting AFM, XPS, x - ray reflectivity (XRR), standing wave x - ray reflectivity (SWXRR), x - ray ...radiation hard - ness measurements, and quantum chemical computation of dielectric constants. Remark- ably, for semiconductors as diverse

Improved performances of CIBER-X: a new tabletop laser-driven electron and x-ray source

NASA Astrophysics Data System (ADS)

Girardeau-Montaut, Jean-Pierre; Kiraly, Bela; Girardeau-Montaut, Claire

2000-11-01

We present the most recent data concerning the performances of the table-top laser driven electron and x-ray source developed in our laboratory. X-ray pulses are produced by a three-step process which consists of the photoelectron emission from a thin metallic photocathode illuminated by 16 ps duration laser pulse at 213 nm. The e-gun is a standard pierce diode electrode type, in which electrons are accelerated by a cw electric fields of 12 MV/m. The photoinjector produced a train of 90 - 100 keV electron pulses of approximately 1 nC and 40 A peak current at a repetition rate of 10 Hz. The electrons, transported outside the diode, are focused onto a target of thulium by magnetic fields produced by two electromagnetic coils to produce x-rays. Applications to low dose imagery of inert and living materials are also presented.

AN OSCILLATOR CONFIGURATION FOR FULL REALIZATION OF HARD X-RAY FREE ELECTRON LASER*

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

Kim, K.-J.; Kolodziej, T.; Lindberg, R. R.

2017-06-01

An x-ray free electron laser oscillator (XFELO) is feasible by employing an X-ray cavity with Bragg mirrors such as diamond crystals. An XFELO at the 5th harmonic frequency may be implemented at the LCLS II using its 4 GeV superconducting linac, producing stable, fully coherent, high-spectral-purity hard x-rays. In addition, its output can be a coherent seed to the LCLS amplifier for stable, high-power, femto-second x-ray pulses. We summarize the recent progress in various R&D efforts addressing critical issues for realizing an XFELO at LCLS II.

In-Orbit Performance of the Digital Electronics for the X-Ray Microcalorimeter Onboard the Hitomi Satellite

NASA Astrophysics Data System (ADS)

Tsujimoto, M.; Tashiro, M. S.; Ishisaki, Y.; Yamada, S.; Seta, H.; Mitsuda, K.; Boyce, K. R.; Eckart, M. E.; Kilbourne, C. A.; Leutenegger, M. A.; Porter, F. S.; Kelley, R. L.

2018-03-01

The pulse shape processor is the onboard digital electronics unit of the X-ray microcalorimeter instrument—the soft X-ray spectrometer—onboard the Hitomi satellite. It processes X-ray events using the optimum filtering with limited resources. It was operated for 36 days in orbit continuously without issues and met the requirement of processing a 150 s^{-1} event rate during the observation of bright sources. Here, we present the results obtained in orbit, focusing on its performance as the onboard digital signal processing unit of an X-ray microcalorimeter.

Normal incidence x-ray mirror for chemical microanalysis

DOEpatents

Carr, M.J.; Romig, A.D. Jr.

1987-08-05

An x-ray mirror for both electron column instruments and micro x-ray fluorescence instruments for making chemical, microanalysis comprises a non-planar mirror having, for example, a spherical reflecting surface for x-rays comprised of a predetermined number of alternating layers of high atomic number material and low atomic number material contiguously formed on a substrate and whose layers have a thickness which is a multiple of the wavelength being reflected. For electron column instruments, the wavelengths of interest lie above 1.5nm, while for x-ray fluorescence instruments, the range of interest is below 0.2nm. 4 figs.

Temporal cross-correlation of x-ray free electron and optical lasers using soft x-ray pulse induced transient reflectivity.

PubMed

Krupin, O; Trigo, M; Schlotter, W F; Beye, M; Sorgenfrei, F; Turner, J J; Reis, D A; Gerken, N; Lee, S; Lee, W S; Hays, G; Acremann, Y; Abbey, B; Coffee, R; Messerschmidt, M; Hau-Riege, S P; Lapertot, G; Lüning, J; Heimann, P; Soufli, R; Fernández-Perea, M; Rowen, M; Holmes, M; Molodtsov, S L; Föhlisch, A; Wurth, W

2012-05-07

The recent development of x-ray free electron lasers providing coherent, femtosecond-long pulses of high brilliance and variable energy opens new areas of scientific research in a variety of disciplines such as physics, chemistry, and biology. Pump-probe experimental techniques which observe the temporal evolution of systems after optical or x-ray pulse excitation are one of the main experimental schemes currently in use for ultrafast studies. The key challenge in these experiments is to reliably achieve temporal and spatial overlap of the x-ray and optical pulses. Here we present measurements of the x-ray pulse induced transient change of optical reflectivity from a variety of materials covering the soft x-ray photon energy range from 500eV to 2000eV and outline the use of this technique to establish and characterize temporal synchronization of the optical-laser and FEL x-ray pulses.

X-Ray Detector for 1 to 30 keV

NASA Technical Reports Server (NTRS)

Alcorn, G.; Jackson, J., Jr; Grant, P.; Marshall, F.

1983-01-01

Array of silicon X-ray detecting diodes measures photon energy and provides image of X-ray pattern. Regardless of thickness of new X-ray detector, depletion region extends through it. Impinging X-rays generate electrons in quantities proportional to X-ray energy. X-ray detector is mated to chargecoupled-device array for image generation and processing. Useful in industrial part inspection, pulsed-plasma research and medical application.

Reflex Triode X-Ray Source Research on Gamble

DTIC Science & Technology

2007-06-01

dosimeters ( TLDs ) located at the vacuum window (18-27 cm from the converter), near the pinhole camera and near the image plate. II. EXPERIMENTAL...MeV- electron beams to thin converters in order to optimize emission of sub-100- keV x-rays. Thin converters reduce self-absorption of low-energy...x-rays, but the beam electrons must pass many times through the converter for efficient x-ray production. The triode configuration was found to be

Precession technique and electron diffractometry as new tools for crystal structure analysis and chemical bonding determination.

PubMed

Avilov, A; Kuligin, K; Nicolopoulos, S; Nickolskiy, M; Boulahya, K; Portillo, J; Lepeshov, G; Sobolev, B; Collette, J P; Martin, N; Robins, A C; Fischione, P

2007-01-01

We have developed a new fast electron diffractometer working with high dynamic range and linearity for crystal structure determinations. Electron diffraction (ED) patterns can be scanned serially in front of a Faraday cage detector; the total measurement time for several hundred ED reflections can be tens of seconds having high statistical accuracy for all measured intensities (1-2%). This new tool can be installed to any type of TEM without any column modification and is linked to a specially developed electron beam precession "Spinning Star" system. Precession of the electron beam (Vincent-Midgley technique) reduces dynamical effects allowing also use of accurate intensities for crystal structure analysis. We describe the technical characteristics of this new tool together with the first experimental results. Accurate measurement of electron diffraction intensities by electron diffractometer opens new possibilities not only for revealing unknown structures, but also for electrostatic potential determination and chemical bonding investigation. As an example, we present detailed atomic bonding information of CaF(2) as revealed for the first time by precise electron diffractometry.

Metalloprotein structures at ambient conditions and in real-time: biological crystallography and spectroscopy using X-ray free electron lasers

DOE PAGES

Kern, Jan; Yachandra, Vittal K.; Yano, Junko

2015-09-02

We have studied the structure of enzymes and the chemistry at the catalytic sites, intensively and have acquired an understanding of the atomic-scale chemistry which requires a new approach beyond steady state X-ray crystallography and X-ray spectroscopy at cryogenic temperatures. Following the dynamic changes in the geometric and electronic structure of metallo-enzymes at ambient conditions, while overcoming the severe X-ray-induced changes to the redox active catalytic center, is key for deriving reaction mechanisms. Such studies become possible by the intense and ultra-short femtosecond (fs) X-ray pulses from an X-ray free electron laser (XFEL) by acquiring a signal before the samplemore » is destroyed. Our review describes the recent and pioneering uses of XFELs to study the protein structure and dynamics of metallo-enzymes using crystallography and scattering, as well as the chemical structure and dynamics of the catalytic complexes (charge, spin, and covalency) using spectroscopy during the reaction to understand the electron-transfer processes and elucidate the mechanism.« less

Metalloprotein structures at ambient conditions and in real-time: biological crystallography and spectroscopy using X-ray free electron lasers

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

Kern, Jan; Yachandra, Vittal K.; Yano, Junko

We have studied the structure of enzymes and the chemistry at the catalytic sites, intensively and have acquired an understanding of the atomic-scale chemistry which requires a new approach beyond steady state X-ray crystallography and X-ray spectroscopy at cryogenic temperatures. Following the dynamic changes in the geometric and electronic structure of metallo-enzymes at ambient conditions, while overcoming the severe X-ray-induced changes to the redox active catalytic center, is key for deriving reaction mechanisms. Such studies become possible by the intense and ultra-short femtosecond (fs) X-ray pulses from an X-ray free electron laser (XFEL) by acquiring a signal before the samplemore » is destroyed. Our review describes the recent and pioneering uses of XFELs to study the protein structure and dynamics of metallo-enzymes using crystallography and scattering, as well as the chemical structure and dynamics of the catalytic complexes (charge, spin, and covalency) using spectroscopy during the reaction to understand the electron-transfer processes and elucidate the mechanism.« less

Experimental characterization of an ultra-fast Thomson scattering x-ray source with three-dimensional time and frequency-domain analysis

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

Kuba, J; Slaughter, D R; Fittinghoff, D N

We present a detailed comparison of the measured characteristics of Thomson backscattered x-rays produced at the PLEIADES (Picosecond Laser-Electron Interaction for the Dynamic Evaluation of Structures) facility at Lawrence Livermore National Laboratory to predicted results from a newly developed, fully three-dimensional time and frequency-domain code. Based on the relativistic differential cross section, this code has the capability to calculate time and space dependent spectra of the x-ray photons produced from linear Thomson scattering for both bandwidth-limited and chirped incident laser pulses. Spectral broadening of the scattered x-ray pulse resulting from the incident laser bandwidth, perpendicular wave vector components in themore » laser focus, and the transverse and longitudinal phase space of the electron beam are included. Electron beam energy, energy spread, and transverse phase space measurements of the electron beam at the interaction point are presented, and the corresponding predicted x-ray characteristics are determined. In addition, time-integrated measurements of the x-rays produced from the interaction are presented, and shown to agree well with the simulations.« less

Mitigation of Hot Electrons from Laser-Plasma Instabilities in Laser-Generated X-Ray Sources

NASA Astrophysics Data System (ADS)

Fein, Jeffrey R.

This thesis describes experiments to understand and mitigate energetic or "hot" electrons from laser-plasma instabilities (LPIs) in an effort to improve radiographic techniques using laser-generated x-ray sources. Initial experiments on the OMEGA-60 laser show evidence of an underlying background generated by x-rays with energies over 10 keV on radiographs using backlit pinhole radiography, whose source is consistent with hard x-rays from LPI-generated hot electrons. Mitigating this background can dramatically reduce uncertainties in measured object densities from radiographs and may be achieved by eliminating the target components in which LPIs are most likely to grow. Experiments were performed on the OMEGA-EP laser to study hot electron production from laser-plasma instabilities in high-Z plasmas relevant to laser-generated x-ray sources. Measurements of hard x-rays show a dramatic reduction in hot-electron energy going from low-Z CH to high-Z Au targets, in a manner that is consistent with steepening electron density profiles that were also measured. The profile-steepening, we infer, increased thresholds of LPIs and contributed to the reduced hot-electron production at higher Z. Possible mechanisms for generating hot electrons include the two-plasmon decay and stimulated Raman scattering instabilities driven by multiple laser beams. Radiation hydrodynamic simulations using the CRASH code predict that both of these instabilities were above threshold with linear threshold parameters that decreased with increasing Z due to steepening length-scales, as well as enhanced laser absorption and increased collisional and Landau damping of electron plasma waves. Another set of experiments were performed on the OMEGA-60 laser to test whether hard x-ray background could be mitigated in backlit pinhole imagers by controlling laser-plasma instabilities. Based on the results above, we hypothesized that LPIs and hot electrons that lead to hard x-ray background would be reduced by increasing the atomic number of the irradiated components in the pinhole imagers. Using higher-Z materials we demonstrate significant reduction in x-rays between 30-70 keV and 70% increase in the signal-to-background ratio. Based on this, a proposed backlighter and detector setup predicts a signal-to-background ratio of up to 4.5:1.

Calibration of high-dynamic-range, finite-resolution x-ray pulse-height spectrometers for extracting electron energy distribution data from the PFRC-2 device

NASA Astrophysics Data System (ADS)

Swanson, C.; Jandovitz, P.; Cohen, S. A.

2017-10-01

Knowledge of the full x-ray energy distribution function (XEDF) emitted from a plasma over a large dynamic range of energies can yield valuable insights about the electron energy distribution function (EEDF) of that plasma and the dynamic processes that create them. X-ray pulse height detectors such as Amptek's X-123 Fast SDD with Silicon Nitride window can detect x-rays in the range of 200eV to 100s of keV. However, extracting EEDF from this measurement requires precise knowledge of the detector's response function. This response function, including the energy scale calibration, the window transmission function, and the resolution function, can be measured directly. We describe measurements of this function from x-rays from a mono-energetic electron beam in a purpose-built gas-target x-ray tube. Large-Z effects such as line radiation, nuclear charge screening, and polarizational Bremsstrahlung are discussed.

X-Ray Microanalytic Concentration Measurements in Unsectioned Specimens: a Technique and its Application to Zinc, Manganese, and Iron Enriched Mechanical Structures of Organisms from Three Phyla

NASA Astrophysics Data System (ADS)

Schofield, Robert M. S.

A method for measuring concentrations of minor elements in microscopic volumes of heterogeneous, unsectioned biological specimens using an ion microprobe is developed. The element quantity is obtained from PIXE (Proton Induced X-ray Emission) and the total quantity of material is derived from STIM (Scanning Transmission Ion Microscopy) energy loss measurements. Sources of error, including changes in x-ray production cross section with proton energy and absorption of induced x-rays, are discussed and a method of calculating the total measurement uncertainty, typically about 25% here, is developed. The measurement accuracy is shown to be improved for symmetric specimens, and a method of using the bremsstrahlung background to correct for x-ray attenuation within irregular specimens is developed. Methods for measuring local concentrations in internal features are also discussed. With this technique, scorpions were found to contain cuticular accumulations of one or more heavy metals (manganese up to 5% of dry weight, iron up to 8%, zinc up to 24%) in the chelicera, pedipalp denticles, tarsal claws, and stingers; different region soften contained different metals. The stingers are argued to be of particular interest because they are not homologous to legs. Similar accumulations were found in spiders, some other chelicerates and crustaceans. Previous reports of manganese and zinc accumulations in insect and worm mouth parts were augmented with local concentration measurements and with the detection of other enrichment features (such as 6% iron in the paragnaths of the worm Nereis vexillosa). Zinc accumulations (up to only 0.1%) were also found in the tips of the teeth of a hagfish, Myxine + glutinosa. X-ray images of several of these features are presented. It is argued that the extreme magnitude of some concentration values suggests that some metals are incorporated in unusual biominerals rather than organically bound. Results of x-ray diffractometry and Vickers microhardness measurements are reported although the results are inconclusive. The atomic ratio of zinc to chlorine in these accumulations is shown not to be constant. It is suggested from their typical locations that at least two of the observed accumulation patterns impart different mechanical properties to the cuticle.

Mode-Locked Multichromatic X-Rays in a Seeded Free-Electron Laser for Single-Shot X-Ray Spectroscopy

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

Xiang, Dao; Ding, Yuantao; Raubenheimer, Tor

2012-05-10

We present the promise of generating gigawatt mode-locked multichromatic x rays in a seeded free-electron laser (FEL). We show that, by using a laser to imprint periodic modulation in electron beam phase space, a single-frequency coherent seed can be amplified and further translated to a mode-locked multichromatic output in an FEL. With this configuration the FEL output consists of a train of mode-locked ultrashort pulses which span a wide frequency gap with a series of equally spaced sharp lines. These gigawatt multichromatic x rays may potentially allow one to explore the structure and dynamics of a large number of atomicmore » states simultaneously. The feasibility of generating mode-locked x rays ranging from carbon K edge ({approx}284 eV) to copper L{sub 3} edge ({approx}931 eV) is confirmed with numerical simulation using the realistic parameters of the linac coherent light source (LCLS) and LCLS-II. We anticipate that the mode-locked multichromatic x rays in FELs may open up new opportunities in x-ray spectroscopy (i.e. resonant inelastic x-ray scattering, time-resolved scattering and spectroscopy, etc.).« less

Rat Phantom Depth Dose Studies in Electron, X-ray, Gamma-Ray, and Reactor Radiation Fields

DTIC Science & Technology

1986-12-01

i©™D©/^ ^1[P@^T Rat phantom depth dose studies in electron , Xrayf gamma-ray, and reactor radiation fields M. Dooley D. M. Eagleson G. H. Zeman...energy electrons , bremsstrahlung, and mixed neutron/gamma radiation fields are sometimes used in radiobiological experiments employing rats. This report...have revealed differing sensitivities of experimental animals that have been exposed to cobalt-60 photons, high-energy electrons , high-energy X rays

CORRELATION OF HARD X-RAY AND WHITE LIGHT EMISSION IN SOLAR FLARES

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

Kuhar, Matej; Krucker, Säm; Battaglia, Marina

A statistical study of the correlation between hard X-ray and white light emission in solar flares is performed in order to search for a link between flare-accelerated electrons and white light formation. We analyze 43 flares spanning GOES classes M and X using observations from the Reuven Ramaty High Energy Solar Spectroscopic Imager and Helioseismic and Magnetic Imager. We calculate X-ray fluxes at 30 keV and white light fluxes at 6173 Å summed over the hard X-ray flare ribbons with an integration time of 45 s around the peak hard-X ray time. We find a good correlation between hard X-raymore » fluxes and excess white light fluxes, with a highest correlation coefficient of 0.68 for photons with energy of 30 keV. Assuming the thick target model, a similar correlation is found between the deposited power by flare-accelerated electrons and the white light fluxes. The correlation coefficient is found to be largest for energy deposition by electrons above ∼50 keV. At higher electron energies the correlation decreases gradually while a rapid decrease is seen if the energy provided by low-energy electrons is added. This suggests that flare-accelerated electrons of energy ∼50 keV are the main source for white light production.« less

Clusters in intense x-ray pulses

NASA Astrophysics Data System (ADS)

Bostedt, Christoph

2012-06-01

Free-electron lasers can deliver extremely intense, coherent x-ray flashes with femtosecond pulse length, opening the door for imaging single nanoscale objects in a single shot. All matter irradiated by these intense x-ray pulses, however, will be transformed into a highly-excited non-equilibrium plasma within femtoseconds. During the x-ray pulse complex electron dynamics and the onset of atomic disorder will be induced, leading to a time-varying sample. We have performed first experiments about x-ray laser pulse -- cluster interaction with a combined spectroscopy and imaging approach at both, the FLASH free electron laser in Hamburg (Germany) and the LCLS x-ray free-electron laser in Stanford (California). Atomic clusters are ideal for investigating the light - matter interaction because their size can be tuned from the molecular to the bulk regime, thus allowing to distinguish between intra and inter atomic processes. Imaging experiments with xenon clusters show power-density dependent changes in the scattering patterns. Modeling the scattering data indicates that the optical constants of the clusters change during the femtosecond pulse due to the transient creation of high charge states. The results show that ultra fast scattering is a promising approach to study transient states of matter on a femtosecond time scale. Coincident recording of time-of-flight spectra and scattering patterns allows the deconvolution of focal volume and particle size distribution effects. Single-shot single-particle experiments with keV x-rays reveal that for the highest power densities an highly excited and hot cluster plasma is formed for which recombination is suppressed. Time resolved infrared pump -- x-ray probe experiments have started. Here, the clusters are pumped into a nanoplasma state and their time evolution is probed with femtosecond x-ray scattering. The data show strong variations in the scattering patterns stemming from electronic reconfigurations in the cluster plasma. The results will be compared to theoretical predictions and discussed in light of current developments at free-electron laser sources.

Photoluminescence studies on Cd(1-x)Zn(x)S:Mn2+ nanocrystals.

PubMed

Sethi, Ruchi; Kumar, Lokendra; Pandey, A C

2009-09-01

Highly monodispersed, undoped and doped with Mn2+, binary and ternary (CdS, ZnS, Cd(1-x)Zn(x)S) compound semiconductor nanocrystals have been synthesized by co-precipitation method using citric acid as a stabilizer. As prepared sample are characterized by X-ray diffraction, Small angle X-ray scattering, Transmission electron microscope, Optical absorption and Photoluminescence spectroscopy, for their optical and structural properties. X-ray diffraction, Small angle X-ray scattering and Transmission electron microscope results confirm the preparation of monodispersed nanocrystals. Photoluminescence studies show a significant blue shift in the wavelength with an increasing concentration of Zn in alloy nanocrystals.

Surface microstructure and high temperature corrosion resistance of arc-sprayed FeCrAl coating irradiated by high current pulsed electron beam

NASA Astrophysics Data System (ADS)

Hao, Shengzhi; Zhao, Limin; He, Dongyun

2013-10-01

The surface microstructure of arc-sprayed FeCrAl coating irradiated by high current pulsed electron beam (HCPEB) with long pulse duration of 200 μs was characterized by using optical microscopy, scanning electron microscopy and X-ray diffractometry. The distribution of chemical composition in modified surface layer was measured with electron probe micro-analyzer. The high temperature corrosion resistance of FeCrAl coating was tested in a saturated Na2SO4 and K2SO4 solution at 650 °C. After HCPEB irradiation, the coarse surface of arc-sprayed coating was changed as discrete bulged nodules with smooth and compact appearance. When using low energy density of 20 J/cm2, the surface modified layer was continuous entirely with an average melting depth of ˜30 μm. In the surface remelted layer, Fe and Cr elements gave a uniform distribution, while Al and O elements agglomerated particularly at the concave part between nodule structures to form α-Al2O3 phase. After high temperature corrosion tests, the FeCrAl coating treated with HCPEB of 20 J/cm2 remained a glossy surface with weight increment of ˜51 mg/cm2, decreased by 20% as compared to the initial sample. With the increasing energy density of HCPEB irradiation, the integrity of surface modified layer got segmented due to the formation of larger bulged nodules and cracks at the concave parts. For the HCPEB irradiation of 40 J/cm2, the high temperature corrosion resistance of FeCrAl coating was deteriorated drastically.

A Flash X-Ray Facility for the Naval Postgraduate School

DTIC Science & Technology

1985-06-01

ionizing radiation, *• NPS has had active programs with a Van de Graaff generator, a reactor, radioactive sources, X-ray machines and a linear electron ...interaction of radiation with matter and with coherent radiation. Currently the most active program is at the linear electron accelerator which over...twenty years has produced some 75 theses. The flash X-ray machine was obtained to expan-i and complement the capabilities of the linear electron

Modeling the gain of inner-shell X-ray laser transitions in neon, argon, and copper driven by X-ray free electron laser radiation using photo-ionization and photo-excitation processes

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

Nilsen, Joseph

2015-12-16

Using an X-ray free electron laser (XFEL) at 960 eV to photo-ionize the 1s electron in neutral neon followed by lasing on the 2p-1s transition in singly-ionized neon, an inner-shell X-ray laser was demonstrated at 849 eV in singly-ionized neon gas several years ago. It took decades to demonstrate this scheme, because it required a very strong X-ray source that could photo-ionize the 1s (K shell) electron in neon on a timescale comparable to the intrinsic Auger lifetime in neon of 2 fs. In this paper, we model the neon inner shell X-ray laser under similar conditions to those usedmore » in the XFEL experiments at the SLAC Linac Coherent Light Source (LCLS), and show how we can improve the efficiency of the neon laser and reduce the drive requirements by tuning the XFEL to the 1s-3p transition in neutral neon in order to create gain on the 2p-1s line in neutral neon. We also show how the XFEL could be used to photo-ionize L-shell electrons to drive gain on n = 3–2 transitions in singly-ionized Ar and Cu plasmas. Furthermore, these bright, coherent, and monochromatic X-ray lasers may prove very useful for doing high-resolution spectroscopy and for studying non-linear process in the X-ray regime.« less

Probing molecular dynamics in solution with x-ray valence-to-core spectroscopy

NASA Astrophysics Data System (ADS)

Doumy, Gilles; March, Anne Marie; Tu, Ming-Feng; Al Haddad, Andre; Southworth, Stephen; Young, Linda; Walko, Donald; Bostedt, Christoph

2017-04-01

Hard X-ray spectroscopies are powerful tools for probing the electronic and geometric structure of molecules in complex or disordered systems and have been particularly useful for studying molecules in the solution phase. They are element specific, sensitive to the electronic structure and the local arrangements of surrounding atoms of the element being selectively probed. When combined in a pump-probe scheme with ultrafast lasers, X-ray spectroscopies can be used to track the evolution of structural changes that occur after photoexcitation. Efficient use of hard x-ray radiation coming from high brilliance synchrotrons and upcoming high repetition rate X-ray Free Electron Lasers requires MHz repetition rate lasers and data acquisition systems. High information content Valence-to-Core x-ray emission is directly sensitive to the molecular orbitals involved in photochemistry. We report on recent progress towards fully enabling this photon-hungry technique for the study of time-resolved molecular dynamics, including efficient detection and use of polychromatic x-ray micro-probe at the Advanced Photon Source. Work was supported by the U.S. Department of Energy, Office of Science, Chemical Sciences, Geosciences, and Biosciences Division.

Low-energy d-d excitations in MnO studied by resonant x-ray fluorescence spectroscopy

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

Butorin, S.M.; Guo, J.; Magnuson, M.

1997-04-01

Resonant soft X-ray emission spectroscopy has been demonstrated to possess interesting abilities for studies of electronic structure in various systems, such as symmetry probing, alignment and polarization dependence, sensitivity to channel interference, etc. In the present abstract the authors focus on the feasibility of resonant soft X-ray emission to probe low energy excitations by means of resonant electronic X-ray Raman scattering. Resonant X-ray emission can be regarded as an inelastic scattering process where a system in the ground state is transferred to a low excited state via a virtual core excitation. The energy closeness to a core excitation of themore » exciting radiation enhances the (generally) low probability for inelastic scattering at these wavelengths. Therefore soft X-ray emission spectroscopy (in resonant electronic Raman mode) can be used to study low energy d-d excitations in transition metal systems. The involvement of the intermediate core state allows one to use the selection rules of X-ray emission, and the appearance of the elastically scattered line in the spectra provides the reference to the ground state.« less

Construction of a magnetic bottle spectrometer and its application to pulse duration measurement of X-ray laser using a pump-probe method

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

Namba, S., E-mail: namba@hiroshima-u.ac.jp; Hasegawa, N.; Kishimoto, M.

To characterize the temporal evolution of ultrashort X-ray pulses emitted by laser plasmas using a pump-probe method, a magnetic bottle time-of-flight electron spectrometer is constructed. The design is determined by numerical calculations of a mirror magnetic field and of the electron trajectory in a flight tube. The performance of the spectrometer is characterized by measuring the electron spectra of xenon atoms irradiated with a laser-driven plasma X-ray pulse. In addition, two-color above-threshold ionization (ATI) experiment is conducted for measurement of the X-ray laser pulse duration, in which xenon atoms are simultaneously irradiated with an X-ray laser pump and an IRmore » laser probe. The correlation in the intensity of the sideband spectra of the 4d inner-shell photoelectrons and in the time delay of the two laser pulses yields an X-ray pulse width of 5.7 ps, in good agreement with the value obtained using an X-ray streak camera.« less

The Focusing Optics X-ray Solar Imager (FOXSI): Instrument and First Flight

NASA Astrophysics Data System (ADS)

Glesener, Lindsay; Christe, S.; Ishikawa, S.; Ramsey, B.; Takahashi, T.; Saito, S.; Lin, R. P.; Krucker, S.; FOXSI Team

2013-04-01

Understanding electron acceleration in solar flares requires hard X-ray studies with greater sensitivity and dynamic range than are available with current solar hard X-ray observers (i.e. the RHESSI spacecraft). Both these capabilities can be advanced by the use of direct focusing optics instead of the indirect Fourier methods of current and previous generations. The Focusing Optics X-ray Solar Imager (FOXSI) sounding rocket payload demonstrates the feasibility and usefulness of hard X-ray focusing optics for solar observation. FOXSI flew for the first time on 2012 November 2, producing images and spectra of a microflare and performing a search for nonthermal X-rays from the quiet Sun. Such measurements are important for characterizing the impact of small "nanoflares" on the solar coronal heating problem. A spaceborne solar observer featuring similar optics could make detailed observations of hard X-rays from flare-accelerated electrons, identifying and characterizing particle acceleration sites and mapping out paths of energetic electrons as they leave these sites and propagate throughout the solar corona. Solar observations from NuSTAR are also expected to be an important step in this direction.

Total rate imaging with x-rays (TRIX)--a simple method of forming a non-projection x-ray image in the SEM using an energy dispersive detector and its application to biological specimens.

PubMed

Ingram, P; Shelburne, J D

1980-01-01

X-ray images can be formed in a conventional scanning electron microscope equipped with a Si(Li) energy dispersive spectrometer. All the x-ray events generated in the electron beam scanning process are synchronously displayed in the same manner as for dot maps. The quasi-digital image formed using Total Rate Imaging with X-rays (TRIX) exhibits good gray scale contrast and is dependent on topography, orientation and atomic number. Although this latter dependence is complex, it has been found useful in locating several types of inclusions in lung tissue (silicosis), human alveolar macrophages and cigarette smoke condensate. This is because of the greater depth of penetration of x-rays than backscattered electrons (BSE) usually used for such localizations in a matrix, and the negligible sensitivity of the Si(Li) detector to x-rays from an organic biological matrix. The optimum procedure is to use a combination of TRIX and BSE to investigate such specimens.

High-resolution multi-MeV x-ray radiography using relativistic laser-solid interaction

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

Courtois, C.; Compant La Fontaine, A.; Barbotin, M.

2011-02-15

When high intensity ({>=}10{sup 19} W cm{sup -2}) laser light interacts with matter, multi-MeV electrons are produced. These electrons can be utilized to generate a MeV bremsstrahlung x-ray emission spectrum as they propagate into a high-Z solid target positioned behind the interaction area. The short duration (<10 ps) and the small diameter (<500 {mu}m) of the x-ray pulse combined with the MeV x-ray spectrum offers an interesting alternative to conventional bremsstrahlung x-ray sources based on an electron accelerator used to radiograph dense, rapidly moving objects. In experiments at the Omega EP laser, a multi-MeV x-ray source is characterized consistently withmore » number of independent diagnostics. An unfiltered x-ray dose of approximately 2 rad in air at 1 m and a source diameter of less than 350 {mu}m are inferred. Radiography of a complex and high area density (up to 61 g/cm{sup 2}) object is then performed with few hundred microns spatial resolution.« less

Surface applicator of a miniature X-ray tube for superficial electronic brachytherapy of skin cancer.

PubMed

Kim, Hyun Nam; Lee, Ju Hyuk; Park, Han Beom; Kim, Hyun Jin; Cho, Sung Oh

2018-01-01

We designed and fabricated a surface applicator of a novel carbon nanotube (CNT)-based miniature X-ray tube for the use in superficial electronic brachytherapy of skin cancer. To investigate the effectiveness of the surface applicator, the performance of the applicator was numerically and experimentally analyzed. The surface applicator consists of a graphite flattening filter and an X-ray shield. A Monte Carlo radiation transport code, MCNP6, was used to optimize the geometries of both the flattening filter and the shield so that X-rays are generated uniformly over the desired region. The performance of the graphite filter was compared with that of conventional aluminum (Al) filters of different geometries using the numerical simulations. After fabricating a surface applicator, the X-ray spatial distribution was measured to evaluate the performance of the applicator. The graphite filter shows better spatial dose uniformity and less dose distortion than Al filters. Moreover, graphite allows easy fabrication of the flattening filter due to its low X-ray attenuation property, which is particularly important for low-energy electronic brachytherapy. The applicator also shows that no further X-ray shielding is required for the application because unwanted X-rays are completely protected. As a result, highly uniform X-ray dose distribution was achieved from the miniature X-ray tube mounted with the surface applicators. The measured values of both flatness and symmetry were less than 5% and the measured penumbra values were less than 1 mm. All these values satisfy the currently accepted tolerance criteria for radiation therapy. The surface applicator exhibits sufficient performance capability for their application in electronic brachytherapy of skin cancers. © 2017 American Association of Physicists in Medicine.

Resonant inelastic soft x-ray scattering of CdS: a two-dimensional electronic structure map approach

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

Weinhardt, L.; Fuchs, O.; Fleszar, A.

2008-09-24

Resonant inelastic x-ray scattering (RIXS) with soft x-rays is uniquely suited to study the elec-tronic structure of a variety of materials, but is currently limited by low (fluorescence yield) count rates. This limitation is overcome with a new high-transmission spectrometer that allows to measure soft x-ray RIXS"maps." The S L2,3 RIXS map of CdS is discussed and compared with density functional calculations. The map allows the extraction of decay channel-specific"absorp-tion spectra," giving detailed insight into the wave functions of occupied and unoccupied elec-tronic states.

Echo-Enabled X-Ray Vortex Generation

NASA Astrophysics Data System (ADS)

Hemsing, E.; Marinelli, A.

2012-11-01

A technique to generate high-brightness electromagnetic vortices with tunable topological charge at extreme ultraviolet and x-ray wavelengths is described. Based on a modified version of echo-enabled harmonic generation for free-electron lasers, the technique uses two lasers and two chicanes to produce high-harmonic microbunching of a relativistic electron beam with a corkscrew distribution that matches the instantaneous helical phase structure of the x-ray vortex. The strongly correlated electron distribution emerges from an efficient three-dimensional recoherence effect in the echo-enabled harmonic generation transport line and can emit fully coherent vortices in a downstream radiator for access to new research in x-ray science.

Calibration of a time-resolved hard-x-ray detector using radioactive sources

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

Stoeckl, C., E-mail: csto@lle.rochester.edu; Theobald, W.; Regan, S. P.

A four-channel, time-resolved, hard x-ray detector (HXRD) has been operating at the Laboratory for Laser Energetics for more than a decade. The slope temperature of the hot-electron population in direct-drive inertial confinement fusion experiments is inferred by recording the hard x-ray radiation generated in the interaction of the electrons with the target. Measuring the energy deposited by hot electrons requires an absolute calibration of the hard x-ray detector. A novel method to obtain an absolute calibration of the HXRD using single photons from radioactive sources was developed, which uses a thermoelectrically cooled, low-noise, charge-sensitive amplifier.

Time-resolved x-ray diffraction and Raman studies of the phase transition mechanisms of methane hydrate

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

Hirai, Hisako, E-mail: hirai@sci.ehime-u.ac.jp; Kadobayashi, Hirokazu; Hirao, Naohisa

The mechanisms by which methane hydrate transforms from an sI to sH structure and from an sH to filled-ice Ih structure were examined using time-resolved X-ray diffractometry (XRD) and Raman spectroscopy in conjunction with charge-coupled device camera observation under fixed pressure conditions. The XRD data obtained for the sI–sH transition at 0.8 GPa revealed an inverse correlation between sI and sH, suggesting that the sI structure is replaced by sH. Meanwhile, the Raman analysis demonstrated that although the 12-hedra of sI are retained, the 14-hedra are replaced sequentially by additional 12-hedra, modified 12-hedra, and 20-hedra cages of sH. With themore » sH to filled-ice Ih transition at 1.8 GPa, both the XRD and Raman data showed that this occurs through a sudden collapse of the sH structure and subsequent release of solid and fluid methane that is gradually incorporated into the filled-ice Ih to complete its structure. This therefore represents a typical reconstructive transition mechanism.« less

X-ray characterization of indium during melting

NASA Astrophysics Data System (ADS)

Gondi, P.; Montanari, R.; Costanza, G.

During melting of Indium the structure of solid and liquid phases have been investigated by X-ray diffractometry (XRD) in 1-g conditions. At the melting point T M a re-orientation of crystalline grains occurs in the solid phase. The texture change, unusually rapid for a thermally activated process, is attributed to an abnormal increase of vacancy concentration. This explanation is in agreement with the observed shifts of XRD peaks towards lower angles. As a consequence of the texture change, the lattice planes facing the first formed liquid are (002) and (101) planes, i.e. those planes allocating 1st and 2nd neighbours around a given atom with shell radii very close to the mean distance of nearest neighbours in liquid as obtained from the radial distribution function (RDF). Convective motions in the liquid can be eliminated by repeating the same XRD measurements in μ-g. To get the best experimental conditions it is discussed the possibility to use thin oxide films grown on the external surface of samples as containers during melting. This technique was already successfully tested by present investigators in the experiment ES 311 A-B carried out during the mission SPACELAB-1.

Multivariate Quantification of the Solid State Phase Composition of Co-Amorphous Naproxen-Indomethacin.

PubMed

Beyer, Andreas; Grohganz, Holger; Löbmann, Korbinian; Rades, Thomas; Leopold, Claudia S

2015-10-27

To benefit from the optimized dissolution properties of active pharmaceutical ingredients in their amorphous forms, co-amorphisation as a viable tool to stabilize these amorphous phases is of both academic and industrial interest. Reports dealing with the physical stability and recrystallization behavior of co-amorphous systems are however limited to qualitative evaluations based on the corresponding X-ray powder diffractograms. Therefore, the objective of the study was to develop a quantification model based on X-ray powder diffractometry (XRPD), followed by a multivariate partial least squares regression approach that enables the simultaneous determination of up to four solid state fractions: crystalline naproxen, γ-indomethacin, α-indomethacin as well as co-amorphous naproxen-indomethacin. For this purpose, a calibration set that covers the whole range of possible combinations of the four components was prepared and analyzed by XRPD. In order to test the model performances, leave-one-out cross validation was performed and revealed root mean square errors of validation between 3.11% and 3.45% for the crystalline molar fractions and 5.57% for the co-amorphous molar fraction. In summary, even four solid state phases, involving one co-amorphous phase, can be quantified with this XRPD data-based approach.

DSC, X-ray and FTIR studies of a gemfibrozil/dimethyl-β-cyclodextrin inclusion complex produced by co-grinding.

PubMed

Aigner, Z; Berkesi, O; Farkas, G; Szabó-Révész, P

2012-01-05

The steps of formation of an inclusion complex produced by the co-grinding of gemfibrozil and dimethyl-β-cyclodextrin were investigated by differential scanning calorimetry (DSC), X-ray powder diffractometry (XRPD) and Fourier transform infrared (FTIR) spectroscopy with curve-fitting analysis. The endothermic peak at 59.25°C reflecting the melting of gemfibrozil progressively disappeared from the DSC curves of the products on increase of the duration of co-grinding. The crystallinity of the samples too gradually decreased, and after 35min of co-grinding the product was totally amorphous. Up to this co-grinding time, XRPD and FTIR investigations indicated a linear correlation between the cyclodextrin complexation and the co-grinding time. After co-grinding for 30min, the ratio of complex formation did not increase. These studies demonstrated that co-grinding is a suitable method for the complexation of gemfibrozil with dimethyl-β-cyclodextrin. XRPD analysis revealed the amorphous state of the gemfibrozil-dimethyl-β-cyclodextrin product. FTIR spectroscopy with curve-fitting analysis may be useful as a semiquantitative analytical method for discriminating the molecular and amorphous states of gemfibrozil. Copyright © 2011 Elsevier B.V. All rights reserved.

Valence-electron configuration of Fe, Cr, and Ni in binary and ternary alloys from Kβ -to- Kα x-ray intensity ratios

NASA Astrophysics Data System (ADS)

Han, I.; Demir, L.

2009-11-01

Kβ -to- Kα x-ray intensity ratios of Fe, Cr, and Ni have been measured in pure metals and in alloys of FexNi1-x ( x=0.8 , 0.7, 0.6, 0.5, 0.4, 0.3, and 0.2), NixCr1-x ( x=0.8 , 0.6, 0.5, 0.4, and 0.2), FexCr1-x ( x=0.9 , 0.7, and 0.5), and FexCryNi1-(x+y) ( x=0.7-y=0.1 , x=0.5-y=0.2 , x=0.4-y=0.3 , x=0.3-y=0.3 , x=0.2-y=0.2 , and x=0.1-y=0.2 ) following excitation by 22.69 keV x rays from a 10 mCi C109d radioactive point source. The valence-electron configurations of these metals were determined by corporation of measured Kβ -to- Kα x-ray intensity ratios with the results of multiconfiguration Dirac-Fock calculation for various valence-electron configurations. Valence-electron configurations of 3d transition metals in alloys indicate significant differences with respect to the pure metals. Our analysis indicates that these differences arise from delocalization and/or charge transfer phenomena in alloys. Namely, the observed change of the valence-electron configurations of metals in alloys can be explained with the transfer of 3d electrons from one element to the other element and/or the rearrangement of electrons between 3d and 4s,4p states of individual metal atoms.

Deducing Electron Properties from Hard X-Ray Observations

NASA Technical Reports Server (NTRS)

Kontar, E. P.; Brown, J. C.; Emslie, A. G.; Hajdas, W.; Holman, G. D.; Hurford, G. J.; Kasparova, J.; Mallik, P. C. V.; Massone, A. M.; McConnell, M. L.;

X-ray compass for determining device orientation

DOEpatents

Da Silva, Luiz B.; Matthews, Dennis L.; Fitch, Joseph P.; Everett, Matthew J.; Colston, Billy W.; Stone, Gary F.

1999-01-01

An apparatus and method for determining the orientation of a device with respect to an x-ray source. In one embodiment, the present invention is coupled to a medical device in order to determine the rotational orientation of the medical device with respect to the x-ray source. In such an embodiment, the present invention is comprised of a scintillator portion which is adapted to emit photons upon the absorption of x-rays emitted from the x-ray source. An x-ray blocking portion is coupled to the scintillator portion. The x-ray blocking portion is disposed so as to vary the quantity of x-rays which penetrate the scintillator portion based upon the particular rotational orientation of the medical device with respect to the x-ray source. A photon transport mechanism is also coupled to the scintillator portion. The photon transport mechanism is adapted to pass the photons emitted from the scintillator portion to an electronics portion. By analyzing the quantity of the photons, the electronics portion determines the rotational orientation of the medical device with respect to the x-ray source.

X-ray compass for determining device orientation

DOEpatents

Da Silva, L.B.; Matthews, D.L.; Fitch, J.P.; Everett, M.J.; Colston, B.W.; Stone, G.F.

1999-06-15

An apparatus and method for determining the orientation of a device with respect to an x-ray source are disclosed. In one embodiment, the present invention is coupled to a medical device in order to determine the rotational orientation of the medical device with respect to the x-ray source. In such an embodiment, the present invention is comprised of a scintillator portion which is adapted to emit photons upon the absorption of x-rays emitted from the x-ray source. An x-ray blocking portion is coupled to the scintillator portion. The x-ray blocking portion is disposed so as to vary the quantity of x-rays which penetrate the scintillator portion based upon the particular rotational orientation of the medical device with respect to the x-ray source. A photon transport mechanism is also coupled to the scintillator portion. The photon transport mechanism is adapted to pass the photons emitted from the scintillator portion to an electronics portion. By analyzing the quantity of the photons, the electronics portion determines the rotational orientation of the medical device with respect to the x-ray source. 25 figs.

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

Establishing nonlinearity thresholds with ultraintense X-ray pulses

DOE PAGES

Szlachetko, Jakub; Hoszowska, Joanna; Dousse, Jean-Claude; ...

2016-09-13

X-ray techniques have evolved over decades to become highly refined tools for a broad range of investigations. Importantly, these approaches rely on X-ray measurements that depend linearly on the number of incident X-ray photons. The advent of X-ray free electron lasers (XFELs) is opening the ability to reach extremely high photon numbers within ultrashort X-ray pulse durations and is leading to a paradigm shift in our ability to explore nonlinear X-ray signals. However, the enormous increase in X-ray peak power is a double-edged sword with new and exciting methods being developed but at the same time well-established techniques proving unreliable.more » Consequently, accurate knowledge about the threshold for nonlinear X-ray signals is essential. Here in this paper we report an X-ray spectroscopic study that reveals important details on the thresholds for nonlinear X-ray interactions. By varying both the incident X-ray intensity and photon energy, we establish the regimes at which the simplest nonlinear process, two-photon X-ray absorption (TPA), can be observed. From these measurements we can extract the probability of this process as a function of photon energy and confirm both the nature and sub-femtosecond lifetime of the virtual intermediate electronic state.« less

Electronic structure of the organic semiconductor Alq3 (aluminum tris-8-hydroxyquinoline) from soft x-ray spectroscopies and density functional theory calculations.

PubMed

DeMasi, A; Piper, L F J; Zhang, Y; Reid, I; Wang, S; Smith, K E; Downes, J E; Peltekis, N; McGuinness, C; Matsuura, A

2008-12-14

The element-specific electronic structure of the organic semiconductor aluminum tris-8-hydroxyquinoline (Alq(3)) has been studied using a combination of resonant x-ray emission spectroscopy, x-ray photoelectron spectroscopy, x-ray absorption spectroscopy, and density functional theory (DFT) calculations. Resonant and nonresonant x-ray emission spectroscopy were used to measure directly the carbon, nitrogen and oxygen 2p partial densities of states in Alq(3), and good agreement was found with the results of DFT calculations. Furthermore, resonant x-ray emission at the carbon K-edge is shown to be able to measure the partial density of states associated with individual C sites. Finally, comparison of previous x-ray emission studies and the present data reveal the presence of clear photon-induced damage in the former.

Stimulated Electronic X-Ray Raman Scattering

NASA Astrophysics Data System (ADS)

Weninger, Clemens; Purvis, Michael; Ryan, Duncan; London, Richard A.; Bozek, John D.; Bostedt, Christoph; Graf, Alexander; Brown, Gregory; Rocca, Jorge J.; Rohringer, Nina

2013-12-01

We demonstrate strong stimulated inelastic x-ray scattering by resonantly exciting a dense gas target of neon with femtosecond, high-intensity x-ray pulses from an x-ray free-electron laser (XFEL). A small number of lower energy XFEL seed photons drive an avalanche of stimulated resonant inelastic x-ray scattering processes that amplify the Raman scattering signal by several orders of magnitude until it reaches saturation. Despite the large overall spectral width, the internal spiky structure of the XFEL spectrum determines the energy resolution of the scattering process in a statistical sense. This is demonstrated by observing a stochastic line shift of the inelastically scattered x-ray radiation. In conjunction with statistical methods, XFELs can be used for stimulated resonant inelastic x-ray scattering, with spectral resolution smaller than the natural width of the core-excited, intermediate state.

Katherine E. Weimer Award: X-ray light sources from laser-plasma and laser-electron interaction: development and applications

NASA Astrophysics Data System (ADS)

Albert, Felicie

2017-10-01

Bright sources of x-rays, such as synchrotrons and x-ray free electron lasers (XFEL) are transformational tools for many fields of science. They are used for biology, material science, medicine, or industry. Such sources rely on conventional particle accelerators, where electrons are accelerated to gigaelectronvolts (GeV) energies. The accelerated particles are wiggled in magnetic structures to emit x-ray radiation that is commonly used for molecular crystallography, fluorescence studies, chemical analysis, medical imaging, and many other applications. One of the drawbacks of these machines is their size and cost, because electric field gradients are limited to about 100 V/M in conventional accelerators. Particle acceleration in laser-driven plasmas is an alternative to generate x-rays via betatron emission, Compton scattering, or bremsstrahlung. A plasma can sustain electrical fields many orders of magnitude higher than that in conventional radiofrequency accelerator structures. When short, intense laser pulses are focused into a gas, it produces electron plasma waves in which electrons can be trapped and accelerated to GeV energies. X-ray sources, driven by electrons from laser-wakefield acceleration, have unique properties that are analogous to synchrotron radiation, with a 1000-fold shorter pulse. An important use of x-rays from laser plasma accelerators is in High Energy Density (HED) science, which requires laser and XFEL facilities to create in the laboratory extreme conditions of temperatures and pressures that are usually found in the interiors of stars and planets. To diagnose such extreme states of matter, the development of efficient, versatile and fast (sub-picosecond scale) x-ray probes has become essential. In these experiments, x-ray photons can pass through dense material, and absorption of the x-rays can be directly measured, via spectroscopy or imaging, to inform scientists about the temperature and density of the targets being studied. Performed under the auspices of the U.S. Department of Energy by Lawrence Livermore National Laboratory under contract DE-AC52-07NA27344, supported by the LLNL LDRD program (16ERD024), and by the DOE Office Science Early Career Research Program (SCW1575).

An adjustable short-focal length, high-gradient PMQ electron-beam final-focus system for the PLEIADES ultra-fast x-ray Thomson source

NASA Astrophysics Data System (ADS)

Lim, Jae-Ku

In the span of a 100 year since the discovery of first x-rays by Roentgen that won him the first Nobel prize in physics, several types of radiation sources have been developed. Currently, radiations at extremely short wavelengths have only been accessed at synchrotron radiation sources. However, the current 3rd generation synchrotron sources can only produce x-rays of energy up to 60 keV and pulse lengths of several picoseconds long. But needs for shorter wavelength and shorter pulse duration radiations demanded by scientists to understand the nature of matter at atomic/molecular scale initiated the new scientific research for the production of sub-picosecond, hard x-rays. At the Lawrence Livermore National Laboratory, a Thomson x-ray source in the backscattering mode---a head-on collision between a high intensity Ti:Sapphire Chirped Pulse Amplification laser and a relativistic electron beam---called the PLEIADES (Picosecond Laser-Electron Inter-Action for the Dynamical Evaluation of Structures) laboratory has been developed. Early works demonstrated the production of quasi-monochromatic, femto-second long, hard x-rays. Initially reported x-ray flux was in the low range of 105--10 6 photons per shot. During the early stage of PLEIADES experiments, 15 T/m electromagnet final focusing quadrupoles (in a triplet lattice configuration) were employed to focus the beam to a 40-50 mum spot-size. A larger focal spot-size beam has a low-density of electron particles available at the interaction with incident photons, which leads to a low scattering probability. The current dissertation shows that by employing a 560 T/m PMQ (Permanent-Magnet Quadrupole) final focus system, an electron beam as small as 10-20 mum can be achieved. The implementation of this final focus system demonstrated the improvement of the total x-ray flux by two orders of magnitude. The PMQ final focus system also produced small electron beams consistently over 30-100 MeV electron beam energy, which enabled the production of x-ray energy over 40-140 keV. In this dissertation, the PLEIADES Thomson x-ray facility will be described in detail includes the 100 MeV linac and the FALCON laser system. Later, we will discuss the design, construction and implementation of the PMQ final focus system in the beamline. The measurement of electron beam parameters before and after the final focus system will be presented. The beam measurements at the interaction region were accomplished with the use of both OTR (Optical Transition Radiation) imaged by a CCD camera and the fast streak camera for respective spatial and temporal alignments. The theoretical analysis in "real beam" effects and spacetime beam jitter effects will be given to help understand the observations. A 3D simulation tool developed for x-ray data analysis was used to provide direct comparisons with the x-ray flux, spectrum distribution and transverse x-ray profile.

Real Time Spectroscopic Ellipsometry Analysis of First Stage CuIn1−xGaxSe2 Growth: Indium-Gallium Selenide Co-Evaporation

PubMed Central

Pradhan, Puja; Aryal, Puruswottam; Attygalle, Dinesh; Ibdah, Abdel-Rahman; Koirala, Prakash; Li, Jian; Bhandari, Khagendra P.; Liyanage, Geethika K.; Ellingson, Randy J.; Heben, Michael J.; Marsillac, Sylvain; Collins, Robert W.; Podraza, Nikolas J.

2018-01-01

Real time spectroscopic ellipsometry (RTSE) has been applied for in-situ monitoring of the first stage of copper indium-gallium diselenide (CIGS) thin film deposition by the three-stage co-evaporation process used for fabrication of high efficiency thin film photovoltaic (PV) devices. The first stage entails the growth of indium-gallium selenide (In1−xGax)2Se3 (IGS) on a substrate of Mo-coated soda lime glass maintained at a temperature of 400 °C. This is a critical stage of CIGS deposition because a large fraction of the final film thickness is deposited, and as a result precise compositional control is desired in order to achieve the optimum performance of the resulting CIGS solar cell. RTSE is sensitive to monolayer level film growth processes and can provide accurate measurements of bulk and surface roughness layer thicknesses. These in turn enable accurate measurements of the bulk layer optical response in the form of the complex dielectric function ε = ε1 − iε2, spectra. Here, RTSE has been used to obtain the (ε1, ε2) spectra at the measurement temperature of 400 °C for IGS thin films of different Ga contents (x) deduced from different ranges of accumulated bulk layer thickness during the deposition process. Applying an analytical expression in common for each of the (ε1, ε2) spectra of these IGS films, oscillator parameters have been obtained in the best fits and these parameters in turn have been fitted with polynomials in x. From the resulting database of polynomial coefficients, the (ε1, ε2) spectra can be generated for any composition of IGS from the single parameter, x. The results have served as an RTSE fingerprint for IGS composition and have provided further structural information beyond simply thicknesses, for example information related to film density and grain size. The deduced IGS structural evolution and the (ε1, ε2) spectra have been interpreted as well in relation to observations from scanning electron microscopy, X-ray diffractometry and energy-dispersive X-ray spectroscopy profiling analyses. Overall the structural, optical and compositional analysis possible by RTSE has assisted in understanding the growth and properties of three stage CIGS absorbers for solar cells and shows future promise for enhancing cell performance through monitoring and control. PMID:29337931

Investigating the effect of Cd-Mn co-doped nano-sized BiFeO3 on its physical properties

NASA Astrophysics Data System (ADS)

Ishaq, B.; Murtaza, G.; Sharif, S.; Azhar Khan, M.; Akhtar, Naeem; Will, I. G.; Saleem, Murtaza; Ramay, Shahid M.

This work deals with the investigation of different effects on the structural, magnetic, electronic and dielectric properties of Cd and Mn doped Bi0.75Cd0.25Fe1-xMnxO3 multiferroic samples by taking fixed ratios of Cd and varying the Mn ratio with values of x = 0.0, 0.5, 0.10 and 0.15. Cd-Mn doped samples were synthesized chemically using a microemulsion method. All the samples were finally sintered at 700 °C for 2 h to obtain the single phase perovskites structure of BiFeO3 materials. The synthesized samples were characterized by different techniques, such as X-ray diffractometry (XRD), Scanning Electron Microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), LCR meter and magnetic properties using VSM. XRD results confirm BFO is a perovskite structure having crystallite size in the range of 24-54 nm. XRD results also reveal observed structural distortion due to doping of Cd at the A-site and Mn at the B-site of BFO. SEM results depict that, as the substitution of Cd-Mn increases in BFO, grain size decreases up to 30 nm. FTIR spectra showed prominent absorption bands at 555 cm-1 and 445 cm-1 corresponding to the stretching vibrations of the metal ions complexes at site A and site B, respectively. Variation of dielectric constant (ɛ‧) and loss tangent (tan δ) at room temperature in the range of 1 MHz to 3 GHz have been investigated. Results reveal that with Cd-Mn co doping a slight decrease in dielectric constant have been observed. Magnetic properties of Cd-Mn doped pure BFO samples have been studied at 300 K. Results reveal that undoped BiFeO3 exhibits weak ferromagnetic ordering due to the canting of its spin. Increase in magnetization and decrease in coercivity is a clear indication that a material can be used in high density recording media and memory devices.

High flux, narrow bandwidth compton light sources via extended laser-electron interactions

DOEpatents

Barty, V P

2015-01-13

New configurations of lasers and electron beams efficiently and robustly produce high flux beams of bright, tunable, polarized quasi-monoenergetic x-rays and gamma-rays via laser-Compton scattering. Specifically, the use of long-duration, pulsed lasers and closely-spaced, low-charge and low emittance bunches of electron beams increase the spectral flux of the Compton-scattered x-rays and gamma rays, increase efficiency of the laser-electron interaction and significantly reduce the overall complexity of Compton based light sources.

A photoluminescence, thermoluminescence and electron paramagnetic resonance study of EFG grown europium doped lithium fluoride (LiF) crystals

NASA Astrophysics Data System (ADS)

Seth, Pooja; Swati, G.; Haranath, D.; Rao, S. M. D.; Aggarwal, Shruti

2018-07-01

Europium (Eu) doped LiF crystals have been grown by the Edge-defined film fed growth (EFG) technique. The designing and installation of the furnace used for the growth of the crystals have been discussed in detail. In the present study, Eu (Eu2O3) has been doped in LiF in different concentration (0.02-0.2 wt %). X-ray diffractometry (XRD) and Energy Dispersive X-ray (EDX) spectroscopy confirms the incorporation of Eu in LiF. The influence of Eu on LiF has been investigated through photoluminescence (PL), thermoluminescence (TL) and electron paramagnetic resonance (EPR) in as-grown and annealed crystals. PL emission spectra shows the presence of both Eu3+ and Eu2+ form in the as-grown crystals which is confirmed by EPR results. Whereas, in annealed crystals, Eu is present predominantly as Eu2+ form. This suggests that growing crystals at high temperature (∼900 °C) in argon gas atmosphere through EFG technique favours the reduction of Eu3+ → Eu2+. This reduction phenomenon has been explained on the basis of charge compensation model. TL study of the LiF: Eu (0.02-0.2 wt %) crystals has been done after irradiation with Co60 gamma rays. In this study, it has been observed that the TL intensity as well as glow curve structure of LiF: Eu crystals are a strong function of Eu concentration. The maximum TL is observed at Eu concentration of 0.05 wt% at which a well defined glow curve structure with a prominent peak at 185 °C and a small peak at 253 °C. Beyond this concentration (0.05 wt %), TL intensity decreases due to aggregation of defects in the host. The peak at 185 °C in LiF: Eu (0.05 wt %) is certainly due to the presence of Eu2+ associated defects which is also supported by the PL spectra. It has been observed that Eu doping have a key role in creation of more defect levels which lead to the increased number of electron and hole traps. Further, trapping parameters are analysed using glow curve deconvolution method to have an insight study of TL phenomena. Further, TL glow curve structure of as-grown and annealed crystal are distinct which may be attributed to the nature of defect traps formed inside the LiF.

Calculating the X-Ray Fluorescence from the Planet Mercury Due to High-Energy Electrons

NASA Technical Reports Server (NTRS)

Burbine, T. H.; Trombka, J. I.; Bergstrom, P. M., Jr.; Christon, S. P.

2005-01-01

The least-studied terrestrial planet is Mercury due to its proximity to the Sun, which makes telescopic observations and spacecraft encounters difficult. Our lack of knowledge about Mercury should change in the near future due to the recent launching of MESSENGER, a Mercury orbiter. Another mission (BepiColombo) is currently being planned. The x-ray spectrometer on MESSENGER (and planned for BepiColombo) can characterize the elemental composition of a planetary surface by measuring emitted fluorescent x-rays. If electrons are ejected from an atom s inner shell by interaction with energetic particles such as photons, electrons, or ions, electrons from an outer shell can transfer to the inner shell. Characteristic x-rays are then emitted with energies that are the difference between the binding energy of the ion in its excited state and that of the ion in its ground state. Because each element has a unique set of energy levels, each element emits x-rays at a unique set of energies. Electrons and ions usually do not have the needed flux at high energies to cause significant x-ray fluorescence on most planetary bodies. This is not the case for Mercury where high-energy particles were detected during the Mariner 10 flybys. Mercury has an intrinsic magnetic field that deflects the solar wind, resulting in a bow shock in the solar wind and a magnetospheric cavity. Electrons and ions accelerated in the magnetosphere tend to follow its magnetic field lines and can impact the surface on Mercury s dark side Modeling has been done to determine if x-ray fluorescence resulting from the impact of high-energy electrons accelerated in Mercury's magnetosphere can be detected by MESSENGER. Our goal is to understand how much bulk chemical information can be obtained from x-ray fluorescence measurements on the dark side of Mercury.

Advanced X-Ray Sources Ensure Safe Environments

NASA Technical Reports Server (NTRS)

2008-01-01

Ames Research Center awarded inXitu Inc. (formerly Microwave Power Technology), of Mountain View, California, an SBIR contract to develop a new design of electron optics for forming and focusing electron beams that is applicable to a broad class of vacuum electron devices. This technology offers an inherently rugged and more efficient X-ray source for material analysis; a compact and rugged X-ray source for smaller rovers on future Mars missions; and electron beam sources to reduce undesirable emissions from small, widely distributed pollution sources; and remediation of polluted sites.

Talbot-Lau x-ray deflectometry phase-retrieval methods for electron density diagnostics in high-energy density experiments.

PubMed

Valdivia, Maria Pia; Stutman, Dan; Stoeckl, Christian; Mileham, Chad; Begishev, Ildar A; Bromage, Jake; Regan, Sean P

2018-01-10

Talbot-Lau x-ray interferometry uses incoherent x-ray sources to measure refraction index changes in matter. These measurements can provide accurate electron density mapping through phase retrieval. An adaptation of the interferometer has been developed in order to meet the specific requirements of high-energy density experiments. This adaptation is known as a moiré deflectometer, which allows for single-shot capabilities in the form of interferometric fringe patterns. The moiré x-ray deflectometry technique requires a set of object and reference images in order to provide electron density maps, which can be costly in the high-energy density environment. In particular, synthetic reference phase images obtained ex situ through a phase-scan procedure, can provide a feasible solution. To test this procedure, an object phase map was retrieved from a single-shot moiré image obtained from a plasma-produced x-ray source. A reference phase map was then obtained from phase-stepping measurements using a continuous x-ray tube source in a small laboratory setting. The two phase maps were used to retrieve an electron density map. A comparison of the moiré and phase-stepping phase-retrieval methods was performed to evaluate single-exposure plasma electron density mapping for high-energy density and other transient plasma experiments. It was found that a combination of phase-retrieval methods can deliver accurate refraction angle mapping. Once x-ray backlighter quality is optimized, the ex situ method is expected to deliver electron density mapping with improved resolution. The steps necessary for improved diagnostic performance are discussed.

Calculation of x-ray spectra emerging from an x-ray tube. Part I. electron penetration characteristics in x-ray targets.

PubMed

Poludniowski, Gavin G; Evans, Philip M

2007-06-01

The penetration characteristics of electron beams into x-ray targets are investigated for incident electron kinetic energies in the range 50-150 keV. The frequency densities of electrons penetrating to a depth x in a target, with a fraction of initial kinetic energy, u, are calculated using Monte Carlo methods for beam energies of 50, 80, 100, 120 and 150 keV in a tungsten target. The frequency densities for 100 keV electrons in Al, Mo and Re targets are also calculated. A mixture of simple modeling with equations and interpolation from data is used to generalize the calculations in tungsten. Where possible, parameters derived from the Monte Carlo data are compared to experimental measurements. Previous electron transport approximations in the semiempirical models of other authors are discussed and related to this work. In particular, the crudity of the use of the Thomson-Whiddington law to describe electron penetration and energy loss is highlighted. The results presented here may be used towards calculating the target self-attenuation correction for bremsstrahlung photons emitted within a tungsten target.

Backscatter of hard X-rays in the solar atmosphere. [Calculating the reflectance of solar x ray emission

NASA Technical Reports Server (NTRS)

Bai, T.; Ramaty, R.

1977-01-01

The solar photosphere backscatters a substantial fraction of the hard X rays from solar flares incident upon it. This reflection was studied using a Monte Carlo simulation which takes into account Compton scattering and photo-electric absorption. Both isotropic and anisotropic X ray sources are considered. The bremsstrahlung from an anisotropic distribution of electrons are evaluated. By taking the reflection into account, the inconsistency is removed between recent observational data regarding the center-to-limb variation of solar X ray emission and the predictions of models in which accelerated electrons are moving down toward the photosphere.

Fluorescence imaging of reactive oxygen species by confocal laser scanning microscopy for track analysis of synchrotron X-ray photoelectric nanoradiator dose: X-ray pump-optical probe.

PubMed

Jeon, Jae Kun; Han, Sung Mi; Kim, Jong Ki

2016-09-01

Bursts of emissions of low-energy electrons, including interatomic Coulomb decay electrons and Auger electrons (0-1000 eV), as well as X-ray fluorescence produced by irradiation of large-Z element nanoparticles by either X-ray photons or high-energy ion beams, is referred to as the nanoradiator effect. In therapeutic applications, this effect can damage pathological tissues that selectively take up the nanoparticles. Herein, a new nanoradiator dosimetry method is presented that uses probes for reactive oxygen species (ROS) incorporated into three-dimensional gels, on which macrophages containing iron oxide nanoparticles (IONs) are attached. This method, together with site-specific irradiation of the intracellular nanoparticles from a microbeam of polychromatic synchrotron X-rays (5-14 keV), measures the range and distribution of OH radicals produced by X-ray emission or superoxide anions ({\\rm{O}}_2^-) produced by low-energy electrons. The measurements are based on confocal laser scanning of the fluorescence of the hydroxyl radical probe 2-[6-(4'-amino)phenoxy-3H-xanthen-3-on-9-yl] benzoic acid (APF) or the superoxide probe hydroethidine-dihydroethidium (DHE) that was oxidized by each ROS, enabling tracking of the radiation dose emitted by the nanoradiator. In the range 70 µm below the irradiated cell, ^\\bullet{\\rm{OH}} radicals derived mostly from either incident X-ray or X-ray fluorescence of ION nanoradiators are distributed along the line of depth direction in ROS gel. In contrast, {\\rm{O}}_2^- derived from secondary electron or low-energy electron emission by ION nanoradiators are scattered over the ROS gel. ROS fluorescence due to the ION nanoradiators was observed continuously to a depth of 1.5 mm for both oxidized APF and oxidized DHE with relatively large intensity compared with the fluorescence caused by the ROS produced solely by incident primary X-rays, which was limited to a depth of 600 µm, suggesting dose enhancement as well as more penetration by nanoradiators. In conclusion, the combined use of a synchrotron X-ray microbeam-irradiated three-dimensional ROS gel and confocal laser scanning fluorescence microscopy provides a simple dosimetry method for track analysis of X-ray photoelectric nanoradiator radiation, suggesting extensive cellular damage with dose-enhancement beyond a single cell containing IONs.

X-ray absorption spectroscopy using a self-seeded soft X-ray free-electron laser

DOE PAGES

Kroll, Thomas; Kern, Jan; Kubin, Markus; ...

2016-09-19

X-ray free electron lasers (XFELs) enable unprecedented new ways to study the electronic structure and dynamics of transition metal systems. L-edge absorption spectroscopy is a powerful technique for such studies and the feasibility of this method at XFELs for solutions and solids has been demonstrated. But, the required x-ray bandwidth is an order of magnitude narrower than that of self-amplified spontaneous emission (SASE), and additional monochromatization is needed. We compare L-edge x-ray absorption spectroscopy (XAS) of a prototypical transition metal system based on monochromatizing the SASE radiation of the linac coherent light source (LCLS) with a new technique based onmore » self-seeding of LCLS. We demonstrate how L-edge XAS can be performed using the self-seeding scheme without the need of an additional beam line monochromator. Lastly, we show how the spectral shape and pulse energy depend on the undulator setup and how this affects the x-ray spectroscopy measurements.« less

X-ray absorption spectroscopy using a self-seeded soft X-ray free-electron laser

PubMed Central

Kroll, Thomas; Kern, Jan; Kubin, Markus; Ratner, Daniel; Gul, Sheraz; Fuller, Franklin D.; Löchel, Heike; Krzywinski, Jacek; Lutman, Alberto; Ding, Yuantao; Dakovski, Georgi L.; Moeller, Stefan; Turner, Joshua J.; Alonso-Mori, Roberto; Nordlund, Dennis L.; Rehanek, Jens; Weniger, Christian; Firsov, Alexander; Brzhezinskaya, Maria; Chatterjee, Ruchira; Lassalle-Kaiser, Benedikt; Sierra, Raymond G.; Laksmono, Hartawan; Hill, Ethan; Borovik, Andrew; Erko, Alexei; Föhlisch, Alexander; Mitzner, Rolf; Yachandra, Vittal K.; Yano, Junko; Wernet, Philippe; Bergmann, Uwe

2016-01-01

X-ray free electron lasers (XFELs) enable unprecedented new ways to study the electronic structure and dynamics of transition metal systems. L-edge absorption spectroscopy is a powerful technique for such studies and the feasibility of this method at XFELs for solutions and solids has been demonstrated. However, the required x-ray bandwidth is an order of magnitude narrower than that of self-amplified spontaneous emission (SASE), and additional monochromatization is needed. Here we compare L-edge x-ray absorption spectroscopy (XAS) of a prototypical transition metal system based on monochromatizing the SASE radiation of the linac coherent light source (LCLS) with a new technique based on self-seeding of LCLS. We demonstrate how L-edge XAS can be performed using the self-seeding scheme without the need of an additional beam line monochromator. We show how the spectral shape and pulse energy depend on the undulator setup and how this affects the x-ray spectroscopy measurements. PMID:27828320

Study the effect of mechanical alloying parameters on synthesis of Cr{sub 2}Nb–Al{sub 2}O{sub 3} nanocomposite

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

Shayesteh, Payam, E-mail: shayesteh.payam@gmail.com; Mirdamadi, Shamseddin; Razavi, Hossein

2014-01-01

Graphical abstract: - Highlights: • Cr{sub 2}Nb–Al{sub 2}O{sub 3} nanocomposite synthesized through MA. • Effect of BPR, rotating speed, milling time and PCA concentration investigated. • After annealing at 1100 °C crystalline phase were appeared. • Williamson–Hall analysis was used in order to study the grain size of nano composite. - Abstract: In this study, Cr{sub 2}Nb–20 vol.% Al{sub 2}O{sub 3} nanocomposite was prepared successfully by mechanochemical reaction between Al, Nb and Cr{sub 2}O{sub 3} powders. Amorphization of powder occurred during mechanical alloying because of high energy collisions between powders and steel balls in milling container which transfer high degreemore » of energy to powders. Therefore, annealing was needed to form crystalline phases. The influence of different mechanical alloying parameters such as BPR, rotating speed, milling time and PCA concentration on synthesis of composite material were investigated. After mechanical alloying, the powder was encapsulated in quartz and then annealed at 1100 °C for 3 h. After annealing, 3 different phases were appeared (Cr{sub 2}Nb (cubic), Cr{sub 2}Nb (hexagonal) and α-Al{sub 2}O{sub 3}). The structural changes of powder particles during mechanical alloying were studied by X-ray diffractometry (XRD), atomic force microscopy (AFM), scanning electron microscopy (SEM) and transmission electron microscopy (TEM)« less

He-irradiation effects on glass-ceramics for joining of SiC-based materials

NASA Astrophysics Data System (ADS)

Gozzelino, L.; Casalegno, V.; Ghigo, G.; Moskalewicz, T.; Czyrska-Filemonowicz, A.; Ferraris, M.

2016-04-01

CaO-Al2O3 (CA) and SiO2-Al2O3-Y2O3 (SAY) glass-ceramics are promising candidates for SiC/SiC indirect joints. In view of their use in locations where high radiation level is expected (i.e. fusion plants) it is important to investigate how radiation-induced damage can modify the material microstructure. To this aim, pellets of both types were irradiated with 5.5 MeV 4He+ ions at an average temperature of 75 °C up to a fluence of almost 2.3·1018 cm-2. This produces a displacement defect density that increases with depth and reaches a value of about 40 displacements per atom in the ion implantation region, where the He-gas reaches a concentration of several thousands of atomic parts per million. X-ray diffractometry and scanning electron microscopy showed no change in the microstructure and in the morphology of the pellet surface. Moreover, a transmission electron microscopy investigation on cross-section lamellas revealed the occurrence of structural defects and agglomerates of He-bubbles in the implantation region for the CA sample and a more homogeneous He-bubble distribution in the SAY pellet, even outside the implantation layer. In addition, no amorphization was found in both samples, even in correspondence to the He implantation zone. The radiation damage induced only occasional micro-cracks, mainly located at grain boundaries (CA) or within the grains (SAY).

Anomalous magnetoelastic behaviour near morphotropic phase boundary in ferromagnetic Tb 1-xNd xCo 2 system

DOE PAGES

Murtaza, Adil; Yang, Sen; Zhou, Chao; ...

2016-08-04

In this study, we report a morphotropic phase boundary (MPB) involved ferromagnetic system Tb 1-xNd xCo 2 and reveal the corresponding structural and magnetoelastic properties of this system. With high resolution synchrotron X-ray diffractometry, the crystal structure of the TbCo 2-rich side is detected to be rhombohedral and that of NdCo 2-rich side is tetragonal below their respective Curie temperatures TC. The MPB composition Tb 0.35Nd 0.65Co 2 corresponds to the coexistence of the rhombohedral phase (R-phase) and tetragonal phase ( T-phase). Contrary to previously reported MPB involved ferromagnetic systems, the MPB composition of Tb 0.35Nd 0.65Co 2 shows minimummore » magnetization which can be understood as compensation of sublattice moments between the R-phase and the T-phase. Furthermore, magnetostriction of Tb 1-xNd xCo 2 decreases with increasing Nd concentration until x = 0.8 and then increases in the negative direction with further increasing Nd concentration; the optimum point for magnetoelastic properties lies towards the rhombohedral phase. Finally, our work not only shows an anomalous type of ferromagnetic MPB but also provides an effective way to design functional materials.« less

Electron acceleration in pulsed-power driven magnetic-reconnection experiments

NASA Astrophysics Data System (ADS)

Halliday, Jonathan; Hare, Jack; Lebedev, Sergey; Suttle, Lee; Bland, Simon; Clayson, Thomas; Tubman, Eleanor; Pikuz, Sergei; Shelkovenko, Tanya

2017-10-01

We present recent results from pulsed-power driven magnetic reconnection experiments, fielded on the MAGPIE generator (1.2 MA, 250 ns). The setup used in these experiments produces plasma inflows which are intrinsically magnetised; persist for many hydrodynamic time-scales; and are supersonic. Previous work has focussed on characterising the dynamics of bulk plasma flows, using a suite of diagnostics including laser interferometry, (imaging) Faraday rotation, and Thompson scattering. Measurements show the formation of a well defined, long lasting reconnection layer and demonstrate a power balance between the power into and out of the reconnection region. The work presented here focuses on diagnosing non-thermal electron acceleration by the reconnecting electric field. To achieve this, metal foils were placed in the path of accelerated electrons. Atomic transitions in the foil were collisionally exited by the electron beam, producing a characteristic X-Ray spectrum. This X-Ray emission was diagnosed using spherically bent crystal X-Ray spectrometry, filtered X-Ray pinhole imaging, and X-Ray sensitive PIN diodes.

50 MeV, Li{sup 3+} - ion irradiation effect on magnetic ordering of Y{sup 3+} - substituted yttrium iron garnet

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

Sharma, P. U.; Zankat, K. B.; Dolia, S. N.

2016-05-06

This communication presents the effect of non-magnetic Y{sup 3+} ions substitution for magnetic Fe{sup 3+} ions and 50 MeV, Li{sup 3+} ion irradiation (fluence: 5 × 10{sup 13} ions/cm{sup 2}) on magnetic ordering and Neel temperature of Y{sub 3+x}Fe{sub 5-x}O{sub 12} (x = 0.0, 0.2, 0.4 and 0.6) garnet system, studied by means of X-ray powder diffractometry and thermal variation of low field (0.5 Oe) ac susceptibility measurements. The un-irradiated compositions exhibit normal ferrimagnetic behavior with decrease in transition temperature (T{sub N}) on increasing Y{sup 3+}-concentration (x). The irradiated counterparts are characterized by tailing effect indicative of non-uniform effect of irradiationmore » and lower value of T{sub N}. The results have been discussed based on the weakening of magnetic exchange interactions and cumulative effect of redistribution of cations and fractional creation of localized paramagnetic centers resulting from swift heavy ion irradiation. The Neel temperatures and exchange integrals have been calculated theoretically.« less

Prediction and Measurement of X-Ray Spectral and Intensity Distributions from Low Energy Electron Impact Sources

NASA Technical Reports Server (NTRS)

Edwards, David L.

1999-01-01

In-vacuum electron beam welding is a technology that NASA considered as a joining technique for manufacture of space structures. The interaction of energetic electrons with metal produces x-rays. The radiation exposure to astronauts performing the in-vacuum electron beam welding must be characterized and minimized to insure safe operating conditions. This investigation characterized the x-ray environment due to operation of an in-vacuum electron beam welding tool. NASA, in a joint venture with the Russian Space Agency, was scheduled to perform a series of welding in space experiments on board the United States Space Shuttle. This series of experiments was named the International Space Welding Experiment (ISWE). The hardware associated with the ISWE was leased to NASA, by the Paton Welding Institute (PWI) in Ukraine, for ground based welding experiments in preparation for flight. Two tests were scheduled, using the ISWE electron beam welding tool, to characterize the radiation exposure to an astronaut during the operation of the ISWE. These radiation exposure tests consisted of Thermoluminescence Dosimeters (TLD's) shielded with material currently used by astronauts during Extra Vehicular Activities (EVA) and exposed to x-ray radiation generated by operation of an in-vacuum electron beam welding tool. This investigation was the first known application of TLD's to measure absorbed dose from x-rays of energy less than 10 KeV. The ISWE hardware was returned to Ukraine before the issue of adequate shielding for the astronauts was verified. Therefore, alternate experimental and analytical methods were developed to measure and predict the x-ray spectral and intensity distribution generated by electron impact with metal. These x-ray spectra were used to calculate the absorbed radiation dose to astronauts. These absorbed dose values were compared to TLD measurements obtained during actual operation of the in-vacuum electron beam welding tool. The calculated absorbed dose values were found to be in good agreement with the TLD values.

High-Performance X-ray Detection in a New Analytical Electron Microscope

NASA Technical Reports Server (NTRS)

Lyman, C. E.; Goldstein, J. I.; Williams, D. B.; Ackland, D. W.; vonHarrach, S.; Nicholls, A. W.; Statham, P. J.

1994-01-01

X-ray detection by energy-dispersive spectrometry in the analytical electron microscope (AEM) is often limited by low collected X-ray intensity (P), modest peak-to-background (P/B) ratios, and limitations on total counting time (tau) due to specimen drift and contamination. A new AFM has been designed with maximization of P. P/B, and tau as the primary considerations. Maximization of P has been accomplished by employing a field-emission electron gun, X-ray detectors with high collection angles, high-speed beam blanking to allow only one photon into the detector at a time, and simultaneous collection from two detectors. P/B has been maximized by reducing extraneous background signals generated at the specimen holder, the polepieces and the detector collimator. The maximum practical tau has been increased by reducing specimen contamination and employing electronic drift correction. Performance improvments have been measured using the NIST standard Cr thin film. The 0-3 steradian solid angle of X-ray collection is the highest value available. The beam blanking scheme for X-ray detection provides 3-4 times greater throughput of X-rays at high count rates into a recorded spectrum than normal systems employing pulse-pileup rejection circuits. Simultaneous X-ray collection from two detectors allows the highest X-ray intensity yet recorded to be collected from the NIST Cr thin film. The measured P/B of 6300 is the highest level recorded for an AEM. In addition to collected X-ray intensity (cps/nA) and P/B measured on the standard Cr film, the product of these can be used as a figure-of-merit to evaluate instruments. Estimated minimum mass fraction (MMF) for Cr measured on the standard NIST Cr thin film is also proposed as a figure-of-merit for comparing X-ray detection in AEMs. Determinations here of the MMF of Cr detectable show at least a threefold improvement over previous instruments.

A Many-Body Formalism of ΔSCF Approach for Simulating X-Ray Spectra from First-Principles

NASA Astrophysics Data System (ADS)

Liang, Yufeng; Vinson, John; Pemmaraju, Sri; Drisdell, Walter; Shirley, Eric; Prendegast, David

Accurately reproducing X-ray spectral fingerprints for materials characterization relies heavily on how to correctly model the many-electron response to the generation of an X-ray core hole. In this talk, we present a novel first-principles theory for simulating X-ray spectra that is based on many-electron wavefunctions. The proposed theory go beyond the electron-hole correlations within the Bethe-Saltpeter Equation and consider higher-order vertex corrections up to the level of Mahan-Noziéres-De Dominicis (MND) theory. An efficient algorithm is invented to incorporate these many-electron processes by using linear algebra rather than iterating over all Feynman diag United States Department of Energy under Contact No. DE-AC02-05CH11231, No. DE-SC0004993.

Observation of Betatron X-Ray Radiation in a Self-Modulated Laser Wakefield Accelerator Driven with Picosecond Laser Pulses

DOE PAGES

Albert, F.; Lemos, N.; Shaw, J. L.; ...

2017-03-31

We investigate a new regime for betatron x-ray emission that utilizes kilojoule-class picosecond lasers to drive wakes in plasmas. When such laser pulses with intensities of ~ 5 × 1 0 18 W / cm 2 are focused into plasmas with electron densities of ~ 1 × 1 0 19 cm - 3 , they undergo self-modulation and channeling, which accelerates electrons up to 200 MeV energies and causes those electrons to emit x rays. The measured x-ray spectra are fit with a synchrotron spectrum with a critical energy of 10–20 keV, and 2D particle-in-cell simulations were used to modelmore » the acceleration and radiation of the electrons in our experimental conditions« less

Overview of options for generating high-brightness attosecond x-ray pulses at free-electron lasers and applications at the European XFEL

NASA Astrophysics Data System (ADS)

Serkez, S.; Geloni, G.; Tomin, S.; Feng, G.; Gryzlova, E. V.; Grum-Grzhimailo, A. N.; Meyer, M.

2018-02-01

The generation of attosecond, highbrightness x-ray pulses is a matter of great interest given their applications in the study of ultra-fast processes. In recent years, the production of x-ray pulses of high brightness, both in the soft and in the hard x-ray range, has been enabled by x-ray free-electron lasers (XFELs). In contrast to conventional quantum lasers, XFELs are based on the use of an ultra-relativistic electron beam as gain medium. They often work in the self-amplified spontaneous emission (SASE) regime, which provides pulses of duration down to a few femtoseconds, composed of several longitudinal modes. In order to further decrease the duration of these pulses, special methods need to be implemented. In this paper we review available methods, with particular focus on the x-ray laser-enhanced attosecond pulse generation, which is one of the most promising techniques. We illustrate the method using the SASE3 soft x-ray undulator of the European XFEL facility as a case study, emphasizing the importance of high-repetition rate attosecond x-ray pulses. The expected attosecond-level radiation output is used for simulations of sequential ionization processes in atoms in the case of ionization in the soft x-ray regime, demonstrating the importance of this opportunity for the user community.

Soft x-ray spectroscopy studies of novel electronic materials using synchrotron radiation

NASA Astrophysics Data System (ADS)

Newby, David, Jr.

Soft x-ray spectroscopy can provide a wealth of information on the electronic structure of solids. In this work, a suite of soft x-ray spectroscopies is applied to organic and inorganic materials with potential applications in electronic and energy generation devices. Using the techniques of x-ray absorption (XAS), x-ray emission spectroscopy (XES), and x-ray photoemission spectroscopy (XPS), the fundamental properties of these different materials are explored. Cycloparaphenylenes (CPPs) are a recently synthesized family of cyclic hydrocarbons with very interesting properties and many potential applications. Unusual UV/Visible fluorescence trends have spurred a number of theoretical investigations into the electronic properties of the CPP family, but thus far no comprehensive electronic structure measurements have been conducted. XPS, XAS, and XES data for two varieties, [8]- and [10]-CPP, are presented here, and compared with the results of relevant DFT calculations. Turning towards more application-centered investigations, similar measurements are applied to two materials commonly used in solid oxide fuel cell (SOFC) cathodes: La1-xSrxMnO 3 (LSMO) and La1-xSr1- xCo1-yFe yO3 (LSCF). Both materials are structurally perovskites, but they exhibit strikingly different electronic properties. SOFC systems very efficiently produce electricity by catalyzing reactions between oxygen and petroleum-based hydrocarbons at high temperatures (> 800 C). Such systems are already utilized to great effect in many industries, but more widespread adoption could be had if the cells could operate at lower temperatures. Understanding the electronic structure and operational evolution of the cathode materials is essential for the development of better low-temperature fuel cells. LSCF is a mixed ion-electron conductor which holds promise for low-temperature SOFC applications. XPS spectra of LSCF thin films are collected as the films are heated and gas-dosed in a controlled environment. The surface evolution of these films is discussed, and the effects of different gas environments on oxygen vacancy concentration are elucidated. LSMO is commonly used in commercial fuel cell devices. Here the resonant soft x-ray emission (RIXS) spectrum of LSMO is examined, and it is shown that the inelastic x-ray emission structure of LSMO arises from local atomic multiplet effects.

Nanoplasma Formation by High Intensity Hard X-rays

PubMed Central

Tachibana, T.; Jurek, Z.; Fukuzawa, H.; Motomura, K.; Nagaya, K.; Wada, S.; Johnsson, P.; Siano, M.; Mondal, S.; Ito, Y.; Kimura, M.; Sakai, T.; Matsunami, K.; Hayashita, H.; Kajikawa, J.; Liu, X.-J.; Robert, E.; Miron, C.; Feifel, R.; Marangos, J. P.; Tono, K.; Inubushi, Y.; Yabashi, M.; Son, S.-K.; Ziaja, B.; Yao, M.; Santra, R.; Ueda, K.

2015-01-01

Using electron spectroscopy, we have investigated nanoplasma formation from noble gas clusters exposed to high-intensity hard-x-ray pulses at ~5 keV. Our experiment was carried out at the SPring-8 Angstrom Compact free electron LAser (SACLA) facility in Japan. Dedicated theoretical simulations were performed with the molecular dynamics tool XMDYN. We found that in this unprecedented wavelength regime nanoplasma formation is a highly indirect process. In the argon clusters investigated, nanoplasma is mainly formed through secondary electron cascading initiated by slow Auger electrons. Energy is distributed within the sample entirely through Auger processes and secondary electron cascading following photoabsorption, as in the hard x-ray regime there is no direct energy transfer from the field to the plasma. This plasma formation mechanism is specific to the hard-x-ray regime and may, thus, also be important for XFEL-based molecular imaging studies. In xenon clusters, photo- and Auger electrons contribute more significantly to the nanoplasma formation. Good agreement between experiment and simulations validates our modelling approach. This has wide-ranging implications for our ability to quantitatively predict the behavior of complex molecular systems irradiated by high-intensity hard x-rays. PMID:26077863

Lightning leader models of terrestrial gamma-ray flashes

NASA Astrophysics Data System (ADS)

Dwyer, J. R.; Liu, N.; Ihaddadene, K. M. A.

2017-12-01

Terrestrial gamma-ray flashes (TGFs) are bright sub-millisecond bursts of gamma rays that originate from thunderstorms. Because lightning leaders near the ground have been observed to emit x-rays, presumably due to runaway electron production in the high-field regions near the leader tips, models of TGFs have been developed by several groups that assume a similar production mechanism of runaway electrons from lightning leaders propagating through thunderclouds. However, it remains unclear exactly how and where these runaway electrons are produced, since lightning propagation at thunderstorm altitudes remains poorly understood. In addition, it is not obvious how to connect the observed behavior of the x-ray production from lightning near the ground with the properties of TGFs. For example, it is not clear how to relate the time structure of the x-ray emission near the ground to that of TGFs, since x-rays from stepped leaders near the ground are usually produced in a series of sub-microsecond bursts, but TGFs are usually observed as much longer pulses without clear substructures, at sub-microsecond timescales or otherwise. In this presentation, spacecraft observations of TGFs, ground-based observations of x-rays from lightning and laboratory sparks, and Monte Carlo and PIC simulations of runaway electron and gamma ray production and propagation will be used to constrain the lightning leader models of TGFs.

Electronic Structure of the Organic Semiconductor Alq3 (aluminum tris-8-hydroxyquinoline) from Soft X-ray Spectroscopies and Density Functional Theory Calculations

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

DeMasi, A.; Piper, L; Zhang, Y

2008-01-01

The element-specific electronic structure of the organic semiconductor aluminum tris-8-hydroxyquinoline (Alq3) has been studied using a combination of resonant x-ray emission spectroscopy, x-ray photoelectron spectroscopy, x-ray absorption spectroscopy, and density functional theory (DFT) calculations. Resonant and nonresonant x-ray emission spectroscopy were used to measure directly the carbon, nitrogen and oxygen 2p partial densities of states in Alq3, and good agreement was found with the results of DFT calculations. Furthermore, resonant x-ray emission at the carbon K-edge is shown to be able to measure the partial density of states associated with individual C sites. Finally, comparison of previous x-ray emission studiesmore » and the present data reveal the presence of clear photon-induced damage in the former.« less

First refraction contrast imaging via Laser-Compton Scattering X-ray at KEK

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

Sakaue, Kazuyuki; Aoki, Tatsuro; Washio, Masakazu

2012-07-31

Laser-Compton Scattering (LCS) is one of the most feasible techniques for high quality, high brightness, and compact X-ray source. High energy electron beam produced by accelerators scatters off the laser photon at a small spot. As a laser target, we have been developing a pulsedlaser storage cavity for increasing an X-ray flux. The X-ray flux was still inadequate that was 2.1 Multiplication-Sign 10{sup 5}/sec, however, we performed first refraction contrast imaging in order to evaluate the quality of LCS X-ray. Edge enhanced contrast imaging was achieved by changing the distance from sample to detector. The edge enhancement indicates that themore » LCS X-ray has small source size, i.e. high brightness. We believe that the result has demonstrated good feasibility of linac-based high brightness X-ray sources via laser-electron Compton scatterings.« less

Erratum: Creation of X-Ray Transparency of Matter by Stimulated Elastic Forward Scattering [Phys. Rev. Lett. 115 , 107402 (2015)

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

Stöhr, J.; Scherz, A.

X-ray absorption by matter has long been described by the famous Beer-Lambert law. Here we show how this fundamental law needs to be modified for high-intensity coherent x-ray pulses, now available at x-ray free electron lasers, due to the onset of stimulated elastic forward scattering. We present an analytical expression for the modified polarization-dependent Beer-Lambert law for the case of resonant core-to-valence electronic transitions and incident transform limited x-ray pulses. Upon transmission through a solid, the absorption and dichroic contrasts are found to vanish with increasing x-ray intensity, with the stimulation threshold lowered by orders of magnitude through a super-radiativemore » coherent effect. Our results have broad implications for the study of matter with x-ray lasers.« less

The study of in-situ formed alumina and aluminide intermetallic reinforced aluminum-based metal matrix composites

NASA Astrophysics Data System (ADS)

Yu, Peng

Aluminum-based metal matrix composites (MMCs) have been widely used as structural materials in the automobile and aerospace industry due to their specific properties. In this thesis, we report the fabrication of in-situ formed alumina and aluminide intermetallic reinforced aluminum-based metal matrix composites by the displacement reactions between Al and selected metal oxides (NiO, CuO and ZnO). These MMCs were produced when the Al-20wt% NiO, Al-20wt% CuO and Al-10wt% ZnO green compacts were reaction sintered in the tube furnaces. In this work, differential thermal analysis (DTA) was performed on the green samples. The green samples were then sintered separately in different tube furnaces for 30 minutes. In order to study the reaction mechanisms, the x-ray diffractometry (XRD) was used to obtain diffraction patterns of these sintered samples, the scanning electron microscope (SEM) and transmission electron microscope (TEM) were used to study the microstructures of these samples. The elemental quantitative compositions of samples were determined by the energy dispersive x-ray spectrometry (EDX). In order to study the effect of cooling rate on the samples, the green samples were further sintered to 1000°C and cooled down to room temperature in different conditions: by furnace-cooling, air-quenching, oil-quenching or NaCl-solution-quenching. The SEM, TEM and atomic force microscopy (AFM) were conducted to investigate their microstructures. A microhardness tester was used to measure the hardness values of these samples. It was found that during sintering of the Al-20wt% NiO green sample, displacement reaction between Al and NiO initially occurred in solid-solid form and was soon halted by its products that separated the NiO particles from the Al matrix. The reaction then resumed in solid-liquid form as the temperature increased to the eutectic temperature of Al3Ni-Al when liquid (Al, Ni) phase appeared in the sample. After cooling, Al2O 3 particles, Al3Ni proeutectic phase and fiber-like Al 3Ni-Al eutectic were found in the sintered Al-MMC sample. (Abstract shortened by UMI.)

Wear mechanisms in hybrid composites of Graphite-20 Pct SiC in A356 Aluminum Alloy (Al-7 Pct Si-0.3 Pct Mg)

NASA Astrophysics Data System (ADS)

Ames, W.; Alpas, A. T.

1995-01-01

The wear behavior of A356 aluminum alloy (Al-7 Pct Si-0.3 Pct Mg) matrix composites reinforced with 20 vol Pct SiC particles and 3 or 10 vol Pct graphite was investigated. These hybrid composites represent the merging of two philosophies in tribological material design: soft-particle lubrication by graphite and hard-particle reinforcement by carbide particles. The wear tests were performed using a block-on-ring (SAE 52100 steel) wear machine under dry sliding conditions within a load range of 1 to 441 N. The microstructural and compositional changes that took place during wear were characterized using scanning electron microscopy (SEM), Auger electron spectroscopy (AES), energy-dispersive X-ray spectroscopy (EDXA), and X-ray diffractometry (XRD). The wear resistance of 3 Pct graphite-20 Pct SiC-A356 hybrid composite was comparable to 20 Pct SiC-A356 without graphite at low and medium loads. At loads below 20 N, both hybrid and 20 Pct SiC-A356 composites without graphite demonstrated wear rates up to 10 times lower than the unreinforced A356 alloy due to the load-carrying capacity of SiC particles. The wear resistance of 3 Pct graphite 20 Pct SiC-A356 was 1 to 2 times higher than 10 Pct graphite-containing hybrid composites at high loads. However, graphite addition reduced the counterface wear. The unreinforced A356 and 20 Pct SiC-A356 showed a transition from mild to severe wear at 95 N and 225 N, respectively. Hybrid composites with 3 Pct and 10 Pct graphite did not show such a transition over the entire load range, indicating that graphite improved the seizure resistance of the composites. Tribolayers, mainly consisting of a compacted mixture of graphite, iron oxides, and aluminum, were generated on the surfaces of the hybrid composites. In the hybrid composites, the elimination of the severe wear (and hence the improvement in seizure resistance) was attributed to the reduction in friction-induced surface heating due to the presence of graphite- and iron-oxide-containing tribolayers.

Electron cyclotron resonance ion source plasma characterization by X-ray spectroscopy and X-ray imaging

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

Mascali, David, E-mail: davidmascali@lns.infn.it; Castro, Giuseppe; Celona, Luigi

2016-02-15

An experimental campaign aiming to investigate electron cyclotron resonance (ECR) plasma X-ray emission has been recently carried out at the ECRISs—Electron Cyclotron Resonance Ion Sources laboratory of Atomki based on a collaboration between the Debrecen and Catania ECR teams. In a first series, the X-ray spectroscopy was performed through silicon drift detectors and high purity germanium detectors, characterizing the volumetric plasma emission. The on-purpose developed collimation system was suitable for direct plasma density evaluation, performed “on-line” during beam extraction and charge state distribution characterization. A campaign for correlating the plasma density and temperature with the output charge states and themore » beam intensity for different pumping wave frequencies, different magnetic field profiles, and single-gas/gas-mixing configurations was carried out. The results reveal a surprisingly very good agreement between warm-electron density fluctuations, output beam currents, and the calculated electromagnetic modal density of the plasma chamber. A charge-coupled device camera coupled to a small pin-hole allowing X-ray imaging was installed and numerous X-ray photos were taken in order to study the peculiarities of the ECRIS plasma structure.« less