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Sample records for microstructural characterization iii

  1. Structural and microstructural characterization of III-nitrides on 6H-silicon carbide (0001) substrates

    Science.gov (United States)

    Preble, Edward Alfred

    Characterization of nitride films on 6H-SiC (0001) wafers via x-ray, TEM, and AFM was accomplished on standard GAN thin films with AlN or AlGaN buffer layers. TEM sample thinning capability was improved through the use of Nomarski in an optical microscope to gauge the thickness of the sample during preparation. TEM analysis was then completed of Au and Pt films deposited on chemical vapor cleaned GaN with annealed up to 800°C. Chemical reactions were detected in x-ray measurements of the 800°C Pt samples and GaN/metal interface roughening were confirmed by TEM images in both metals. Interface roughening is attributed to the chemical reactions and interfacial stresses greater than the yield stress of the metal created during heat treatments by the difference in the thermal expansion coefficients of the Ga and the metals. The GaN rocking curves were found to track very closely to the values of the underlying substrate and changes in buffer layer growth temperatures were found to change the screw and edge dislocation populations of subsequent GaN layers. GaN grown on 1030°C AlN buffer layers showed the lowest edge dislocation populations when compared against buffers grown in the range of 1010--1220°C, even though the 1220°C AlN was much smoother. AlGaN buffer layers provided more edge dislocation reduction, with a 1090°C Al0.2Ga0.8N layer yielding the best GaN rocking curve values found in this work. GaN films with AlN buffer layers grown on hydrogen etched SiC substrates did not show rocking curve improvement when compared against samples with unetched substrates. The AlN layers showed extremely narrow, substrate limited, on-axis rocking curve values, but it is not clear as to whether additional defects are present that may broaden the off-axis rocking curves, causing the poorer results seen in the GaN films. Reciprocal space maps of uncoalesced, maskless pendeo epitaxy samples revealed that the wing regions are shielded from poor substrate material when

  2. Quantitative characterization of microstructure of asphalt mixtures

    Science.gov (United States)

    2010-10-01

    The microstructure of the fine aggregate matrix has a significant influence on the : mechanical properties and evolution of damage in an asphalt mixture. However, very little : work has been done to define and quantitatively characterize the microstr...

  3. Microstructural characterization of stone wool fibre network

    DEFF Research Database (Denmark)

    Chapelle, Lucie; Brøndsted, Povl; Kusano, Yukihiro

    2014-01-01

    Understanding the mechanical properties of fibrous network as complex as stone wool materials requires a relevant description of their microstructure and architecture. In this study, different methods have been proposed to characterize the fibre orientation, diameter and length of fibres as well ...

  4. Microstructural characterization of nickel subjected to dynamic plastic deformation

    DEFF Research Database (Denmark)

    Luo, Z.P.; Mishin, Oleg; Zhang, Yubin

    2012-01-01

    Average microstructural parameters and the extent of microstructural heterogeneity in nickel deformed at a high strain rate have been characterized quantitatively and compared to those after compression at a quasi-static strain rate. The microstructure in the high strain rate sample was found to ...

  5. Fabrication and Optical Recombination in III-Nitride Microstructures and Devices

    Science.gov (United States)

    2003-10-01

    Fabrication and optical investigations of III-nitride microstructures Our group has pioneered the fabrication of micro - and nano -size photonic... pumped individual III-nitride micro -size LEDs and micro -LED arrays and observed enhanced quantum efficiencies. The micro -size LEDs were fabricated...quality III-nitride QWs, heterostructures, microstructures, and micro -devices and to study their optical and optoeletronic properties. By optimizing

  6. High-Resolution Characterization of UMo Alloy Microstructure

    Energy Technology Data Exchange (ETDEWEB)

    Devaraj, Arun [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Kovarik, Libor [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Joshi, Vineet V. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Jana, Saumyadeep [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Manandhar, Sandeep [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Arey, Bruce W. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Lavender, Curt A. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States)

    2016-11-30

    This report highlights the capabilities and procedure for high-resolution characterization of UMo fuels in PNNL. Uranium-molybdenum (UMo) fuel processing steps, from casting to forming final fuel, directly affect the microstructure of the fuel, which in turn dictates the in-reactor performance of the fuel under irradiation. In order to understand the influence of processing on UMo microstructure, microstructure characterization techniques are necessary. Higher-resolution characterization techniques like transmission electron microscopy (TEM) and atom probe tomography (APT) are needed to interrogate the details of the microstructure. The findings from TEM and APT are also directly beneficial for developing predictive multiscale modeling tools that can predict the microstructure as a function of process parameters. This report provides background on focused-ion-beam–based TEM and APT sample preparation, TEM and APT analysis procedures, and the unique information achievable through such advanced characterization capabilities for UMo fuels, from a fuel fabrication capability viewpoint.

  7. Microstructural characterization of the γ-TiAl alloy samples ...

    Indian Academy of Sciences (India)

    Home; Journals; Bulletin of Materials Science; Volume 25; Issue 7. Microstructural characterization of the -TiAl alloy samples fabricated by direct laser fabrication rapid prototype technique. D Srivastava. Alloys and Steels Volume 25 ... Keywords. Titanium aluminide; microstructure; direct laser fabrication; rapid prototyping.

  8. Microstructural evaluation of heteroepitaxial III-V semiconductor thin films

    Science.gov (United States)

    Chen, Eric Brice

    Microstructural features of single and multilayered strained (In xGa1-xAs/GaAs, (Al)GaAs1-ySb y/GaAs) and unstrained (In0.49Ga0.51P/GaAs) heteroepitaxial structures were evaluated. During growth of a 1.5% mismatched InxGa 1-xAs layer on GaAs at 470°C, real-time multibeam optical stress sensor measurements revealed an unexpected shoulder in the strain-thickness profile. Real-time data was used to pause film growth at pre-determined stress-states surrounding the shoulder region (pre-, mid- and post-shoulder) to probe its origin. Dislocation structure of each stress-state was characterized by transmission electron microscopy. The shoulder coincided with reactions between 60° dislocations forming edge dislocations, suggesting an increased dislocation mobility which is required for multiplication. Dislocation half-loops were observed via cross-sectional microscopy, resulting in rapid relaxation of the film. In-graded (InxGa1-xAs) and Sb-graded (Al0.5Ga0.5As1-ySby, GaAs 1-ySby) compositionally step-graded multilayer buffers were analyzed to determine the optimal alloy for preventing the propagation of threading dislocations to the epitaxial surface. Multilayers were graded from a lattice parameter of 0.564 nm to 0.591 nm (4.6% mismatch) over a 1 mum film thickness. Threading dislocation density in the top-most layer of the Sb-graded structures (≤109 cm-2) was lower than the In-graded alloy (>1010 cm-2). In the InxGa1-xAs structure, threading dislocations were observed to congregate in discrete channels directly correlated to surface crosshatches. As/Sb compositional modulations in the Sb-graded structures reveal a more planar growth surface, preventing threading dislocation trapping. Characterization of dislocation structure indicated a directional asymmetry in the 60° and edge dislocation density for the GaAs1-ySb y multilayer. Replacing Ga with Al0.5Ga0.5 in the Sb-graded ternary improved planarity, resulting in a more uniform dislocation density. Residual strain

  9. Quantitative Microstructure Characterization of a NMC Electrode

    Energy Technology Data Exchange (ETDEWEB)

    Usseglio-Viretta, François Laurent Emilien; Smith, Kandler

    2017-07-07

    Performance of lithium-ion batteries (LIBs) is strongly influenced by the porous microstructure of their electrodes. In this work, 3D microstructures of calendared and un-calendared positive electrode LiNi1/3Mn1/3Co1/3O2 (NMC) have been investigated in order to extract relevant properties useful for battery modeling. Transport (volume fraction, connectivity, particle size and tortuosity) and electrochemical (specific surface area) properties have been calculated for the pore and the active material. Special attention has been paid to determine the size of the so-called representative volume element (RVE) required to be statistically representative of the heterogeneous medium. Several parameters have been calculated using a panel of different numerical methods in order to compare their results. Besides, the image level of detail has been evaluated (using original criteria based upon edge detection) to assess the overall data quality available for the study.

  10. Quantitative Microstructure Characterization of a NMC Electrode

    Energy Technology Data Exchange (ETDEWEB)

    Usseglio Viretta, Francois L [National Renewable Energy Laboratory (NREL), Golden, CO (United States); Smith, Kandler A [National Renewable Energy Laboratory (NREL), Golden, CO (United States)

    2017-09-28

    Performance of lithium-ion batteries (LIBs) is strongly influenced by the porous microstructure of their electrodes. In this work, 3D microstructures of calendared and un-calendared positive electrode LiNi1/3Mn1/3Co1/3O2 (NMC) have been investigated in order to extract relevant properties useful for battery modeling. Transport (volume fraction, connectivity, particle size and tortuosity) and electrochemical (specific surface area) properties have been calculated for the pore and the active material. Special attention has been paid to determine the size of the so-called representative volume element (RVE) required to be statistically representative of the heterogeneous medium. Several parameters have been calculated using a panel of different numerical methods in order to compare their results. Besides, the image level of detail has been evaluated (using original criteria based upon edge detection) to assess the overall data quality available for the study.

  11. Microstructural and Mechanical Characterization of Solidified Austenitic Stainless Steels

    Directory of Open Access Journals (Sweden)

    Aktaş Çelik G.

    2017-09-01

    Full Text Available Among the family of stainless steels, cast austenitic stainless steels (CASSs are preferably used due to their high mechanical properties and corrosion resistance. These steels owe their properties to their microstructural features consisting of an austenitic matrix and skeletal or lathy type δ-ferrite depending on the cooling rate. In this study, the solidification behavior of CASSs (304L and 316L grades was studied using ThermoCalc software in order to determine the solidification sequence and final microstructure during cooling. Theoretical findings were supported by the microstructural examinations. For the mechanical characterization, not only hardness measurements but also tribological studies were carried out under dry sliding conditions and worn surfaces were examined by microscopy and 3D profilometric analysis. Results were discussed according to the type and amount of microstructural features.

  12. Automated Characterization of Uranium-Molybdenum Fuel Microstructures

    Energy Technology Data Exchange (ETDEWEB)

    Ryan Collette; Jeffrey King; Dennis keiser, Jr.; Jason Schulthess

    2015-04-01

    Currently, performance evaluators rely on visual inspection or manual segmentation to assess most parameters of interest within an irradiated microstructure. Automating this process has the potential to significantly speed up the data extraction process, enhance its reliability, and improve its correctness. Automatic image segmentation of target features is a critical tool for providing measurements of features that may be used to increase the fidelity of fuel performance modeling. This summary will present the progress made in developing and testing automated image processing routines capable of fully characterizing the presence of fission gas bubbles in irradiated U-Mo plate-type fuel microstructures.

  13. Microstructural characterization of a Canadian oil sand

    CERN Document Server

    Dinh, Hong Doan; Nauroy, Jean-François; Tang, Anh-Minh; Souhail, Youssef; 10.1139/T2012-072

    2013-01-01

    The microstructure of oil sand samples extracted at a depth of 75 m from the estuarine Middle McMurray formation (Alberta, Canada) has been investigated by using high resolution 3D X-Ray microtomography ($\\mu$CT) and Cryo Scanning Electron Microscopy (CryoSEM). $\\mu$CT images evidenced some dense areas composed of highly angular grains surrounded by fluids that are separated by larger pores full of gas. 3D Image analysis provided in dense areas porosity values compatible with in-situ log data and macroscopic laboratory determinations, showing that they are representative of intact states. $\\mu$CT hence provided some information on the morphology of the cracks and disturbance created by gas expansion. The CryoSEM technique, in which the sample is freeze fractured within the SEM chamber prior to observation, provided pictures in which the (frozen) bitumen clearly appears between the sand grains. No evidence of the existence of a thin connate water layer between grains and the bitumen, frequently mentioned in th...

  14. Characterization Of The Graded Microstructure In Powder Sintered Porous Titanium

    Directory of Open Access Journals (Sweden)

    Oak J.-J.

    2015-06-01

    Full Text Available The proposed sintering process produce porosity and functional graded microstructure in the sinterd titanium powders. Titanium powders with different micro sizes were sintered at the proposed temperature region at 1200 and 1300°C for 2h. The apatite-forming on the graded microstructure is observed by immersion test in Hanks balanced salt soluion at 37°C. Sintering condition of titanium powders is estimated by thermogravitmetry-differential thermal analysis (TG-DTA. The synthersied surface structures and apatite-forming ability were characterized by a field emission scanning electron microscopy (FE-SEM observation and energy dispersive X-ray spectroscopy (EDS analysis. As results, these graded microstructure of sintered porous titanium powders reveals apatite-forming ability as osseointegration by calcification in Hanks balanced salt soluion(HBSS at 37°C.

  15. Multi-scale Microstructure Characterization for Improved Understanding of Microstructure-Property Relationship in Additive Manufacturing

    Science.gov (United States)

    Song, Hye Yun

    Additive manufacturing (AM) is the process for making 3-D objects by adding materials layer by layer. It can result in a marked reduction of the time and cost associated with designing and producing highly complex parts. Over the past decade, significant progress has been made in machine hardware and control software for process development to achieve dimensional accuracy and mitigate defects. On the other hand, the knowledge on microstructure-property relationship in the additively manufactured builds is still being established. In additive manufacturing, the interactions between the heat source and the material lead to a series of physical phenomena including localized heating, melting, solidification and micro-segregation, and cooling. Far-from-equilibrium microstructure can form as the material experiences a large number of repeated, rapid heating and cooling cycles (i.e. temperature gyrations) during depositions. The mechanical properties of additively manufactured parts are significantly influenced by their final microstructure. The overarching goal of the present research is to improve the fundamental understanding of microstructure-property relationship for AM parts. Specially, it is investigated the high-temperature creep strength of InconelRTM 718 (abbreviated as IN718 thereafter) fabricated by laser-powder bed fusion (L-PBF) AM. The specific objectives include (1) effect of support on the local microstructure, (2) microstructure evolution during post-built heat treatment, and (3) creep strength. Detailed microstructure characterization is performed using a multitude of tools including micro-hardness mapping, scanning electron microscope (SEM) along with electron backscatter diffraction (EBSD), and transmission electron microscope (TEM) for selected area diffraction (SAD) analysis and energy-dispersive X-ray spectroscopy (EDS). The characterized microstructure is correlated to the mechanical properties. Highlights of the research findings are discussed in

  16. Microstructural pavement material characterization: some examples

    CSIR Research Space (South Africa)

    Mgangira, Martin B

    2008-07-01

    Full Text Available The utilisation of advanced measurement techniques should assist in the characterization of pavement materials at a micro-scale. The motivating factor for such an approach is that material properties at the micro-level have a critical role...

  17. Microstructural characterization of nuclear-waste ceramics

    Energy Technology Data Exchange (ETDEWEB)

    Ryerson, F.J.; Clarke, D.R.

    1982-09-22

    Characterization of nuclear waste ceramics requires techniques possessing high spatial and x-ray resolution. XRD, SEM, electron microprobe, TEM and analytical EM techniques are applied to ceramic formulations designed to immobilize both commercial and defense-related reactor wastes. These materials are used to address the strengths and limitations of the techniques above. An iterative approach combining all these techniques is suggested. 16 figures, 2 tables.

  18. Looseness in bovine leather: microstructural characterization.

    Science.gov (United States)

    Wells, Hannah C; Holmes, Geoff; Haverkamp, Richard G

    2016-06-01

    A substantial proportion of bovine leather production may be of poor quality, with the leather suffering from a characteristic known as looseness. This defect results in a poor visual appearance and greatly reduced value. The structural mechanism of looseness is not well understood. Samples of loose and tight bovine leather are characterized using small-angle X-ray scattering, ultrasonic imaging, and electron microscopy. The density of fibre packing and orientation of the fibrils are analysed. Tensile strength is also measured. Loose leather is characterized by more highly aligned collagen fibrils. This results in a weaker connection between the layers. There is a looser packing of the fibres in loose leather than in tight leather, with more gaps between fibre bundles, particularly in a region in the lower grain. This region is visible with in situ ultrasonic imaging. Loose leather has a higher tensile strength than tight leather. While a high degree of collagen fibril alignment is normally associated with strong leather, it has been shown that too much alignment results in loose leather. Understanding the physical basis of looseness is the first step in identifying looseness in hides and learning how to prevent looseness from developing during leather manufacture. © 2015 Society of Chemical Industry. © 2015 Society of Chemical Industry.

  19. Microstructural characterization and adsorption properties of alkali-activated materials based on metakaolin

    Directory of Open Access Journals (Sweden)

    Trivunac Katarina

    2016-01-01

    Full Text Available The microstructural characterization and adsorption properties of metakaolin (MK and alkali-activated metakaolin, known as geopolymer materials (GP were investigated. The structure and properties of the metakaolin and obtained geopolymer were studied by X-ray diffraction (XRD, scanning electron microscopy (SEM and Fourier transform infrared (FTIR spectroscopy. Furthermore, based on the analysis of adsorption efficiency, microstructure and mineral structure, the difference between geopolymer and metakaolin on the performance of immobilizing heavy metals have been discussed. The kinetics of adsorption can be represented by pseudo-second order equation. The results of lead ions adsorption experiments were best fitted by Freundlich adsorption isotherm for both investigated adsorbents. The highest removal efficiencies of alkali-activated material based on metakaolin was found 97.5% at pH 4 and metakaolin removal efficiencies was found 92% at pH 5.5.[Projekat Ministarstva nauke Republike Srbije, br. III 45012 i br. 172007

  20. Surface microstructure of bitumen characterized by atomic force microscopy.

    Science.gov (United States)

    Yu, Xiaokong; Burnham, Nancy A; Tao, Mingjiang

    2015-04-01

    Bitumen, also called asphalt binder, plays important roles in many industrial applications. It is used as the primary binding agent in asphalt concrete, as a key component in damping systems such as rubber, and as an indispensable additive in paint and ink. Consisting of a large number of hydrocarbons of different sizes and polarities, together with heteroatoms and traces of metals, bitumen displays rich surface microstructures that affect its rheological properties. This paper reviews the current understanding of bitumen's surface microstructures characterized by Atomic Force Microscopy (AFM). Microstructures of bitumen develop to different forms depending on crude oil source, thermal history, and sample preparation method. While some bitumens display surface microstructures with fine domains, flake-like domains, and dendrite structuring, 'bee-structures' with wavy patterns several micrometers in diameter and tens of nanometers in height are commonly seen in other binders. Controversy exists regarding the chemical origin of the 'bee-structures', which has been related to the asphaltene fraction, the metal content, or the crystallizing waxes in bitumen. The rich chemistry of bitumen can result in complicated intermolecular associations such as coprecipitation of wax and metalloporphyrins in asphaltenes. Therefore, it is the molecular interactions among the different chemical components in bitumen, rather than a single chemical fraction, that are responsible for the evolution of bitumen's diverse microstructures, including the 'bee-structures'. Mechanisms such as curvature elasticity and surface wrinkling that explain the rippled structures observed in polymer crystals might be responsible for the formation of 'bee-structures' in bitumen. Despite the progress made on morphological characterization of bitumen using AFM, the fundamental question whether the microstructures observed on bitumen surfaces represent its bulk structure remains to be addressed. In addition

  1. Microstructure characterization of nitride thin films and heterostructures

    Science.gov (United States)

    Zhou, Lin

    This dissertation has involved the microstructural characterization of epitaxial III-nitride thin films and heterostructures, and correlation with growth conditions and electronic properties. For AlGaN/GaN high-electron-mobility-transistor (HEMT) structures, when the AlN nucleation layer growth was in the N-rich growth regime, a sharp GaN/AlN interface was observed together with a high threading dislocation (TD) density in the GaN epilayer. When the Al/N flux ratio was increased, the AlN growth was in an intermediate growth regime, resulting in the initial formation of cubic-GaN but lower TD density in the subsequent GaN layer. The presence of c-GaN correlated with an abrupt change in isolation current from 0.089nA to 4.2nA, while the decrease of TD density was related to an increase in the Hall electron mobility. For InAlN/GaN HEMT structures, a vertical honeycomb structure within the InAlN layers was observed. The phase separation was two-dimensional in nature, occurring on the growth surface, and aligned perpendicular to and directions. Development of this honeycomb structure is likely to adversely affect the distribution of any two-dimensional electron gas at the InAlN/GaN interface and would thus be expected to degrade device conductivity. Transmission electron microscopy (TEM) observations of GaN QDs embedded in an AlN matrix showed that the truncated pyramid GaN QDs were dislocation-free. They tended to nucleate beside an edge component TD, with GaN wetting layer thickness of 2-2.5 ML in between. Observations of InN QDs and islands grown on Ga-polar GaN were consistent with a three-dimensional growth mode, with periodic arrays of misfit dislocations at the InN/GaN interface that provided strain relief for the relaxed QDs. The majority of the InN islands were associated with TDs in the GaN buffer layer having edge-type components. The density of TDs in GaN, particularly edge/mixed-type TDs, can be substantially reduced by overgrowth on a porous TiN network

  2. Microstructural Characterization of Friction Stir Welded Aluminum-Steel Joints

    Science.gov (United States)

    Patterson, Erin E.; Hovanski, Yuri; Field, David P.

    2016-06-01

    This work focuses on the microstructural characterization of aluminum to steel friction stir welded joints. Lap weld configuration coupled with scribe technology used for the weld tool have produced joints of adequate quality, despite the significant differences in hardness and melting temperatures of the alloys. Common to friction stir processes, especially those of dissimilar alloys, are microstructural gradients including grain size, crystallographic texture, and precipitation of intermetallic compounds. Because of the significant influence that intermetallic compound formation has on mechanical and ballistic behavior, the characterization of the specific intermetallic phases and the degree to which they are formed in the weld microstructure is critical to predicting weld performance. This study used electron backscatter diffraction, energy dispersive spectroscopy, scanning electron microscopy, and Vickers micro-hardness indentation to explore and characterize the microstructures of lap friction stir welds between an applique 6061-T6 aluminum armor plate alloy and a RHA homogeneous armor plate steel alloy. Macroscopic defects such as micro-cracks were observed in the cross-sectional samples, and binary intermetallic compound layers were found to exist at the aluminum-steel interfaces of the steel particles stirred into the aluminum weld matrix and across the interfaces of the weld joints. Energy dispersive spectroscopy chemical analysis identified the intermetallic layer as monoclinic Al3Fe. Dramatic decreases in grain size in the thermo-mechanically affected zones and weld zones that evidenced grain refinement through plastic deformation and recrystallization. Crystallographic grain orientation and texture were examined using electron backscatter diffraction. Striated regions in the orientations of the aluminum alloy were determined to be the result of the severe deformation induced by the complex weld tool geometry. Many of the textures observed in the weld

  3. Microstructural characterization of concrete prepared with recycled aggregates.

    Science.gov (United States)

    Guedes, Mafalda; Evangelista, Luís; de Brito, Jorge; Ferro, Alberto C

    2013-10-01

    Several authors have reported the workability, mechanical properties, and durability of concrete produced with construction waste replacing the natural aggregate. However, a systematic microstructural characterization of recycled aggregate concrete has not been reported. This work studies the use of fine recycled aggregate to replace fine natural aggregate in the production of concrete and reports the resulting microstructures. The used raw materials were natural aggregate, recycled aggregate obtained from a standard concrete, and Portland cement. The substitution extent was 0, 10, 50, and 100 vol%; hydration was stopped at 9, 24, and 96 h and 28 days. Microscopy was focused on the cement/aggregate interfacial transition zone, enlightening the effect of incorporating recycled aggregate on the formation and morphology of the different concrete hydration products. The results show that concretes with recycled aggregates exhibit typical microstructural features of the transition zone in normal strength concrete. Although overall porosity increases with increasing replacement, the interfacial bond is apparently stronger when recycled aggregates are used. An addition of 10 vol% results in a decrease in porosity at the interface with a corresponding increase of the material hardness. This provides an opportunity for development of increased strength Portland cement concretes using controlled amounts of concrete waste.

  4. Characterization of ribonuclease III from Brucella.

    Science.gov (United States)

    Wu, Chang-Xian; Xu, Xian-Jin; Zheng, Ke; Liu, Fang; Yang, Xu-Dong; Chen, Chuang-Fu; Chen, Huan-Chun; Liu, Zheng-Fei

    2016-04-01

    Bacterial ribonuclease III (RNase III) is a highly conserved endonuclease, which plays pivotal roles in RNA maturation and decay pathways by cleaving double-stranded structure of RNAs. Here we cloned rncS gene from the genomic DNA of Brucella melitensis, and analyzed the cleavage properties of RNase III from Brucella. We identified Brucella-encoding small RNA (sRNA) by high-throughput sequencing and northern blot, and found that sRNA of Brucella and Homo miRNA precursor (pre-miRNA) can be bound and cleaved by B.melitensis ribonuclease III (Bm-RNase III). Cleavage activity of Bm-RNase III is bivalent metal cations- and alkaline buffer-dependent. We constructed several point mutations in Bm-RNase III, whose cleavage activity indicated that the 133th Glutamic acid residue was required for catalytic activity. Western blot revealed that Bm-RNase III was differently expressed in Brucella virulence strain 027 and vaccine strain M5-90. Collectively, our data suggest that Brucella RNase III can efficiently bind and cleave stem-loop structure of small RNA, and might participate in regulation of virulence in Brucella. Copyright © 2016 Elsevier B.V. All rights reserved.

  5. Microstructural characterization of radiation effects in nuclear materials

    CERN Document Server

    2017-01-01

    Microstructural Characterization of Radiation Effects in Nuclear Materials provides an overview into experimental techniques that can be used to examine those effects (both neutron and charged particle) and can be used by researchers, technicians or students as a tool to introduce them to the various techniques. The need to examine the effect of radiation on materials is becoming increasingly important as nuclear energy is emerging as a growing source of renewable energy. The book opens with a discussion of why it is important to study the effects of radiation on materials and looks at current and future reactor designs and the various constraints faced by materials as a result of those designs. The book also includes an overview of the radiation damage mechanisms. The next section explores the various methods for characterizing damage including transmission electron microscopy, scanning transmission electron microscopy, analytical electron microscopy, electron backscatter diffraction, atom probe tomography,...

  6. Microstructural characterization of Mg–Al–Sr alloys

    Directory of Open Access Journals (Sweden)

    M. Aljarrah et al

    2007-01-01

    Full Text Available The microstructural details of fourteen Mg–Al–Sr alloys were investigated in the as-cast form by a combination of scanning electron microscopy/energy dispersive spectrometer (SEM/EDS analysis and quantitative electron probe microanalysis (EPMA. The heat transfer method coupled with the DSC measurement has been utilized to determine the solidification curves of the alloys. The morphology and the chemical composition of the phases were characterized. The microstructure of the alloys is primarily dominated by (Mg and (Al4Sr. In the present investigation, ternary solid solubility of three binary compounds extended into the ternary system has been reported and denoted as: (Al4Sr, (Mg17Sr2 and (Mg38Sr9. The (Al4Sr phase is a substitutional solid solution represented by MgxAl4−xSr and has a plate-like structure. The maximum solubility of Al in Mg17Sr2 was found to be 21.3 at%. It was also observed that Mg38Sr9 dissolved 12.5 at% Al.

  7. Microstructure characterization of porous microalloyed aluminium-silicate ceramics

    Directory of Open Access Journals (Sweden)

    Purenović Jelena

    2011-01-01

    Full Text Available Kaolinite and bentonite clay powders mixed with active additives, based on Mg(NO32 and Al(NO32, sintered at high temperatures produce very porous ceramics with microcrystalline and amorphous regions and highly developed metalized surfaces (mainly with magnesium surplus. Microstructure investigations have revealed non-uniform and highly porous structure with broad distribution of grain size, specifically shaped grains and high degree of agglomeration. The ceramics samples were characterized by scanning electron microscopy (SEM, energy dispersive spectrometer (EDS, X-ray diffraction analysis (XRD and IR spectroscopy analysis, prior and after treatment in “synthetic water”, i.e. in aqueous solution of arsenic-salt. Grain size distribution for untreated and treated samples was done with software SemAfore 4. It has shown great variety in size distribution of grains from clay powders to sintered samples.

  8. Microstructural characterization and simulation of damage for geared sheet components

    Science.gov (United States)

    Gerstein, G.; Isik, K.; Gutknecht, F.; Sieczkarek, P.; Ewert, J.; Tekkaya, A. E.; Clausmeyer, T.; Nürnberger, F.

    2017-09-01

    The evolution of damage in geared components manufactured from steel sheets was investigated, to analyse the influence of damage caused by the sheet-bulk-metal forming. Due to the inhomogeneous and multi-axial deformation in the investigated parts, different aspects such as the location-dependent shape and size of voids are analysed by means of various microscopic methods. In particular, a method to characterize the state of damage evolution, i. e. void nucleation, growth and coalescence using scanning electron microscopy (SEM) is applied. The investigations reveal a strong dependence of the void area fraction, shape of voids and thus damage evolution on the loading mode. The microstructural analysis is complemented with FEM simulations using material models which consider the characteristics of the void evolution.

  9. Microstructure and thermophysical characterization of mixed oxide fuels

    Energy Technology Data Exchange (ETDEWEB)

    Freibert, Franz J [Los Alamos National Laboratory; Salich, Tarik A [Los Alamos National Laboratory; Schwartz, Daniel S [Los Alamos National Laboratory; Hampel, Fred G [Los Alamos National Laboratory; Mitchell, Jeremy N [Los Alamos National Laboratory; Davis, Charles C [Los Alamos National Laboratory; Neuman, Angelique D [Los Alamos National Laboratory; Willson, Steve P [Los Alamos National Laboratory; Dunwoody, John T [Los Alamos National Laboratory

    2009-01-01

    Pre-irradiated thermodynamic and microstructural properties of nuclear fuels form the necessary set of data against which to gauge fuel performance and irradiation damage evolution. This paper summarizes recent efforts in mixed-oxide and minor actinide-bearing mixed-oxide ceramic fuels fabrication and characterization at Los Alamos National Laboratory. Ceramic fuels (U{sub 1-x-y-z}u{sub x}Am{sub y}Np{sub z})O{sub 2} fabricated in the compositional ranges of 0.19 {le} x {le} 0.3 Pu, 0 {le} y {le} 0.05 Am, and O {le} z {le} O.03 Np exhibited a uniform crystalline face-centered cubic phase with an average grain size of 14{micro}m; however, electron microprobe analysis revealed segregation of NpO{sub 2} in minor actinide-bearing fuels. Immersion density and porosity analysis demonstrated an average density of 92.4% theoretical for mixed-oxide fuels and an average density of 89.5 % theoretical density for minor actinide-bearing mixed-oxide fuels. Examined fuels exhibited mean thermal expansion value of 12.56 x 10{sup -6} C{sup -1} for temperature range (100 C < T < 1500 C) and ambient temperature Young's modulus and Poisson's ratio of 169 GPa and of 0.327, respectively. Internal dissipation as determined from mechanical resonances of these ceramic fuels has shown promise as a tool to gauge microstructural integrity and to interrogate fundamental properties.

  10. Microstructural and mechanical characterization of Al–Zn–Si nanocomposites

    Energy Technology Data Exchange (ETDEWEB)

    García-Villarreal, S. [Centro de Investigación en Materiales Avanzados S.C. Monterrey, 66600, Alianza Nte. 202, Parque PIIT, Apodaca, N.L. (Mexico); Chávez-Valdez, A. [Katcon Institute for Innovation and Technology KIIT, 66629, Alianza Sur 200, Apodaca, N.L. (Mexico); Moreno, K.J. [Instituto Tecnológico de Celaya, Apartado Postal 57, 38010 Celaya, Guanajuato (Mexico); Leyva, C.; Aguilar-Martínez, J.A. [Centro de Investigación en Materiales Avanzados S.C. Monterrey, 66600, Alianza Nte. 202, Parque PIIT, Apodaca, N.L. (Mexico); Hurtado, A. [Centro de Investigación en Materiales Avanzados S.C., 31109, Miguel de Cervantes 120, Chih., Chih. (Mexico); Arizmendi-Morquecho, A., E-mail: ana.arizmendi@cimav.edu.mx [Centro de Investigación en Materiales Avanzados S.C. Monterrey, 66600, Alianza Nte. 202, Parque PIIT, Apodaca, N.L. (Mexico)

    2013-09-15

    In this paper the addition of silicon nanoparticles into Al–Zn alloys to form metallic matrix nanocomposites by mechanical alloying process was investigated. The influence of various process parameters such as milling time and Si concentration in the Al–Zn matrix has an interesting effect on the microstructure and mechanical properties of the synthesized nanocomposites. The microstructural characterization of the nanocomposites was evaluated by transmission electron microscopy and energy dispersive X-ray spectroscopy (TEM–EDXS) and the mechanical properties were measured by nanoindentation and micro-hardness tests. The results showed that during mechanical milling Si is added to the Al–Zn matrix achieving a uniform and homogeneous dispersion. After solidification, it forms small particles of AlZnSi with blocky morphology in interdendritic regions. The nanoindentation profiles showed that the elastic modulus and hardness properties increase with increasing milling time. However, a high concentration of Si (> 1.2 wt.%) results in a saturation of Si in the Al–Zn matrix, which adversely affects the mechanical properties. Thus, it is important to tune the milling time and concentration of Si added to the Al–Zn alloys to control the growth of brittle phases that result in reduction of the mechanical properties of the material. - Highlights: • A novel technique for addition of Si nanocomposites into Al–Zn liquid alloy is reported. • Good dispersion and homogeneity of Si in the Al–Zn matrix are obtained. • Increasing Si content above 1.2 wt.% decreases the mechanical properties of Al–Zn alloy. • The saturation point of Si in 1.2 wt.% differs from Galvalume® composition. • The Al–Zn–1.5Si alloy with addition of nanocomposite shows 5.7 GPa of hardness.

  11. Measurement and characterization of three-dimensional microstructures on precision roller surfaces

    Science.gov (United States)

    Kong, L. B.; Cheung, C. F.; Lee, W. B.; To, S.; Ren, M. J.

    2016-01-01

    Precision roller with microstructures is the key tooling component in the precision embossing by roller process such as Roll-to-Roll to manufacture optical plastic plates or films with three dimensional (3D)-microstructures. Measurement and analysis of 3D-microstructures on a precision roller is essential before the embossing process is being undertaken to ensure the quality of the embossed surfaces. Different from 3D-microstructures on a planar surface, it is difficult to measure and characterize the 3D-microstructures on the cylindrical surface of a precision roller due to the geometrical complexity of such integrated surfaces such as V-groove microstructures on a cylindrical surface. This paper presents a study of method and algorithms for the measurement and characterization of 3D-microstructures on a precision roller surface. A feature-based characterization method (FBCM) is proposed to analyze the V-groove microstructures. In this method, a normal template is generated based on the design specifications, and the measured data is fitted with the feature points. Hence alignment and matching of the measured data to the normal template based on the derived feature points are undertaken. After that the V-groove is characterized by some feature parameters such as pitch, depth, angle of the V-grooves. The method also provides an approach for the analysis of burs generated during the machining of Vgroove microstructures. A precision roller with V-groove microstructures has been machined by a Four-axis ultraprecision machine and the machined surface is measured by a contact measuring instrument. The measured data are then characterized and analyzed by the proposed FBCM. The results are presented and discussed, and they indicate the dominant and regular machining errors that are involved in the machining of the V-groove microstructures on roller surfaces.

  12. Microstructural and Fractographic Characterization of a Thermally Embrittled Nuclear Grade Steel: Part I - Annealing

    Directory of Open Access Journals (Sweden)

    Tarpani José R.

    2002-01-01

    Full Text Available A nuclear reactor pressure vessel steel was submitted to different annealing heat treatments aimed at simulating neutron irradiation damage. The obtained microstructures were mechanically tested with subsequent metallographic and fractographic characterization. The relevant microstructural and fractographic aspects were employed in the interpretation of the mechanical behavior of the microstructures in both quasi-static (J-R curve and dynamic (Charpy impact loading regimes. A well defined relationship was determined between the elastic-plastic fracture toughness parameter J-integral and the Charpy impact energy for very most of the microstructures.

  13. Microstructural characterization of as-cast hf-b alloys

    Directory of Open Access Journals (Sweden)

    João Carlos Jânio Gigolotti

    2012-04-01

    Full Text Available An accurate knowledge of several metal-boron phase diagrams is important to evaluation of higher order systems such as metal-silicon-boron ternaries. The refinement and reassessment of phase diagram data is a continuous work, thus the reevaluation of metal-boron systems provides the possibility to confirm previous data from an investigation using higher purity materials and better analytical techniques. This work presents results of rigorous microstructural characterization of as-cast hafnium-boron alloys which are significant to assess the liquid composition associated to most of the invariant reactions of this system. Alloys were prepared by arc melting high purity hafnium (minimum 99.8% and boron (minimum 99.5% slices under argon atmosphere in water-cooled copper crucible with non consumable tungsten electrode and titanium getter. The phases were identified by scanning electron microscopy, using back-scattered electron image mode and X-ray diffraction. In general, a good agreement was found between our data and those from the currently accepted Hafnium-Boron phase diagram. The phases identified are αHfSS and B-RhomSS, the intermediate compounds HfB and HfB2 and the liquide L. The reactions are the eutectic L ⇔ αHfSS + HfB and L ⇔ HfB2 + B-Rhom, the peritectic L + HfB2 ⇔ HfB and the congruent formation of HfB2.

  14. Microstructural Characterization of Alloy 617 Crept into the Tertiary Regime

    Energy Technology Data Exchange (ETDEWEB)

    Lillo, Thomas Martin [Idaho National Laboratory; Wright, Richard Neil [Idaho National Laboratory

    2015-07-01

    The microstructure of Alloy 617 was characterized following creep tests interrupted at total creep strains ranging from 2-20%. A range of creep temperatures (750-1000oC) and initial creep stresses (10-145 MPa) produced creep test durations ranging from 1 to 5800 hours. Image analysis of optical photomicrographs on longitudinal sections of the gage length was used to document the fraction of creep porosity as a function of creep parameters. Creep porosity was negligible below tertiary creep strains of 10% and increased with tertiary creep strain, thereafter. For a given temperature and total creep strain, creep porosity increased with decreasing creep stress. Creep porosity increased linearly with duration of the creep experiment. TEM performed on the gage sections did not reveal significant creep cavity formation on grain boundaries at the sub-micron level. It was concluded that the onset of tertiary creep did not result from creep cavitation and more likely arose due to the formation of low energy dislocation substructures with increasing tertiary strain.

  15. Characterization of the biochemical properties of Campylobacter jejuni RNase III.

    Science.gov (United States)

    Haddad, Nabila; Saramago, Margarida; Matos, Rute G; Prévost, Hervé; Arraiano, Cecília M

    2013-11-25

    Campylobacter jejuni is a foodborne bacterial pathogen, which is now considered as a leading cause of human bacterial gastroenteritis. The information regarding ribonucleases in C. jejuni is very scarce but there are hints that they can be instrumental in virulence mechanisms. Namely, PNPase (polynucleotide phosphorylase) was shown to allow survival of C. jejuni in refrigerated conditions, to facilitate bacterial swimming, cell adhesion, colonization and invasion. In several microorganisms PNPase synthesis is auto-controlled in an RNase III (ribonuclease III)-dependent mechanism. Thereby, we have cloned, overexpressed, purified and characterized Cj-RNase III (C. jejuni RNase III). We have demonstrated that Cj-RNase III is able to complement an Escherichia coli rnc-deficient strain in 30S rRNA processing and PNPase regulation. Cj-RNase III was shown to be active in an unexpectedly large range of conditions, and Mn2+ seems to be its preferred co-factor, contrarily to what was described for other RNase III orthologues. The results lead us to speculate that Cj-RNase III may have an important role under a Mn2+-rich environment. Mutational analysis strengthened the function of some residues in the catalytic mechanism of action of RNase III, which was shown to be conserved.

  16. Microstructure characterization of Cu processed by compression with oscillatory torsion

    Energy Technology Data Exchange (ETDEWEB)

    Rodak, K., E-mail: kinga.rodak@polsl.pl [Institute of Materials Science, Silesian University of Technology, Krasińskiego 8, 40-019 Katowice (Poland); Pawlicki, J., E-mail: jacek.pawlicki@polsl.pl [Department of Automotive Vehicle Construction, Silesian University of Technology, Krasińskiego 8, 40–019 Katowice (Poland)

    2014-08-15

    High purity Cu (99.9%) was subjected to severe plastic deformation up to a total effective strain ε{sub ft} = 130 through compression with the oscillatory torsion method at room temperature. This method produces an ultrafine grain microstructure. The microstructure evolution was investigated with respect to the value of the total effective strain using a scanning electron microscope with an electron-backscattered diffraction technique and a scanning transmission electron microscope. The results of the structural analyses show that increasing ε{sub ft} from 2 to 50 causes progress in the grain refinement. A quantitative study of the microstructure parameters, such as fraction of high angle boundaries, grain and subgrain diameter, and the area fraction of grains up to 1 μm, shows that deformation at ε{sub ft} = 45 guaranteed the best conditions for refining the microstructure of Cu. Using high values of ε{sub ft} in the range 60 to 130 restricts grain refinement because intensive recovery begins to dominate in the microstructure. - Highlights: • Cu was processed by SPD metodto an effective strain 130. • The microstructure evolution has been investigated. • The method allows to produce an ultrafine grain microstructure.

  17. Microstructural characterization of multiphase chocolate using X-ray microtomography.

    Science.gov (United States)

    Frisullo, Pierangelo; Licciardello, Fabio; Muratore, Giuseppe; Del Nobile, Matteo Alessandro

    2010-09-01

    In this study, X-ray microtomography (μCT) was used for the image analysis of the microstructure of 12 types of Italian aerated chocolate chosen to exhibit variability in terms of cocoa mass content. Appropriate quantitative 3-dimensional parameters describing the microstructure were calculated, for example, the structure thickness (ST), object structure volume ratio (OSVR), and the percentage object volume (POV). Chemical analysis was also performed to correlate the microstructural data to the chemical composition of the samples. Correlation between the μCT parameters acquired for the pore microstructure evaluation and the chemical analysis revealed that the sugar crystals content does not influence the pore structure and content. On the other hand, it revealed that there is a strong correlation between the POV and the sugar content obtained by chemical analysis. The results from this study show that μCT is a suitable technique for the microstructural analysis of confectionary products such as chocolates and not only does it provide an accurate analysis of the pores and microstructure but the data obtained could also be used to aid in the assessment of its composition and consistency with label specifications. X-ray microtomography (μCT) is a noninvasive and nondestructive 3-D imaging technique that has several advantages over other methods, including the ability to image low-moisture materials. Given the enormous success of μCT in medical applications, material science, chemical engineering, geology, and biology, it is not surprising that in recent years much attention has been focused on extending this imaging technique to food science as a useful technique to aid in the study of food microstructure. X-ray microtomography provides in-depth information on the microstructure of the food product being tested; therefore, a better understanding of the physical structure of the product and from an engineering perspective, knowledge about the microstructure of

  18. Characterization of the microstructure in Mg based alloy

    KAUST Repository

    Kutbee, Arwa T

    2013-06-01

    The cast products Mg–Sn based alloys are promising candidates for automobile industries, since they provide a cheap yet thermally stable alternative to existing alloys. One drawback of the Mg–Sn based alloys is their insufficient hardness. The hardenability can be improved by engineering the microstructure through additions of Zn to the base alloy and selective aging conditions. Therefore, detailed knowledge about the microstructural characteristics and the role of Zn to promote precipitation hardening is essential for age hardenable Mg-based alloys. In this work, microstructural investigation of the Mg–1.4Sn–1.3Zn–0.1Mn (at.%) precipitation system was performed using TEM. The chemical composition of the precipitates was analyzed using EDS. APT was employed to obtain precise chemical information on the distribution of Zn in the microstructure. It was found from microstructural studies that different precipitates with varying sizes and phases were present; lath-shaped precipitates of the Mg2Sn phase have an incoherent interface with the matrix, unlike the lath-shaped MgZn2 precipitates. Furthermore, nano-sized precipitates dispersed in the microstructure with short-lath morphology can either be enriched with Sn or Zn. On the other hand, APT analysis revealed the strong repulsion between Sn and Zn atoms in a portion of the analysis volume. However, larger reconstruction volume required to identify the role of Zn is still limited to the optimization of specimen preparation.

  19. Linking Experimental Characterization and Computational Modeling in Microstructural Evolution

    Energy Technology Data Exchange (ETDEWEB)

    Demirel, Melik Cumhar [Univ. of Pittsburgh, PA (United States)

    2002-06-01

    It is known that by controlling microstructural development, desirable properties of materials can be achieved. The main objective of our research is to understand and control interface dominated material properties, and finally, to verify experimental results with computer simulations. In order to accomplish this objective, we studied the grain growth in detail with experimental techniques and computational simulations. We obtained 5170-grain data from an Aluminum-film (120μm thick) with a columnar grain structure from the Electron Backscattered Diffraction (EBSD) measurements. Experimentally obtained starting microstructure and grain boundary properties are input for the three-dimensional grain growth simulation. In the computational model, minimization of the interface energy is the driving force for the grain boundary motion. The computed evolved microstructure is compared with the final experimental microstructure, after annealing at 550 ºC. Two different measures were introduced as methods of comparing experimental and computed microstructures. Modeling with anisotropic mobility explains a significant amount of mismatch between experiment and isotropic modeling. We have shown that isotropic modeling has very little predictive value. Microstructural evolution in columnar Aluminum foils can be correctly modeled with anisotropic parameters. We observed a strong similarity between grain growth experiments and anisotropic three-dimensional simulations.

  20. Linking Experimental Characterization and Computational Modeling in Microstructural Evolution

    Energy Technology Data Exchange (ETDEWEB)

    Demirel, Melik Cumhur [Univ. of California, Berkeley, CA (United States)

    2002-06-01

    It is known that by controlling microstructural development, desirable properties of materials can be achieved. The main objective of our research is to understand and control interface dominated material properties, and finally, to verify experimental results with computer simulations. In order to accomplish this objective, we studied the grain growth in detail with experimental techniques and computational simulations. We obtained 5170-grain data from an Aluminum-film (120μm thick) with a columnar grain structure from the Electron Backscattered Diffraction (EBSD) measurements. Experimentally obtained starting microstructure and grain boundary properties are input for the three-dimensional grain growth simulation. In the computational model, minimization of the interface energy is the driving force for the grain boundary motion. The computed evolved microstructure is compared with the final experimental microstructure, after annealing at 550 ºC. Two different measures were introduced as methods of comparing experimental and computed microstructures. Modeling with anisotropic mobility explains a significant amount of mismatch between experiment and isotropic modeling. We have shown that isotropic modeling has very little predictive value. Microstructural evolution in columnar Aluminum foils can be correctly modeled with anisotropic parameters. We observed a strong similarity

  1. Spectral characterization and DNA binding properties of lanthanide(III)

    African Journals Online (AJOL)

    ... with CT-DNA was investigated using absorption spectrophotometry. Based on spectral changes, groove binding of complexes to DNA is suggested. KEY WORDS: Lanthanide(III) complexes, 2-Acetylpyridine isonicotinoylhydrazone, Spectral characterization, DNA binding. Bull. Chem. Soc. Ethiop. 2016, 30(2), 221-230.

  2. Synthesis and Characterization of a Schiff Base Cobalt (III) Complex ...

    African Journals Online (AJOL)

    2017-12-18

    Dec 18, 2017 ... Synthesis and Characterization of a Schiff Base Cobalt (III) Complex and. Assessment of its Anti-Cancer Activity. Gwaram, N. S.. Department of Pure and Industrial Chemistry, Umaru Musa Yar'Adua University. P.M.B. 2211, Katsina, ... compounds of cobalt, copper, nickel, manganese, zinc, palladium ...

  3. Synthesis and characterization of a Schiff base Cobalt (III) complex ...

    African Journals Online (AJOL)

    Cobalt (III) tris(azido)-2-Morpholino-N-(1-(2-pyridyl)ethylidene)ethanamine complex was synthesized, characterized and evaluated for in vitro anticancer activities. The chemical structure of the compound was assessed by elemental analysis, single crystal x-ray crystallography, FT-IR and UV-Visible spectroscopy.

  4. Microstructural Characterization of Low Temperature Gas Nitrided Martensitic Stainless Steel

    DEFF Research Database (Denmark)

    Fernandes, Frederico Augusto Pires; Christiansen, Thomas Lundin; Somers, Marcel A. J.

    2015-01-01

    The present work presents microstructural investigations of the surface zone of low temperature gas nitrided precipitation hardening martensitic stainless steel AISI 630. Grazing incidence X-ray diffraction was applied to investigate the present phases after successive removal of very thin sectio...

  5. Quantitative characterization of processing-microstructure-properties relationships in pressure die-cast magnesium alloys

    Science.gov (United States)

    Lee, Soon Gi

    The central goal of this research is to quantitatively characterize the relationships between processing, microstructure, and mechanical properties of important high-pressure die-cast (HPDC) Mg-alloys. For this purpose, a new digital image processing technique for automatic detection and segmentation of gas and shrinkage pores in the cast microstructure is developed and it is applied to quantitatively characterize the effects of HPDC process parameters on the size distribution and spatial arrangement of porosity. To get better insights into detailed geometry and distribution of porosity and other microstructural features, an efficient and unbiased montage based serial sectioning technique is applied for reconstruction of three-dimensional microstructures. The quantitative microstructural data have been correlated to the HPDC process parameters and the mechanical properties. The analysis has led to hypothesis of formation of new type of shrinkage porosity called, "gas induced shrinkage porosity" that has been substantiated via simple heat transfer simulations. The presence of inverse surface macrosegregation has been also shown for the first time in the HPDC Mg-alloys. An image analysis based technique has been proposed for simulations of realistic virtual microstructures that have realistic complex pore morphologies. These virtual microstructures can be implemented in the object oriented finite elements framework to model the variability in the fracture sensitive mechanical properties of the HPDC alloys.

  6. Characterization of human carbonic anhydrase III from skeletal muscle.

    Science.gov (United States)

    Carter, N; Jeffery, S; Shiels, A; Edwards, Y; Tipler, T; Hopkinson, D A

    1979-10-01

    A third form of human carbonic anhydrase (CA III), found at high concentrations in skeletal muscle, has been purified and characterized. This isozyme shows relatively poor hydratase and esterase activities compared to the red cell isozymes, CA I and CA II, but is similar to these isozymes in subunit structure (monomer) and molecular size (28,000). CA III is liable to posttranslational modification by thiol group interaction. Monomeric secondary isozymes, sensitive to beta-mercaptoethanol, are found in both crude and purified material and can be generated in vitro by the addition of thiol reagents. Active dimeric isozymes, generated apparently by the formation of intermolecular disulfide bridges, also occur but account for only a small proportion of the total protein and appear only when the concentration of CA III is particularly high.

  7. [Characterization of Bacillus thuringiensis spoIII D gene mutation].

    Science.gov (United States)

    Zhang, Qianqian; Shu, Changlong; Zhang, Jie; Huang, Dafang; Song, Fuping

    2009-09-01

    Construction and characterization of a spoIII D gene deletion mutant of Bacillus thuringiensis. Scanning electron microscopy and spore formation analysis were used to detect the ability of sporulation and formation of crystal protein in both the mutant and the wild strain. SDS-PAGE analysis was used to detect the expression of crystal protein. Scanning electron microscopy and spore formation analysis showed that spores were hardly produced and the crystal existed in the spoIII D deletion strain. SDS-PAGE results showed that the expression of cry gene in the mutant was decreased in Luria-Bertani medium, but not affected obviously in Schaeffer's sporulation medium (SSM). This indicated that the spoIII D gene was one of the essential genes for the sporulation of Bacillus thuringiensis, and influenced the expression of crystal protein.

  8. Characterization and influence of deformation microstructure heterogeneity on recrystallization

    DEFF Research Database (Denmark)

    Godfrey, A.; Mishin, Oleg V.; Yu, Tianbo

    2015-01-01

    . A methodology for quantifying this type of heterogeneity based on the identification of areas classified as low misorientation regions (LMRs) is described, and some parameters for quantification of both the extent and length scale of LMRs are presented. It is then shown how this approach can be used......The microstructure resulting from plastic deformation of metals typically contains heterogeneity on several length scales. This is also true for samples deformed to large strains, where an important form of heterogeneity is in the variation in microstructural refinement by high angle boundaries...... to investigate the early stages of recrystallization in samples deformed to large strains, by direct comparison of electron backscatter diffraction (EBSD) maps of the same area before and after annealing. Methods for estimation of the stored energy of deformation from EBSD data are also surveyed and the problems...

  9. Microstructure characterization and magnetic properties of nano structured materials

    Energy Technology Data Exchange (ETDEWEB)

    Sun, X.C

    2000-07-01

    The present thesis deals with the unique microstructural properties and their novel magnetic properties of core-shell Ni-Ce nano composite particles, carbon encapsulated Fe, Co, and Ni nanoparticles and the nano crystallization behavior of typical ferromagnetic Fe{sub 78}Si{sub 9}B{sub 13} ribbons. These properties have intensively been investigated by high resolution transmission electron microscopy (HREM), X-ray diffraction (XRD), scanning electron microscopy (Sem), X-ray energy dispersive spectroscopy [eds.]; selected area electron diffraction pattern (SAED), Ft-IR, differential scanning calorimeter (DSC). In addition, magnetic moments measurements at different temperatures and applied fields have been performed by transmission Moessbauer spectroscopy, superconducting quantum interference device magnetometer (SQUID), and vibrating sample magnetometer (VSM). The present studies may provide the insights for the better understanding of the correlation between the unique microstructure and novel magnetic properties for several magnetic nano structured materials. (Author)

  10. Microstructure Characterization and Modeling for Improved Electrode Design

    Energy Technology Data Exchange (ETDEWEB)

    Smith, Kandler A [National Renewable Energy Laboratory (NREL), Golden, CO (United States); Usseglio Viretta, Francois L [National Renewable Energy Laboratory (NREL), Golden, CO (United States); Graf, Peter A [National Renewable Energy Laboratory (NREL), Golden, CO (United States); Santhanagopalan, Shriram [National Renewable Energy Laboratory (NREL), Golden, CO (United States); Pesaran, Ahmad A [National Renewable Energy Laboratory (NREL), Golden, CO (United States); Yao, Koffi (Pierre) [Argonne National Laboratory; ; Dees, Dennis [Argonne National Laboratory; Jansen, Andy [Argonne National Laboratory; Mukherjee, Partha [Texas A& M University; Mistry, Aashutosh [Texas A& M University; Verma, Ankit [Texas A& M University

    2017-08-03

    This presentation describes research work led by NREL with team members from Argonne National Laboratory and Texas A&M University in microstructure analysis, modeling and validation under DOE's Computer-Aided Engineering of Batteries (CAEBAT) program. The goal of the project is to close the gaps between CAEBAT models and materials research by creating predictive models that can be used for electrode design.

  11. Meal Microstructure Characterization from Sensor-Based Food Intake Detection

    Directory of Open Access Journals (Sweden)

    Abul Doulah

    2017-07-01

    Full Text Available To avoid the pitfalls of self-reported dietary intake, wearable sensors can be used. Many food ingestion sensors offer the ability to automatically detect food intake using time resolutions that range from 23 ms to 8 min. There is no defined standard time resolution to accurately measure ingestive behavior or a meal microstructure. This paper aims to estimate the time resolution needed to accurately represent the microstructure of meals such as duration of eating episode, the duration of actual ingestion, and number of eating events. Twelve participants wore the automatic ingestion monitor (AIM and kept a standard diet diary to report their food intake in free-living conditions for 24 h. As a reference, participants were also asked to mark food intake with a push button sampled every 0.1 s. The duration of eating episodes, duration of ingestion, and number of eating events were computed from the food diary, AIM, and the push button resampled at different time resolutions (0.1–30s. ANOVA and multiple comparison tests showed that the duration of eating episodes estimated from the diary differed significantly from that estimated by the AIM and the push button (p-value <0.001. There were no significant differences in the number of eating events for push button resolutions of 0.1, 1, and 5 s, but there were significant differences in resolutions of 10–30s (p-value <0.05. The results suggest that the desired time resolution of sensor-based food intake detection should be ≤5 s to accurately detect meal microstructure. Furthermore, the AIM provides more accurate measurement of the eating episode duration than the diet diary.

  12. Methods for the In-Situ Characterization of Cast Austenitic Stainless Steel Microstructures

    Science.gov (United States)

    Ramuhalli, P.; Good, M. S.; Harris, R. J.; Bond, L. J.; Ruud, C. O.; Diaz, A. A.; Anderson, M. T.

    2011-06-01

    Cast austenitic stainless steel (CASS) that was commonly used in U.S. nuclear power plants is a coarse-grained, elastically anisotropic material. Its engineering properties made it a material of choice for selected designs of nuclear power reactor systems. However, the material manufacturing and fabrication processes result in a variety of coarse-grain microstructures that make current ultrasonic in-service inspection of components quite challenging. To address inspection needs, new ultrasonic inspection approaches are being sought. However, overcoming the deleterious and variable effects of the microstructure on the interrogating ultrasonic beam may require knowledge of the microstructure, for potential optimization of inspection parameters to enhance the probability of detection (POD). The ability to classify microstructure type (e.g. polycrystalline or columnar) has the potential to guide selection of optimal NDE approaches. This paper discusses the application of ultrasonic and electromagnetic methods for classifying CASS microstructures, when making measurements from the outside surface of the component. Results to date demonstrate the potential of these measurements to discriminate between two consistent microstructures—equiaxed-grain material versus columnar-grain material. The potential for fusion of ultrasonic and electromagnetic measurements for in-situ microstructure characterization in CASS materials will be explored.

  13. SEM Characterization of the High Burn-up Microstructure of U-7Mo Alloy

    Energy Technology Data Exchange (ETDEWEB)

    Dennis D. Keiser, Jr.; Jan-Fong Jue; Jian Gan; Brandon Miller; Adam Robinson; Pavel Medvedev; James Madden; Dan Wachs; M. Teague

    2014-04-01

    During irradiation, the microstructure of U-7Mo evolves until at a fission density near 5x1021 f/cm3 a high-burnup microstructure exists that is very different than what was observed at lower fission densities. This microstructure is dominated by randomly distributed, relatively large, homogeneous fission gas bubbles. The bubble superlattice has collapsed in many microstructural regions, and the fuel grain sizes, in many areas, become sub-micron in diameter with both amorphous fuel and crystalline fuel present. Solid fission product precipitates can be found inside the fission gas bubbles. To generate more information about the characteristics of the high-fission density microstructure, three samples irradiated in the RERTR-7 experiment have been characterized using a scanning electron microscope equipped with a focused ion beam. The FIB was used to generate samples for SEM imaging and to perform 3D reconstruction of the microstructure, which can be used to look for evidence of possible fission gas bubble interlinkage.

  14. Classification and characterization of class III malocclusion in Chinese individuals.

    Science.gov (United States)

    Li, Cai; Cai, Ying; Chen, Sihui; Chen, Fengshan

    2016-11-07

    Class III malocclusion is a maxillofacial disorder that is characterised by a concave profile and can be attributed to both genetic inheritance and environmental factors. It is a clinical challenge due to our limited understanding of its aetiology. Revealing its prototypical diversity will contribute to our sequential exploration of the underlying aetiological information. The objective of this study was to characterize phenotypic variations of Class III malocclusion via a lateral cephalometric analysis in a community of Chinese individuals. One-hundred-and-forty-four individuals (58 males ≥18 and 86 females ≥16) with Class III malocclusion ranging from mild to severe were enrolled in this study. Principal component analysis and cluster analysis were performed using 61 lateral cephalometric measurements. Six principal components were discovered in the examined population and were responsible for 73.7 % of the variability. Four subtypes were revealed by cluster analysis. Subtype 1 included subjects with mild mandibular prognathism with a steep mandibular plane. Subjects in subtype 2 showed a combination of prognathic mandibular and retrusive maxillary with a flat or normal mandibular plane. Subtype 3 included individuals with purely severe mandibular prognathism and a normal mandibular plane. Individuals in subtype 4 had a mild maxillary deficiency and severe mandibular prognathism with the lowest mandibular plane angle. The six principal components extracted among the 61 variables improve our knowledge of lateral cephalometric analysis for diagnoses. We successfully identified four Class III malocclusion subtypes, indicating that cluster analysis could supplement the classification of Class III malocclusion among a Chinese population and may assist in our on-going genetic study.

  15. Relationship Between Microstructure, Strength, and Fracture in an Al-Zn-Mg Electron Beam Weld: Part I: Microstructure Characterization

    Science.gov (United States)

    Puydt, Quentin; Flouriot, Sylvain; Ringeval, Sylvain; De Geuser, Frédéric; Parry, Guillaume; Deschamps, Alexis

    2014-12-01

    This work presents a detailed, multiscale, spatially resolved study of the microstructure of an electron beam butt weld of the EN-AW 7020 (Al-Zn-Mg) alloy. Using a combination of optical, scanning and transmission electron microscopy, differential scanning calorimetry, and small-angle X-ray scattering, the distribution of phases in the different areas of the heat-affected zone and of the fusion zone is quantitatively characterized, for two different aging states: naturally aged after welding and artificially aged at 423 K (150 °C). The heat-affected zone consists of regions experiencing different levels of precipitate dissolution and coarsening during welding as well as new precipitation during post-welding heat treatment (PWHT). The microstructure of the fusion zone is typical from a fast solidification process, with a strong solute segregation in the interdendritic zones. The precipitate distribution after PWHT follows this solute distribution, and the resulting hardness is much lower than the relatively homogeneous value in the base metal and the heat-affected zone.

  16. Microstructure characterization in the weld metals of HQ130 + QJ63 ...

    Indian Academy of Sciences (India)

    Unknown

    2002-11-27

    Nov 27, 2002 ... Abstract. Microstructural characterization of the weld metals of HQ130 + QJ63 high strength steels, welded under 80% Ar + 20% CO2 gas shielded metal arc welding and different weld heat inputs, was carried out by means of scanning electron microscopy (SEM) and transmission electron microscopy ...

  17. Microstructure characterization in the weld metals of HQ130+ QJ63 ...

    Indian Academy of Sciences (India)

    Microstructural characterization of the weld metals of HQ130 + QJ63 high strength steels, welded under 80% Ar + 20% CO2 gas shielded metal arc welding and different weld heat inputs, was carried out by means of scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The relative contents of ...

  18. Post irradiated microstructural characterization of Zr–1Nb alloy by X ...

    Indian Academy of Sciences (India)

    Abstract. Zr–1Nb samples were irradiated with 116 MeV O5+ ions at different doses ranging from 5 × 1017 to 8 ×. 1018 O5+/m2. X-ray diffraction line profile analysis was performed to characterize the microstructural parameters of these samples. Average domain size, microstrain and dislocation density were estimated as a ...

  19. Structural characterization of Spinacia oleracea trypsin inhibitor III (SOTI-III).

    Science.gov (United States)

    Glotzbach, Bernhard; Schmelz, Stefan; Reinwarth, Michael; Christmann, Andreas; Heinz, Dirk W; Kolmar, Harald

    2013-01-01

    In recent decades, several canonical serine protease inhibitor families have been classified and characterized. In contrast to most trypsin inhibitors, those from garden four o'clock (Mirabilis jalapa) and spinach (Spinacia oleracea) do not share sequence similarity and have been proposed to form the new Mirabilis serine protease inhibitor family. These 30-40-amino-acid inhibitors possess a defined disulfide-bridge topology and belong to the cystine-knot miniproteins (knottins). To date, no atomic structure of this inhibitor family has been solved. Here, the first structure of S. oleracea trypsin inhibitor III (SOTI-III), in complex with bovine pancreatic trypsin, is reported. The inhibitor was synthesized by solid-phase peptide synthesis on a multi-milligram scale and was assayed to test its inhibitory activity and binding properties. The structure confirmed the proposed cystine-bridge topology. The structural features of SOTI-III suggest that it belongs to a new canonical serine protease inhibitor family with promising properties for use in protein-engineering and medical applications.

  20. Characterization, Microstructure, and Dielectric properties of cubic pyrochlore structural ceramics

    KAUST Repository

    Li, Yangyang

    2013-05-01

    The (BMN) bulk materials were sintered at 1050°C, 1100°C, 1150°C, 1200°C by the conventional ceramic process, and their microstructure and dielectric properties were investigated by Scanning electron microscopy (SEM), X-ray diffraction (XRD), Raman spectroscopy, Transmission electron microscopy (TEM) (including the X-ray energy dispersive spectrometry EDS and high resolution transmission electron microscopy HRTEM) and dielectric impedance analyzer. We systematically investigated the structure, dielectric properties and voltage tunable property of the ceramics prepared at different sintering temperatures. The XRD patterns demonstrated that the synthesized BMN solid solutions had cubic phase pyrochlore-type structure when sintered at 1050°C or higher, and the lattice parameter (a) of the unit cell in BMN solid solution was calculated to be about 10.56Å. The vibrational peaks observed in the Raman spectra of BMN solid solutions also confirmed the cubic phase pyrochlore-type structure of the synthesized BMN. According to the Scanning Electron Microscope (SEM) images, the grain size increased with increasing sintering temperature. Additionally, it was shown that the densities of the BMN ceramic tablets vary with sintering temperature. The calculated theoretical density for the BMN ceramic tablets sintered at different temperatures is about 6.7521 . The density of the respective measured tablets is usually amounting more than 91% and 5 approaching a maximum value of 96.5% for sintering temperature of 1150°C. The microstructure was investigated by using Scanning Transmission Electron Microscope (STEM), X-ray diffraction (XRD). Combined with the results obtained from the STEM and XRD, the impact of sintering temperature on the macroscopic and microscopic structure was discussed. The relative dielectric constant ( ) and dielectric loss ( ) of the BMN solid solutions were measured to be 161-200 and (at room temperature and 100Hz-1MHz), respectively. The BMN solid

  1. Microstructural and mechanical characterization of laser deposited advanced materials

    Science.gov (United States)

    Sistla, Harihar Rakshit

    Additive manufacturing in the form of laser deposition is a unique way to manufacture near net shape metallic components from advanced materials. Rapid solidification facilitates the extension of solid solubility, compositional flexibility and decrease in micro-segregation in the melt among other advantages. The current work investigates the employment of laser deposition to fabricate the following: 1. Functionally gradient materials: This allows grading dissimilar materials compositionally to tailor specific properties of both these materials into a single component. Specific compositions of the candidate materials (SS 316, Inconel 625 and Ti64) were blended and deposited to study the brittle intermetallics reported in these systems. 2. High entropy alloys: These are multi- component alloys with equiatomic compositions of 5 or more elements. The ratio of Al to Ni was decreased to observe the transition of solid solution from a BCC to an FCC crystal structure in the AlFeCoCrNi system. 3. Structurally amorphous alloys: Zr-based metallic glasses have been reported to have high glass forming ability. These alloys have been laser deposited so as to rapidly cool them from the melt into an amorphous state. Microstructural analysis and X-ray diffraction were used to study the phase formation, and hardness was measured to estimate the mechanical properties.

  2. Microstructural and Mechanical Characterization of Actively Brazed Alumina Specimens

    Energy Technology Data Exchange (ETDEWEB)

    Hosking, F.M.; Cadden, C.H.; Stephens, J.J.; Glass, S.J.; Yang, N.Y.C.; Vianco, P.V.; Walker, C.A.

    1999-08-26

    Alumina (94 and 99.8% grade compositions) was brazed directly to itself with gold-based active brazing alloys (ABA's) containing vanadium additions of 1,2 and 3 weight percent. The effects of brazing conditions on the joint properties were investigated. Wetting behavior, interfacial reactions, microstructure, hermeticity and tensile strength were determined. Wetting was fair to good for the ABA and base material combinations. Microanalysis identified a discontinuous Al-V-O spinel reaction product at the alumina-braze interface. Tensile strength results for 94% alumina were uniformly good and generally not sensitive to the vanadium concentration, with tensile values of 85-105 MPa. There was more variability in the 99.8% alumina strength results, with values ranging from 25-95 MPa. The highest vanadium concentration (3 wt. %) yielded the highest joint strength for the brazed 99.8% alumina. Failures in the 99.8% alumina samples occurred at the braze-alumina interface, while the 94% alumina specimens exhibited fracture of the ceramic substrate.

  3. Ceramic foams porous microstructure characterization by X-ray microtomography

    Directory of Open Access Journals (Sweden)

    Carlos Roberto Appoloni

    2004-12-01

    Full Text Available Knowledge of the porous structure of amorphous materials is of fundamental importance in calculating geometrical parameters such as total porosity, pore size distribution and physical parameters relating to fluid flow inside void space. The present work deals with the measurement of the microstructural parameters of porous ceramic filters. Microtomographic measurements of samples were taken using an X-ray tube. Bremsstrahlung radiation was filtered in transmission mode with a Sn filter at 58.5 and 28.3 keV and the images analyzed in two ways. The first method consisted in analyzing transepts of the images in order to calculate total porosity based on the average particle size and media linear attenuation coefficients. The second method involved a study of the images using an image analysis software, called Imago, which allows one to calculate total porosity and pore size distribution. The total measured porosity of the filter C90 was 73.8%, 71.1%, 74.4% and 71.5% by, respectively, the Arquimedes method, simple gamma ray transmission, transept analysis and analysis of the microtomographic images at 28.3 keV.

  4. Microstructural Characterization Of Polycrystalline Ice From The East Rongbuk Glacier (Mt. Everest)

    Science.gov (United States)

    Sieg, K. E.; Obbard, R. W.; Baker, I.; Mayewski, P.; Kang, S.; Hou, S.; Kaspari, S.

    2005-12-01

    The microstructural texture and fabric of meteoric glacial ice, collected from the northern slope of Mt. Everest (28°01'N, 86°58'E; elevation 6500 m a.s.l.), is analyzed using a variety of characterization techniques including optical image analysis, scanning electron microscopy, electron dispersive spectroscopy and electron backscatter diffraction. The product of a low latitude mountain environment, this Himalayan ice presents some interesting differences from meteoric glacier ice from polar cores. A comparison between the Mt. Everest ice and that from Antarctica (Vostok) and Greenland (GISP2) illustrates the impact of mean temperature, seasonal differences in aerosol transport, unidirectional flow and state of stress on glacial microstructure. This work forms a benchmark for the further study of temperate zone glacier microstructure, and will help scientists to better interpret ice core records and learn more about atmospheric circulation and anthropogenic climate change.

  5. Generation and Characterization of Anisotropic Microstructures in Rare Earth-Iron-Boron Alloys

    Energy Technology Data Exchange (ETDEWEB)

    Oster, Nathaniel [Iowa State Univ., Ames, IA (United States)

    2012-01-01

    The goal of this work is to investigate methods in which anisotropy could be induced in fine-grained alloys. We have identified two general processing routes to creating a fine, textured microstructure: form an amorphous precursor and devitrify in a manner that induces texture or form the fine, textured microstructure upon cooling directly from the liquid state. Since it is possible to form significant amounts of amorphous material in RE-Fe-B alloys, texture could be induced through biasing the orientationof the crystallites upon crystallization of the amorphous material. One method of creating this bias is to form glassy material and apply uniaxial pressure during crystallization. Experiments on this are presented. All of the work presented here utilizes melt-spinning, either to create precursor material, or to achieve a desired final microstructure. To obtain greater control of the system to process these materials, a study was done on the effects of heating the wheel and modifying the wheel’s surface finish on glass formation and phase selection. The second general approach—creating the desired microstructure directly from the liquid—can be done through directional rapid solidification. In particular, alloys melt-spun at low tangential wheel speeds often display directional columnar growth through a portion of the ribbon. By refining and stabilizing the columnar growth, a highly textured fine microstructure is achieved. The effects of adding a segregating element (Ag) on the columnar growth are characterized and presented.

  6. Characterization of the microstructure of tin-silver lead free solder

    Energy Technology Data Exchange (ETDEWEB)

    Hurtony, Tamás, E-mail: hurtony@ett.bme.hu [Department of Electronics Technology, Budapest University of Technology and Economics, Egry József utca 18, Budapest, H-1111 (Hungary); Szakál, Alex; Almásy, László [Neutron Spectroscopy Department, Wigner Research Centre for Physics, Budapest (Hungary); Len, Adél [Neutron Spectroscopy Department, Wigner Research Centre for Physics, Budapest (Hungary); Faculty of Engineering and Information Technology, University of Pécs (Hungary); Kugler, Sándor [Department of Theoretical Physics, Budapest University of Technology and Economics (Hungary); Bonyár, Attila; Gordon, Péter [Department of Electronics Technology, Budapest University of Technology and Economics, Egry József utca 18, Budapest, H-1111 (Hungary)

    2016-07-05

    Reliability and lifetime are the two most relevant design considerations in the production of safety critical assemblies. For example in a modern automobile dozens of electronic assemblies are integrated in which thousands of solder joints are mounting the electronic components to the printed circuit boards. There exists no standardised and universal observation method for characterising the fine microstructure of such solder joints. Previously we have developed a new method for the quantitative characterization of lead-free solder alloys and in present study the validity of the proposed method is demonstrated. Microstructure of Sn-3.5Ag lead free solder alloy was investigated by electrochemical impedance spectroscopy. Solder samples were solidified with different cooling rates in order to induce differences in the microstructure. Microstructure of the ingots was revealed by selective electrochemical etching. Electrochemical impedance spectra (EIS) were measured before and after the selective etching process. The complex impedance spectra contain information about microstructure of the solder alloys. Comparison and modelling of two EIS spectra allowed obtaining a characteristic parameter of surface structure of the etched specimens. The EIS measurements were complemented with small angle neutron scattering measurements and scanning electron microscopy, in order to correlate the EIS parameter with the magnitude of the interface of the β-Sn and Ag{sub 3}Sn phases.

  7. Process Optimization and Microstructure Characterization of Ti6Al4V Manufactured by Selective Laser Melting

    Science.gov (United States)

    junfeng, Li; zhengying, Wei

    2017-11-01

    Process optimization and microstructure characterization of Ti6Al4V manufactured by selective laser melting (SLM) were investigated in this article. The relative density of sampled fabricated by SLM is influenced by the main process parameters, including laser power, scan speed and hatch distance. The volume energy density (VED) was defined to account for the combined effect of the main process parameters on the relative density. The results shown that the relative density changed with the change of VED and the optimized process interval is 55∼60J/mm3. Furthermore, compared with laser power, scan speed and hatch distance by taguchi method, it was found that the scan speed had the greatest effect on the relative density. Compared with the microstructure of the cross-section of the specimen at different scanning speeds, it was found that the microstructures at different speeds had similar characteristics, all of them were needle-like martensite distributed in the β matrix, but with the increase of scanning speed, the microstructure is finer and the lower scan speed leads to coarsening of the microstructure.

  8. Characterization of PPLN-microstructures by means of Raman spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Hammoum, R.; Fontana, M.D.; Bourson, P. [University Paul Verlaine of Metz and Supelec, Laboratoire Materiaux Optiques, Photonique et Systemes - UMR CNRS 7132, Metz (France); Shur, V.Y. [Ural State University, Ferroelectric Laboratory, Ekaterinburg (Russian Federation)

    2008-04-15

    In this paper we show how the Raman microprobe can be used for characterization of the domain structure in periodically poled lithium niobate (PPLN). The Raman scattered intensity of the transverse and longitudinal optical phonons was recorded across the stripe ferroelectric domains at the surface of a z-cut congruent PPLN sample. The change of integrated intensities across the domain structure was attributed to the influence of mechanical stresses and partially screened depolarization fields. (orig.)

  9. Heating Changes Bio-Schwertmannite Microstructure and Arsenic(III Removal Efficiency

    Directory of Open Access Journals (Sweden)

    Xingxing Qiao

    2017-01-01

    Full Text Available Schwertmannite (Sch is an efficient adsorbent for arsenic(III removal from arsenic(III-contaminated groundwater. In this study, bio-schertmannite was synthesized in the presence of dissolved ferrous ions and Acidithiobacillus ferrooxidans LX5 in a culture media. Bio-synthesized Sch characteristics, such as total organic carbon (TOC, morphology, chemical functional groups, mineral phase, specific surface area, and pore volume were systematically studied after it was dried at 105 °C and then heated at 250–550 °C. Differences in arsenic(III removal efficiency between 105 °C dried-sch and 250–550 °C heated-sch also were investigated. The results showed that total organic carbon content in Sch and Sch weight gradually decreased when temperature increased from 105 °C to 350 °C. Sch partly transformed to another nanocrystalline or amorphous phase above 350 °C. The specific surface area of 250 °C heated-sch was 110.06 m2/g compared to 5.14 m2/g for the 105 °C dried-sch. Total pore volume of 105 °C dried-sch was 0.025 cm3/g with 32.0% mesopore and 68.0% macropore. However, total pore volume of 250 °C heated-mineral was 0.106 cm3/g with 23.6% micropore, 33.0% mesopore, and 43.4% macropore. The arsenic(III removal efficiency from an initial 1 mg/L arsenic(III solution (pH 7.5 was 25.1% when 0.25 g/L of 105 °C dried-sch was used as adsorbent. However, this efficiency increased to 93.0% when using 250 °C heated-sch as adsorbent. Finally, the highest efficiency for arsenic(III removal was obtained with sch-250 °C due to high amounts of sorption sites in agreement with the high specific surface area (SSA obtained for this sample.

  10. Synthesis, Characterization of La(III, Nd(III, and Er(III Complexes with Schiff Bases Derived from Benzopyran-4-one and Thier Fluorescence Study

    Directory of Open Access Journals (Sweden)

    Aida L. El-Ansary

    2012-01-01

    Full Text Available The Schiff bases, L1, L2, and L3, are synthesized from the condensation of 5,7-dihydroxy-6-formyl-2-methylbenzopyran-4-one (L with 2-aminopyridine (1, p-phenylenediamine (2, and o-phenylenediamine (3. The prepared Schiff bases react with lanthanum (III, neodymium (III, and erbium (III nitrate to give complexes with stoichiometric ratio (1 : 1 (ligand : metal. The binuclear complexes of Er(III with L3 and the three metal ions with L2 are separated. The complexes have been characterized by elemental analysis, molar conductance, electronic absorption, and infrared, 1H-NMR spectral studies. The presence of hydrated and coordinated water molecules is inferred from thermogravimetric analysis. Thermal degradation studies show that the final product is the metal oxide. The luminescence properties of the Nd(III and Er(III complexes in dimethylformamide (DMF solutions were investigated.

  11. Microstructural Characterization of Co-Cr-Mo-W Alloy as Casting for Odontological Application

    Directory of Open Access Journals (Sweden)

    Priscila S. N. Mendes

    2017-03-01

    Full Text Available Interest in the analysis and material characterization is rising due to the necessity of the adequate material selection based on system performance in study. The analysis and knowledge of the microstructure and the mechanical properties of any material are of utmost importance since it aims primarily to estimate the performance during the material life span, minimizing the possibility of degradation and undesirable flaws during product utilization. Co-Cr-Mo-W alloys have been well accepted in odontology as prosthesis material, due to its high mechanical resistance, good corrosion resistance and exceptional biocompatibility properties. This study aims to characterize the microstructure of a cobalt based alloy (Co-Cr-Mo-W obtained through vacuum casting process. Optical microscopy, electronic sweeping microscopy and X-ray were employed and Vickers hardness test with loads of 100 gf, 500 gf and 1000 gf during 10 s. Microstructure casting is characterized by a Co-fcc dendritic matrix with a secondary phase, as well as M23C6 precipitate carbides in the interdendritics zones and grain boundaries. The precipitation of carbides represents the main device of strengthening in the cast state for these types of alloys and is also responsible for its lower mechanical properties. The material attained hardness between 25 and 35 HRC, meeting the ASTM F75 standards.

  12. Minor ampullate silks from Nephila and Argiope spiders: tensile properties and microstructural characterization.

    Science.gov (United States)

    Guinea, G V; Elices, M; Plaza, G R; Perea, G B; Daza, R; Riekel, C; Agulló-Rueda, F; Hayashi, C; Zhao, Y; Pérez-Rigueiro, J

    2012-07-09

    The mechanical behavior and microstructure of minor ampullate gland silk (miS) of two orb-web spinning species, Argiope trifasciata and Nephila inaurata, were extensively characterized, enabling detailed comparison with other silks. The similarities and differences exhibited by miS when compared with the intensively studied major ampullate gland silk (MAS) and silkworm (Bombyx mori) silk offer a genuine opportunity for testing some of the hypotheses proposed to correlate microstructure and tensile properties in silk. In this work, we show that miSs of different species show similar properties, even when fibers spun by spiders that diverged over 100 million years are compared. The tensile properties of miS are comparable to those of MAS when tested in air, significantly in terms of work to fracture, but differ considerably when tested in water. In particular, miS does not show a supercontraction effect and an associated ground state. In this regard, the behavior of miS in water is similar to that of B. mori silk, and it is shown that the initial elastic modulus of both fibers can be explained using a common model. Intriguingly, the microstructural parameters measured in miS are comparable to those of MAS and considerably different from those found in B. mori. This fact suggests that some critical microstructural information is still missing in our description of silks, and our results suggest that the hydrophilicity of the lateral groups or the large scale organization of the sequences might be routes worth exploring.

  13. Chairside CAD/CAM materials. Part 1: Measurement of elastic constants and microstructural characterization.

    Science.gov (United States)

    Belli, Renan; Wendler, Michael; de Ligny, Dominique; Cicconi, Maria Rita; Petschelt, Anselm; Peterlik, Herwig; Lohbauer, Ulrich

    2017-01-01

    A deeper understanding of the mechanical behavior of dental restorative materials requires an insight into the materials elastic constants and microstructure. Here we aim to use complementary methodologies to thoroughly characterize chairside CAD/CAM materials and discuss the benefits and limitations of different analytical strategies. Eight commercial CAM/CAM materials, ranging from polycrystalline zirconia (e.max ZirCAD, Ivoclar-Vivadent), reinforced glasses (Vitablocs Mark II, VITA; Empress CAD, Ivoclar-Vivadent) and glass-ceramics (e.max CAD, Ivoclar-Vivadent; Suprinity, VITA; Celtra Duo, Dentsply) to hybrid materials (Enamic, VITA; Lava Ultimate, 3M ESPE) have been selected. Elastic constants were evaluated using three methods: Resonant Ultrasound Spectroscopy (RUS), Resonant Beam Technique (RBT) and Ultrasonic Pulse-Echo (PE). The microstructures were characterized using Scanning Electron Microscopy (SEM), Energy Dispersive X-ray Spectroscopy (EDX), Raman Spectroscopy and X-ray Diffraction (XRD). Young's modulus (E), Shear modulus (G), Bulk modulus (B) and Poisson's ratio (ν) were obtained for each material. E and ν reached values ranging from 10.9 (Lava Ultimate) to 201.4 (e.max ZirCAD) and 0.173 (Empress CAD) to 0.47 (Lava Ultimate), respectively. RUS showed to be the most complex and reliable method, while the PE method the easiest to perform but most unreliable. All dynamic methods have shown limitations in measuring the elastic constants of materials showing high damping behavior (hybrid materials). SEM images, Raman spectra and XRD patterns were made available for each material, showing to be complementary tools in the characterization of their crystal phases. Here different methodologies are compared for the measurement of elastic constants and microstructural characterization of CAD/CAM restorative materials. The elastic properties and crystal phases of eight materials are herein fully characterized. Copyright © 2016 The Academy of Dental Materials

  14. Characterization of Microstructure and Mechanical Properties of Resistance Spot Welded DP600 Steel

    Directory of Open Access Journals (Sweden)

    Ali Ramazani

    2015-09-01

    Full Text Available Resistance spot welding (RSW as a predominant welding technique used for joining steels in automotive applications needs to be studied carefully in order to improve the mechanical properties of the spot welds. The objectives of the present work are to characterize the resistance spot weldment of DP600 sheet steels. The mechanical properties of the welded joints were evaluated using tensile-shear and cross-tensile tests. The time-temperature evolution during the welding cycle was measured. The microstructures observed in different sites of the welds were correlated to thermal history recorded by thermocouples in the corresponding areas. It was found that cracks initiated in the periphery region of weld nuggets with a martensitic microstructure and a pull-out failure mode was observed. It was also concluded that tempering during RSW was the main reason for hardness decrease in HAZ.

  15. TEM characterization of microstructure evolution of 12%Cr heat resistant steels

    Energy Technology Data Exchange (ETDEWEB)

    Rojas, D.; Prat, O.; Sauthoff, G. [Max-Planck-Institut fuer Eisenforschung GmbH, Duesseldorf (Germany); Garcia, J. [Helmholtz-Zentrum Berlin fuer Materialien und Energie GmbH, Berlin (Germany); Kaysser-Pyzalla, A.R. [Helmholtz-Zentrum Berlin fuer Materialien und Energie GmbH, Berlin (Germany); Bochum Univ. (Germany)

    2010-07-01

    A detailed characterization of the microstructure evolution of 12%Cr heat resistant steels at different creep times (100 MPa / 650 C / 8000 h) were carried out by scanning transmission electron microscopy (STEM). The results of the microstructure analysis are correlated with the mechanical properties in order to investigate the influence of different precipitates (especially M{sub 23}C{sub 6}) on the creep strength of the alloys. Precipitation of Laves phase and Z-phase was observed after several hours creep time. Very few Z-phase of the type Cr(V,Ta)N nucleating from existing (V,Ta)(C,N) was observed. Both alloys show growth and coarsening of Laves phase, meanwhile the MX carbonitrides present a very slow growth and coarsening rate. Alloys containing Laves phase, MX and M{sub 23}C{sub 6} precipitates show best creep properties. (orig.)

  16. Design and characterization of microstructure evolution during creep of 12% Cr heat resistant steels

    Energy Technology Data Exchange (ETDEWEB)

    Rojas, D. [Max Planck Institute fuer Eisenforschung GmbH, Max Planck Str. 1, 40237 Duesseldorf (Germany); Garcia, J., E-mail: jose.garcia@helmholtz-berlin.de [Helmholtz-Zentrum Berlin fuer Materialien und Energie GmbH, Hahn-Meitner-Platz 1, 14109 Berlin (Germany); Prat, O. [Max Planck Institute fuer Eisenforschung GmbH, Max Planck Str. 1, 40237 Duesseldorf (Germany); Carrasco, C. [Universidad de Concepcion, Departamento de Ingenieria de Materiales, Edmundo Larenas 270, Concepcion (Chile); Sauthoff, G. [Max Planck Institute fuer Eisenforschung GmbH, Max Planck Str. 1, 40237 Duesseldorf (Germany); Kaysser-Pyzalla, A.R. [Helmholtz-Zentrum Berlin fuer Materialien und Energie GmbH, Hahn-Meitner-Platz 1, 14109 Berlin (Germany); Ruhr Universitaet Bochum, Universitaetstr. 150 IA2, 44780 Bochum (Germany)

    2010-06-25

    12% Cr heat resistant steels with a fine dispersion of nano precipitates were designed supported by thermodynamic modeling. A detailed characterization of the microstructure evolution at different creep times (100 MPa/650 deg. C/8000 h) was carried out by scanning transmission electron microscopy (STEM). The results of the microstructure analysis are correlated with the mechanical properties in order to investigate the influence of different precipitates (especially M{sub 23}C{sub 6}) on the creep strength of the alloys. Precipitation of Laves phase and Z-phase was observed after several hours creep time. Very few Z-phase of the type Cr(V,Ta)N nucleating from existing (V,Ta)(C,N) was observed. Both alloys show growth and coarsening of Laves phase, meanwhile the MX carbonitrides present a very slow growth and coarsening rate. Alloys containing Laves phase, MX and M{sub 23}C{sub 6} precipitates show best creep properties.

  17. Characterization of Nickel Diffusion and its Effect on the Microstructure of Nickel PM Steels

    Science.gov (United States)

    Tougas, Bernard; Blais, Carl; Chagnon, François; Pelletier, Sylvain

    2013-02-01

    Admixing pure elements to powder mixes can cause the formation of heterogeneous microstructures in sintered parts. For instance, nickel is renowned for forming nickel-rich areas (NRA) in powder metallurgy (PM) nickel steels due to its poor diffusivity in iron matrix (or lattice). The present work is aimed at characterizing the principal diffusion mechanisms of nickel and their influence on microstructures and properties of PM nickel steels. A new wavelength dispersive X-ray spectrometry (WDS) approach linking line scans and X-ray maps to concentration maps is proposed. Grain boundary and volume diffusion coefficients of admixed nickel have been determined in PM nickel steels using Suzuoka's equation. Results also show that nickel distributes itself in the iron matrix mainly by surface and grain boundary diffusion.

  18. A new characterization approach for studying relationships between microstructure and creep damage mechanisms of uranium dioxide

    Energy Technology Data Exchange (ETDEWEB)

    Iltis, X., E-mail: xaviere.iltis@cea.fr [CEA, DEN, DEC, Cadarache, 13108 Saint-Paul-Lez-Durance (France); Ben Saada, M. [CEA, DEN, DEC, Cadarache, 13108 Saint-Paul-Lez-Durance (France); Laboratoire d' Etudes des Microstructures et de Mécanique des Matériaux (LEM3), CNRS UMR 7239, Université de Lorraine, Ile du Saulcy, 57045 Metz Cedex 1 (France); Mansour, H.; Gey, N.; Hazotte, A.; Maloufi, N. [Laboratoire d' Etudes des Microstructures et de Mécanique des Matériaux (LEM3), CNRS UMR 7239, Université de Lorraine, Ile du Saulcy, 57045 Metz Cedex 1 (France)

    2016-06-15

    Four batches of UO{sub 2} pellets were studied comparatively, before and after creep tests, to evaluate a characterization methodology aimed to determine the links between microstructure and damage mechanisms induced by compressive creep of uranium dioxide at 1500 °C. They were observed by means of scanning electron microscopy (SEM) coupled with image analysis, to quantify their fabrication porosity and the occurrence of inter-granular cavities after creep, and electron back scattered diffraction (EBSD), especially to characterize sub-structures development associated with plastic deformation. Electron channeling contrast imaging (ECCI) was also applied to evidence dislocations, at an exploratory stage, on one of the deformed pellets. This approach helped to identify and quantify microstructural differences between batches. Their as-fabricated microstructures differed in terms of grain size and fabrication porosity distribution. The pellets which had the lowest strain rates were those with the largest number of intra-granular pores, regardless of their grain size. They also exhibited less numerous sub-boundaries within the grains. These first results clearly illustrate the benefit of systematic examinations of crept UO{sub 2} pellets at a mesoscopic scale, by SEM and EBSD, to study their deformation process. In addition, ECCI appears as a powerful tool to evidence local dislocations arrangements, in bulk samples. Even if the sampling was limited, the results of this study also tend to indicate that the intra-granular pores population, resulting from the manufacturing of the samples by powder metallurgy, could have a significant influence on the UO{sub 2} viscoplastic deformation mechanisms. - Highlights: • Four different UO{sub 2} pellets batches are microstructurally compared, before and after compression creep tests. • Development of sub-boundaries within the original grains, in crept samples, is quantified by EBSD. • Links are observed between the intra

  19. TEM Characterization of High Burn-up Microstructure of U-7Mo Alloy

    Energy Technology Data Exchange (ETDEWEB)

    Jian Gan; Brandon Miller; Dennis Keiser; Adam Robinson; James Madden; Pavel Medvedev; Daniel Wachs

    2014-04-01

    As an essential part of global nuclear non-proliferation effort, the RERTR program is developing low enriched U-Mo fuels (< 20% U-235) for use in research and test reactors that currently employ highly enriched uranium fuels. One type of fuel being developed is a dispersion fuel plate comprised of U-7Mo particles dispersed in Al alloy matrix. Recent TEM characterizations of the ATR irradiated U-7Mo dispersion fuel plates include the samples with a local fission densities of 4.5, 5.2, 5.6 and 6.3 E+21 fissions/cm3 and irradiation temperatures of 101-136?C. The development of the irradiated microstructure of the U-7Mo fuel particles consists of fission gas bubble superlattice, large gas bubbles, solid fission product precipitates and their association to the large gas bubbles, grain subdivision to tens or hundreds of nanometer size, collapse of bubble superlattice, and amorphisation. This presentation will describe the observed microstructures specifically focusing on the U-7Mo fuel particles. The impact of the observed microstructure on the fuel performance and the comparison of the relevant features with that of the high burn-up UO2 fuels will be discussed.

  20. Cloning and functional characterization of a class III chitinase gene ...

    African Journals Online (AJOL)

    Analysis of the VvChiF III amino acid sequence showed that this gene corresponds to the Glyco-hydro-18 super family that consisting of a signal peptide with the length of 25 amino acids. Purified VvChiF III showed chitinase activity toward the soluble substrate, glycolchitin and antifungal activity against Botrytis cinerea.

  1. Human milk fat globules from different stages of lactation: a lipid composition analysis and microstructure characterization.

    Science.gov (United States)

    Zou, Xiao-Qiang; Guo, Zheng; Huang, Jian-Hua; Jin, Qing-Zhe; Cheong, Ling-Zhi; Wang, Xing-Guo; Xu, Xue-Bing

    2012-07-25

    The physicochemical properties of human milk fat globules (MFG) at different lactation stages from Danish mothers and the microstructure changes of MFG membrane (MFGM) at varied temperatures were investigated, and the relationship between chemical composition and the microstructure of MFGM was elucidated. The fat content in MFG was found to be significantly increased as lactation progressed, and colostrum MFG had the largest mean diameter of 5.75 ± 0.81 μm and the lowest ζ potential of -5.60 ± 0.12 mV. Chemical composition analyses of MFG revealed the following: (i) Colostrum milk fat constituted higher content in PUFAs (ω-6, and long-chain ω-6 and ω-3) than transitional and mature milk fats, with the corresponding lower content of SFA in its sn-2 position. (ii) The content of polar lipids among total lipids varied during lactation course (maximized at transitional stage); however, in terms of subclasses of polar lipids, no significant change of the relative content of sphingomyelin was observed, while the content of phosphatidycholine in mature milk was higher than that in colostrum and transitional milk. (iii) Inspection of fatty acid composition in phospholipids from different lactation milk revealed no remarkable and regular changes could be generalized; and no obvious difference of the morphologies of MFGM at different lactation stages can be visualized. An investigation of the microstructure change of MFGM vs temperature demonstrated that the segregated domains became larger as temperature decreased to 4 °C, while it became smaller when increased to 37 °C. This phenomenon indicated that, in addition to sphingimyelin and cholesterol, phospholipids might also contribute to increasing the segregated domains at lower temperature, while, at elevated temperature, these domains could be diminished, most likely due to a restructuring or distributing of sphingimyelin and cholesterol.

  2. MICROSTRUCTURAL CHARACTERIZATION AND PHOTOCATALYTIC ACTIVITY OF ZINC OXIDE NANOSTRUCTURED SYNTHESIZED BY COMBUSTION IN SOLUTION

    Directory of Open Access Journals (Sweden)

    Waleska Campos Guaglianoni

    2015-06-01

    Full Text Available Nanostructured zinc oxide (ZnO was obtained by combustion synthesis in solution using zinc nitrate and citric acid. Morphology, weight loss, phase transformation and crystallite size were characterized scanning electron microscopy (SEM, thermal gravimetric (TGA and thermal differential (DTA analysis, and X-ray diffraction (XRD. The photocatalytic activity was evaluated by the degradation of a solution of methyl orange. We investigated the influence of different fuel/oxidant molar ratios in the microstructure and in the photocatalytic activity of ZnO. The results showed a higher crystallinity and photocatalytic performance for the products obtained with disabilities fuel in the reaction.

  3. Growth and structural characterization of III-V semiconductor nanowires

    OpenAIRE

    Rieger, Torsten

    2015-01-01

    In this thesis, the growth and structural properties of III-V semiconductor nanowires and nanowire heterostructures are studied. These nanowires represent structures suitable for both fundamental physics and applications in electronic devices such as (tunnel) field effect transistors. The III-V nanowires are grown with molecular beam epitaxy, high κ dielectric layers are deposited conformally around the nanowires by atomic layer deposition. The morphological and structural characteristics of ...

  4. A new characterization approach for studying relationships between microstructure and creep damage mechanisms of uranium dioxide

    Science.gov (United States)

    Iltis, X.; Ben Saada, M.; Mansour, H.; Gey, N.; Hazotte, A.; Maloufi, N.

    2016-06-01

    Four batches of UO2 pellets were studied comparatively, before and after creep tests, to evaluate a characterization methodology aimed to determine the links between microstructure and damage mechanisms induced by compressive creep of uranium dioxide at 1500 °C. They were observed by means of scanning electron microscopy (SEM) coupled with image analysis, to quantify their fabrication porosity and the occurrence of inter-granular cavities after creep, and electron back scattered diffraction (EBSD), especially to characterize sub-structures development associated with plastic deformation. Electron channeling contrast imaging (ECCI) was also applied to evidence dislocations, at an exploratory stage, on one of the deformed pellets. This approach helped to identify and quantify microstructural differences between batches. Their as-fabricated microstructures differed in terms of grain size and fabrication porosity distribution. The pellets which had the lowest strain rates were those with the largest number of intra-granular pores, regardless of their grain size. They also exhibited less numerous sub-boundaries within the grains. These first results clearly illustrate the benefit of systematic examinations of crept UO2 pellets at a mesoscopic scale, by SEM and EBSD, to study their deformation process. In addition, ECCI appears as a powerful tool to evidence local dislocations arrangements, in bulk samples. Even if the sampling was limited, the results of this study also tend to indicate that the intra-granular pores population, resulting from the manufacturing of the samples by powder metallurgy, could have a significant influence on the UO2 viscoplastic deformation mechanisms.

  5. Microstructure Characterization of Fiber Laser Welds of S690QL High-Strength Steels

    Science.gov (United States)

    Li, Baoming; Xu, Peiquan; Lu, Fenggui; Gong, Hongying; Cui, Haichao; Liu, Chuangen

    2018-02-01

    The use of fiber laser welding to join S690QL steels has attracted interest in the field of construction and assembly. Herein, 13-mm-thick S690QL welded joints were obtained without filler materials using the fiber laser. The as-welded microstructures and the impact energies of the joints were characterized and measured using electron microscopy in conjunction with high-resolution transmission electron images, X-ray diffraction, and impact tests. The results indicated that a single-sided welding technique could be used to join S690QL steels up to a thickness of 12 mm (fail to fuse the joint in the root) when the laser power is equal to 12 kW (scan speed 1 m/min). Double-side welding technique allows better weld penetration and better control of heat distribution. Observation of the samples showed that the fusion zone exhibited bainitic and martensitic microstructures with increased amounts of martensites (Ms) compared with the base materials. Also, the grains in the fusion zone increased in coarseness as the heat input was increased. The fusion zone exhibited increased hardness (397 HV0.2) while exhibiting a simultaneous decrease in the impact toughness. The maximum impact energy value of 26 J was obtained from the single-side-welded sample, which is greater than those obtained from the double-side-welded samples (maximum of 18 J). Many more dislocations and plastic deformations were found in the fusion zone than the heat-affected zone in the joint, which hardened the joints and lowered the impact toughness. The microstructures characterized by FTEM-energy-dispersive X-ray spectrometer also exhibited laths of M, as well as stacking faults and dislocations featuring high-density, interfacial structure ledges that occur between the high-angle grain boundaries and the M and bainite.

  6. Microstructure characterization of LAE442 magnesium alloy processed by extrusion and ECAP

    Energy Technology Data Exchange (ETDEWEB)

    Minárik, Peter; Král, Robert; Pešička, Josef [Charles University, Department of Physics of Materials, Prague (Czech Republic); Daniš, Stanislav [Charles University, Department Condensed Matter Physics, Prague (Czech Republic); Janeček, Miloš, E-mail: janecek@met.mff.cuni.cz [Charles University, Department of Physics of Materials, Prague (Czech Republic)

    2016-02-15

    The magnesium alloy LAE442 was processed by extrusion and equal channel angular pressing (ECAP) to achieve ultrafine grained microstructure. Detailed characterization of the microstructure was performed by scanning electron microscope, electron back scattered diffraction (EBSD) and transmission electron microscope. The initial, as-cast, microstructure consisted of large grains of ~ 1 mm. The grain refinement due to the processing by severe plastic deformation led to a decrease of the average grain size to ~ 1.7 μm after the final step of ECAP. A detailed characterization of secondary phases showed the precipitation of Al{sub 11}RE{sub 3}, Al{sub 2}Ca and Al{sub 10}RE{sub 2}Mn{sub 7} intermetallic phases. X-ray diffraction measurements proved that Li is dissolved within the magnesium matrix in the as-cast condition. Newly formed Al{sub 3}Li phase was observed after ECAP. The texture formation due to the extrusion and ECAP was different from that in the other magnesium alloys due to the activation of non-basal slip systems as a result of the decrease of the c/a ratio. - Highlights: • Combined extrusion and equal channel angular pressing results in significant grain refinement by factor 1000 approximately. • Al{sub 11}RE{sub 3}, Al{sub 2}Ca and Al{sub 10}RE{sub 2}Mn{sub 7} secondary phases are present in the as-cast material while Li was dissolved in the Mg matrix. • Extrusion and ECAP have no effect on the composition of the secondary phases but they influence strongly their distribution. • Texture evolution is affected by decrease of c/a ratio due to the presence of Li and resulting activation of non-basal slip.

  7. Electrodeposition of Ni-W Alloy and Characterization of Microstructure and Properties of the Deposits

    DEFF Research Database (Denmark)

    Mizushima, Io

    2007-01-01

    The subject of this thesis is an electrodeposition of Ni-W alloy and characterization of microstructure and properties of the deposits. In Chapter 3 background such as theoretical comments and literature reviews which provided suggestions for the way to tackle this subject, is described. The expe......The subject of this thesis is an electrodeposition of Ni-W alloy and characterization of microstructure and properties of the deposits. In Chapter 3 background such as theoretical comments and literature reviews which provided suggestions for the way to tackle this subject, is described......-section observation with focused ion beam microscopy, compositional analysis with glow discharge optical emission spectroscopy and line broadening analysis of X-ray diffraction etc are given in Chapter 3. In Chapter 4 the effect of the complexing agents citrate, glycine and triethanolamine (TEA......) on the electrodeposition of Ni-W layers from electrolytes based on NiSO4 and Na2WO4, is investigated. High W content and current efficiency could be realized by using electrolytes containing all of the three complexing agents. The results show that small amounts of glycine in a citrate-triethanolamine based electrolyte...

  8. Multi-scale microstructural characterization of micro-textured Ti-6Al-4V surfaces

    Energy Technology Data Exchange (ETDEWEB)

    Soboyejo, W.O.; Mercer, C.; Allameh, S.; Nemetski, B. [Princeton Materials Inst., NJ (United States). Dept. of Mechanical and Aerospace Engineering; Marcantonio, N. [Brown Univ., Providence, RI (United States). Div. of Engineering; Ricci, J.L. [Univ. of Medicine and Dentistry of New Jersey, Newark, NJ (United States). Dept. of Orthodontics

    2001-07-01

    This paper presents the results of a multi-scale microstructural characterization of micro-textured Ti-6Al-4V surfaces that are used in biomedical implants. The hierarchies of substructural and microstructural features associated with laser micro-texturing, mechanical polishing and surface blasting with alumina pellets are elucidated via atomic force microscopy (AFM), transmission electron microscopy (TEM), scanning electron microscopy (SEM) and optical microscopy (OM). The nano-scale roughness profiles for the different surface textures are characterized via AFM. Sub-micron precipitates and dislocation substructures associated with wrought processing and laser processing are revealed by TEM. OM and SEM micro- and mesoscale images of the groove structures and then described before discussing the implications of the result for the optimization of laser processing schemes. The implications of the results are examined for the fabrication of micro-textured surfaces that will facilitate the self organization of proteins, and the attachment of mammalian cells to the Ti-6Al-4V surfaces in biomedical implants. (orig.)

  9. Mechanical and microstructural characterization of geopolymer synthesized from low calcium fly ash

    Directory of Open Access Journals (Sweden)

    Kramar Sabina

    2015-01-01

    Full Text Available This study deals with the mechanical and microstructural characterization of geopolymers synthesized from locally available fly ash. A low calcium fly ash was activated using a sodium silicate solution. Samples were characterized by means of flexural and compressive tests, Fourier Transform Infrared (FTIR spectroscopy, X-ray powder diffraction (XRD, and scanning electron microscopy (SEM. Porosity and pore size distributions were identified using mercury intrusion porosimetry and gas sorption. The compressive strength of the produced geopolymers, which is in the range of 1.6 to 53.3 N/mm2, is strongly related to the water content as well as SiO2/Na2O mass ratio of an alkali activator. The compressive strength significantly increased with decreases in the water content and increased silicon concentration used for the synthesis of geopolymers.

  10. Synthesis and characterization of a novel (glycinato-N,O) yttrium(III) complex (SHORT COMMUNICATION)

    OpenAIRE

    S. R. NIKETIC; I. M. HODZIC

    2001-01-01

    A novel yttrium(III) complex with glycine has been synthesized starting from tris(ethanedioato-O,O)yttrium(III) by the substitution of the acetylacetonato chelate ligands with glycine. The reaction product was purified by ion-exchange chromatography and characterized on the basis of infrared spectroscopy. The structure of the product was tentatively established as tris(glycinato-N,O)yttrium(III) dihydrate.

  11. Synthesis and characterization of a novel (glycinato-N,O yttrium(III complex (SHORT COMMUNICATION

    Directory of Open Access Journals (Sweden)

    S. R. NIKETIC

    2001-05-01

    Full Text Available A novel yttrium(III complex with glycine has been synthesized starting from tris(ethanedioato-O,Oyttrium(III by the substitution of the acetylacetonato chelate ligands with glycine. The reaction product was purified by ion-exchange chromatography and characterized on the basis of infrared spectroscopy. The structure of the product was tentatively established as tris(glycinato-N,Oyttrium(III dihydrate.

  12. spectral characterization and dna binding properties of lanthanide(iii)

    African Journals Online (AJOL)

    complexes exhibit characteristic patterns of paramagnetic component. The positive slope of the curve clearly indicates paramagnetic nature of the complexes [32]. The lanthanum(III) complex,. [La(APINH)2(NO3)](NO3)2 is diamagnetic and other tripositive lanthanide complexes are paramagnetic. The observed magnetic ...

  13. Ferroelectric KNNT Fibers by Thermoplastic Extrusion Process: Microstructure and Electromechanical Characterization

    Directory of Open Access Journals (Sweden)

    Tony Lusiola

    2015-05-01

    Full Text Available B-site substitution in KNN with tantalum results in a higher d33 and dielectric constant. This higher value makes KNNT interesting for lead-free actuator applications. KNNT fibers with diameters of 300 and 500 μm have been extruded and sintered at 1200 °C in a KNNT-enriched atmosphere. Subsequently, the influence of fiber diameter on the microstructure (porosity and grain size was investigated. The measurements revealed that with decreasing fiber diameter, the porosity increases, whereas the grain size decreases. The influence of these microstructural differences on the piezoelectric properties was evaluated using a novel characterization procedure for single fibers. The larger diameter fibers show an increase in the electromechanical properties measured, i.e., d33, tanδ, Pr, Ec and the free longitudinal fiber displacement, when compared to smaller diameter fibers. The lower alkali losses result in a larger grain size, a higher density during sintering and lead to higher electromechanical properties.

  14. Microstructural characterization of radio frequency and direct current plasma-sprayed Al2O3 coatings

    Science.gov (United States)

    Chen, H. C.; Pfender, E.; Dzur, B.; Nutsch, G.

    2000-06-01

    Microstructures of radio frequency (RF) and direct current (DC) plasma-sprayed Al2O3 coatings deposited onto steel substrates were characterized using scanning electron microscopy (SEM), X-ray diffraction (XRD), electron microprobe analysis (EMPA), polarizing optical microscopy (OM), and transmission electron microscopy (TEM). Because RF and DC plasmas produce different particle heating and acceleration, the morphology, phase structure, and fracture modes of the coatings vary substantially. In the case of RF coatings, a clear lamellar microstructure with relatively thick lamellae was observed, which is due to the large particles and the low particle velocities, with α-Al2O3 as the predominant phase and with delamination type of fracture detected on the fracture surface. In contrast, the DC coatings consisted of predominantly metastable γ-Al2O3 as well as amorphous phases, with a mixed fracture mode of the coating observed. In spite of limited interfacial interdiffusion detected by EMPA, TEM showed an interfacial layer existing at the interface between the coating and the substrate for both cases. For RF coatings, the interfacial layer on the order of 1 µm was composed of three sublayers, each of which was different in composition and morphology. However, the interfacial layer for the DC coating consisted primarily of an amorphous phase, containing both coating and substrate materials with or without platelike microcrystals; although in some regions a thick amorphous Al2O3 layer was in direct contact with the substrate.

  15. Two-Photon Polymerization Metrology: Characterization Methods of Mechanisms and Microstructures

    Directory of Open Access Journals (Sweden)

    Christopher N. LaFratta

    2017-03-01

    Full Text Available The ability to create complex three-dimensional microstructures has reached an unprecedented level of sophistication in the last 15 years. For the most part, this is the result of a steady development of the additive manufacturing technique named two-photon polymerization (TPP. In a short amount of time, TPP has gone from being a microfabrication novelty employed largely by laser specialists to a useful tool in the hands of scientists and engineers working in a wide range of research fields including microfluidics. When used in combination with traditional microfabrication processes, TPP can be employed to add unique three-dimensional components to planar platforms, thus enabling the realization of lab-on-a-chip solutions otherwise impossible to create. To take full advantage of TPP, an in-depth understanding is required of the materials photochemistry and the fabricated microstructures’ mechanical and chemical properties. Thus, we review methods developed so far to investigate the underling mechanism involved during TPP and analytical methods employed to characterize TPP microstructures. Furthermore, we will discuss potential opportunities for using optofluidics and lab-on-a-chip systems for TPP metrology.

  16. Microstructural and mechanical characterization of Cu-0.8 wt.%Y

    Energy Technology Data Exchange (ETDEWEB)

    Carro, G., E-mail: gcarro@fis.uc3m.es; Muñoz, A.; Monge, M.A.; Savoini, B.; Pareja, R.

    2015-10-15

    Dispersion strengthened Cu-0.8 wt.%Y has been produced by a powder metallurgy route and subsequent consolidation by hot isostatic pressing at 1123 K and 172 MPa. A fully dense alloy has been obtained that exhibits a microstructure characterized by equiaxed grains with sizes ranging from 0.5 to 50 μm. Yttrium-rich particles with an average size of 0.92 μm have been observed inside the grains and decorating the grain boundaries. As expected, the tensile tests carried out from room temperature to 773 K have revealed that both the YS and the UTS decrease with increasing temperature. This alloy exhibits better tensile properties and microhardness than OFHC Cu. This improvement is attributed to the presence of the Y-rich particles.

  17. Mineralogical, Microstructural and Thermal Characterization of Coal Fly Ash Produced from Kazakhstani Power Plants

    Science.gov (United States)

    Tauanov, Z.; Abylgazina, L.; Spitas, C.; Itskos, G.; Inglezakis, V.

    2017-09-01

    Coal fly ash (CFA) is a waste by-product of coal combustion. Kazakhstan has vast coal deposits and is major consumer of coal and hence produces huge amounts of CFA annually. The government aims to recycle and effectively utilize this waste by-product. Thus, a detailed study of the physical and chemical properties of material is required as the data available in literature is either outdated or not applicable for recently produced CFA samples. The full mineralogical, microstructural and thermal characterization of three types of coal fly ash (CFA) produced in two large Kazakhstani power plants is reported in this work. The properties of CFAs were compared between samples as well as with published values.

  18. Experimental Characterization and Simulation of Slip Transfer at Grain Boundaries and Microstructurally-Sensitive Crack Propagation

    Science.gov (United States)

    Gupta, Vipul; Hochhalter, Jacob; Yamakov, Vesselin; Scott, Willard; Spear, Ashley; Smith, Stephen; Glaessgen, Edward

    2013-01-01

    A systematic study of crack tip interaction with grain boundaries is critical for improvement of multiscale modeling of microstructurally-sensitive fatigue crack propagation and for the computationally-assisted design of more durable materials. In this study, single, bi- and large-grain multi-crystal specimens of an aluminum-copper alloy are fabricated, characterized using electron backscattered diffraction (EBSD), and deformed under tensile loading and nano-indentation. 2D image correlation (IC) in an environmental scanning electron microscope (ESEM) is used to measure displacements near crack tips, grain boundaries and within grain interiors. The role of grain boundaries on slip transfer is examined using nano-indentation in combination with high-resolution EBSD. The use of detailed IC and EBSD-based experiments are discussed as they relate to crystal-plasticity finite element (CPFE) model calibration and validation.

  19. Production and Characterization of Polycarbonate Microstructured Polymer Optical Fiber Bragg Grating Sensor

    DEFF Research Database (Denmark)

    Fasano, Andrea; Woyessa, Getinet; Stajanca, P.

    2015-01-01

    and strain sensing. The PC optical fibers are for some applications an attractive alternative to conventional materials used in POF fabrication, such as polymethyl methacrylate (PMMA). In general, PC can be used at temperature up to 120 °C and breaks at considerably higher strains than PMMA.......We present the fabrication and characterization of a polycarbonate (PC) microstructured polymer optical fiber (mPOF) and the writing of a fiber Bragg grating (FBG) in it to obtain a polymer optical FBG sen-sor. The manufacturing process of the PC mPOF consists of multiple consecutive stages......, such as casting of pol-ymer granulates into a solid rod, machining and drilling of a 3-ring hexagonal lattice of holes into it, and finally drawing into fiber. We demonstrate that the obtained PC mPOF is photosensitive and FBGs can be conveniently inscribed into it, thereby enabling FBG-based temperature...

  20. Microstructural and mechanical property characterization of ingot metallurgy ODS iron aluminide

    Energy Technology Data Exchange (ETDEWEB)

    Sikka, V.K.; Howell, C.R. [Oak Ridge National Lab., TN (United States); Hall, F.; Valykeo, J. [Hoskins Mfg. Co., Hamburg, MI (United States)

    1997-12-01

    This paper deals with a novel, lower cost method of producing a oxide dispersion strengthened (ODS) iron-aluminide alloy. A large 250-kg batch of ODS iron-aluminide alloy designated as FAS was produced by Hoskins Manufacturing Company (Hoskins) [Hamburg, Michigan] using the new process. Plate and bar stock of the ODS alloy were the two major products received. Each of the products was characterized for its microstructure, including grain size and uniformity of oxide dispersion. Tensile tests were completed from room temperature to 1100 C. Only 100-h creep tests were completed at 800 and 1000 C. The results of these tests are compared with the commercial ODS alloy designated as MA-956. An assessment of these data is used to develop future plans for additional work and identifying applications.

  1. Microstructural Characterization of a Prototype Titanium Alloy Structure Processed via Direct Laser Deposition (DLD)

    Science.gov (United States)

    Clark, Daniel; Whittaker, Mark T.; Bache, Martin R.

    2012-04-01

    Processing trials have produced a three-dimensional, thin-walled structure of representative aerospace component geometry, fabricated directly by laser melting of Ti 6Al4V powder. This additive-built form has been subjected to metallographic characterization. The fabrication technique is evaluated as an economic, commercial process that can add features such as bosses or flanges as a hybrid-manufacturing route for existing forms of gas turbine components. The samples were extracted from six locations with different wall thickness, varying forms, and intersecting ligament geometries. A fine-scale Widmanstätten colony microstructure was consistent throughout the structure within grains elongated parallel to the axis of epitaxy. Evidence of limited grain boundary α was detected; however, this was never continuous around individual grains. A moderate Burgers texture was measured employing electron backscatter diffraction (EBSD), which is consistent with the melt/cast titanium alloy forms cooling through the β transus.

  2. An Integrated Approach Linking Process to Structural Modeling With Microstructural Characterization for Injections-Molded Long-Fiber Thermoplastics

    Energy Technology Data Exchange (ETDEWEB)

    Nguyen, Ba Nghiep; Bapanapalli, Satish K.; Smith, Mark T.; Kunc, Vlastimil; Frame, Barbara; Norris, Robert E.; Phelps, Jay; Tucker III, Charles L.; Jin, Xiaoshi; Wang, Jin

    2008-09-01

    The objective of our work is to enable the optimum design of lightweight automotive structural components using injection-molded long fiber thermoplastics (LFTs). To this end, an integrated approach that links process modeling to structural analysis with experimental microstructural characterization and validation is developed. First, process models for LFTs are developed and implemented into processing codes (e.g. ORIENT, Moldflow) to predict the microstructure of the as-formed composite (i.e. fiber length and orientation distributions). In parallel, characterization and testing methods are developed to obtain necessary microstructural data to validate process modeling predictions. Second, the predicted LFT composite microstructure is imported into a structural finite element analysis by ABAQUS to determine the response of the as-formed composite to given boundary conditions. At this stage, constitutive models accounting for the composite microstructure are developed to predict various types of behaviors (i.e. thermoelastic, viscoelastic, elastic-plastic, damage, fatigue, and impact) of LFTs. Experimental methods are also developed to determine material parameters and to validate constitutive models. Such a process-linked-structural modeling approach allows an LFT composite structure to be designed with confidence through numerical simulations. Some recent results of our collaborative research will be illustrated to show the usefulness and applications of this integrated approach.

  3. 3D microstructural characterization of nickel superalloys via serial-sectioning using a dual beam FIB-SEM

    Energy Technology Data Exchange (ETDEWEB)

    Uchic, Michael D. [Air Force Research Laboratory, Materials and Manufacturing Directorate, Wright-Patterson AFB, OH 45433 (United States)]. E-mail: michael.uchic@wpafb.af.mil; Groeber, Michael A. [Ohio State University, Department of Materials Science and Engineering, Columbus, OH 43210 (United States); Dimiduk, Dennis M. [Air Force Research Laboratory, Materials and Manufacturing Directorate, Wright-Patterson AFB, OH 45433 (United States); Simmons, J.P. [Air Force Research Laboratory, Materials and Manufacturing Directorate, Wright-Patterson AFB, OH 45433 (United States)

    2006-07-15

    Dual beam focused ion beam-scanning electron microscopes are well suited for characterizing micron and sub-micron size microstructural features in three dimensions via serial-sectioning procedures. Importantly, these commally-available instruments can be used to collect morphological, crystallographic, and chemical information throughout a serial-sectioning experiment. Selected examples are shown to demonstrate these capabilities.

  4. Characterization of the 3-dimensional microstructure of a graphite negative electrode from a Li-ion battery

    DEFF Research Database (Denmark)

    Shearing, P.R.; Howard, L.E.; Jørgensen, Peter Stanley

    2010-01-01

    The 3-dimensional microstructure of a porous electrode from a lithium-ion battery has been characterized for the first time. We use X-ray tomography to reconstruct a 43 × 348 × 478 μm sample volume with voxel dimensions of 480 nm, subsequent division of the reconstructed volumes into sub-volumes ...

  5. Chitinase III in Euphorbia characias latex: Purification and characterization.

    Science.gov (United States)

    Spanò, Delia; Pospiskova, Kristyna; Safarik, Ivo; Pisano, Maria Barbara; Pintus, Francesca; Floris, Giovanni; Medda, Rosaria

    2015-12-01

    This paper deals with the purification of a class III endochitinase from Euphorbia characias latex. Described purification method includes an effective novel separation step using magnetic chitin particles. Application of magnetic affinity adsorbent noticeably simplifies and shortens the purification procedure. This step and the subsequently DEAE-cellulose chromatography enable to obtain the chitinase in homogeneous form. One protein band is present on PAGE in non-denaturing conditions and SDS-PAGE profile reveals a unique protein band of 36.5 ± 2 kDa. The optimal chitinase activity is observed at 50 °C, pH 5.0. E. characias latex chitinase is able to hydrolyze colloidal chitin giving, as reaction products, N-acetyl-D-glucosamine, chitobiose and chitotriose. Moreover, we observed that calcium and magnesium ions enhance chitinase activity. Finally, we cloned the cDNA encoding the E. characias latex chitinase. The partial cDNA nucleotide sequence contains 762 bp, and the deduced amino acid sequence (254 amino acids) is homologous to the sequence of several plant class III endochitinases. Copyright © 2015 Elsevier Inc. All rights reserved.

  6. Graphite Microstructural Characterization Using Time-Domain and Correlation-Based Ultrasonics

    Energy Technology Data Exchange (ETDEWEB)

    Spicer, James [Johns Hopkins Univ., Baltimore, MD (United States)

    2017-12-06

    how these measurements can be used to assess elastic anisotropy in nuclear graphites. Using models developed in this program, ultrasonic data were interpreted to extract orientation distribution coefficients that could be used to represent anisotropy in these materials. This demonstration showed the use of ultrasonic methods to quantify anisotropy and how these methods provide more detailed information than do measurements of thermal expansion – a technique commonly used for assessing anisotropy in nuclear graphites. Finally, we have employed laser-based, ultrasonic-correlation techniques in attempts to quantify aspects of graphite microstructure such as pore size and distribution. Results of these measurements indicate that additional work must be performed to make this ultrasonic approach viable for quantitative microstructural characterization.

  7. Magnesium substitution in carbonated hydroxyapatite: Structural and microstructural characterization by Rietveld's refinement

    Energy Technology Data Exchange (ETDEWEB)

    Lala, S. [Materials Science Division, Department of Physics, The University of Burdwan, Golapbag, Burdwan 713104, West Bengal (India); Ghosh, M.; Das, P.K. [Department of Biological Chemistry, Indian Association for the Cultivation of Science, Jadavpur, Kolkata 700 032 (India); Das, D. [UGC-DAE Consortium for Scientific Research, Kolkata 700098 (India); Kar, T. [Department of Materials Science, Indian Association for the Cultivation of Science, Jadavpur, Kolkata 700032 (India); Pradhan, S.K., E-mail: skpradhan@phys.buruniv.ac.in [Materials Science Division, Department of Physics, The University of Burdwan, Golapbag, Burdwan 713104, West Bengal (India)

    2016-02-15

    Four stoichiometric compositions of nanocrystalline Mg doped carbonated hydroxyapatite (cHAp) powders are synthesized by mechanical alloying (ball milling) the powder mixtures of CaCO{sub 3}, CaHPO{sub 4}.2H{sub 2}O and MgO in open air at room temperature. FTIR analysis confirms the A-type carbonation in all milled HAp powder samples (A-cHAp). Microstructure characterization in terms of lattice imperfections and phase quantification of ball milled samples are made by analyzing XRD patterns employing Rietveld's structure refinement method. Transmission electron microscopy (TEM) study of 15 mol % Mg doped A-cHAp sample reveals microstructure similar to that obtained from XRD pattern analysis. Cumulative effect of Mg substitution and mechanical alloying results in amorphization of a major part of crystalline A-cHAp, analogous to native bone mineral. Rietveld analysis reveals that the Ca2 vacancy site is energetically more favorable for occupation of Mg substitution. MTT [3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide] assay test reveals sufficiently high percentage cell viability confirming the cytocompatibility of the sample. - Graphical abstract: Mg substitution for Ca2 site. - Highlights: • Single phase Mg doped A-cHAp synthesized by mechanical alloying (MA). • FTIR analysis confirms A-type carbonation in HAp. • Amorphization of a part of crystalline A-cHAp due to MA and Mg insertion. • Mg{sup 2+} ions substitute the Ca2 vacancy site. • High cell viability under MTT assay.

  8. Microstructural Consequences of Blast Lung Injury Characterized with Digital Volume Correlation

    Directory of Open Access Journals (Sweden)

    Hari Arora

    2017-12-01

    Full Text Available This study focuses on microstructural changes that occur within the mammalian lung when subject to blast and how these changes influence strain distributions within the tissue. Shock tube experiments were performed to generate the blast injured specimens (cadaveric Sprague-Dawley rats. Blast overpressures of 100 and 180 kPa were studied. Synchrotron tomography imaging was used to capture volumetric image data of lungs. Specimens were ventilated using a custom-built system to study multiple inflation pressures during each tomography scan. These data enabled the first digital volume correlation (DVC measurements in lung tissue to be performed. Quantitative analysis was performed to describe the damaged architecture of the lung. No clear changes in the microstructure of the tissue morphology were observed due to controlled low- to moderate-level blast exposure. However, significant focal sites of injury were observed using DVC, which allowed the detection of bias and concentration in the patterns of strain level. Morphological analysis corroborated the findings, illustrating that the focal damage caused by a blast can give rise to diffuse influence across the tissue. It is important to characterize the non-instantly fatal doses of blast, given the transient nature of blast lung in the clinical setting. This research has highlighted the need for better understanding of focal injury and its zone of influence (alveolar interdependency and neighboring tissue burden as a result of focal injury. DVC techniques show great promise as a tool to advance this endeavor, providing a new perspective on lung mechanics after blast.

  9. Characterization of resistant starch type III from banana (Musa acuminata).

    Science.gov (United States)

    Lehmann, Undine; Jacobasch, Gisela; Schmiedl, Detlef

    2002-08-28

    Banana starch (Musa acuminata var. Nandigobe) was evaluated for its use in generating resistant starch (RS) type III. Structural, physicochemical, and biological properties of these products were analyzed. The investigated process includes debranching of the native starch and retrogradation under different storage temperatures and starch concentrations. After enzymatic debranching, a high amount of low-molecular-weight polymers with a degree of polymerization between 10 and 35 glucose units beside a higher molecular weight fraction were found. The resulting products comprised RS contents of about 50%. After heat-moisture treatment, the RS yield increased up to 84%. Peak temperatures of about 145 degrees C found in DSC measurements pointed to a high thermal stability of the RS products. In vitro fermentations of the RS products, carried out with intestinal microflora of healthy humans, resulted in a molar ratio of acetate:propionate:butyrate of about 49:17:34. The established method allowed the production of a high-quality RS with prebiotic properties for health preventing applications.

  10. Synthesis, characterization, antiplasmodial and antitrypanosomal activity of some metal(III complexes of sulfadiazine

    Directory of Open Access Journals (Sweden)

    P.A. Ajibade

    2008-08-01

    Full Text Available The Fe(III, Ru(III, Rh(III, and Cr(III complexes of 4-amino-N-(2-pyrimidinylbenzene sulfonamide (sulfadiazine have been synthesized and characterized by elemental analysis, electronic and IR spectroscopy, conductance and room temperature magnetic susceptibility measurements. Sulfadiazine acts as a bidentate ligand through the sulfonamido and the pyrimidinic N-atoms. The compounds are non-electrolytes and the electronic spectra are consistent with the proposed octahedral geometry around the metal ions. The complexes were tested for in vitro activity against cultures of the resistant strains of Plasmodium falciparum, tripamastigotes T. b. rhodesiense and amastigotes L. donovani to determine their antiprotozoal activities. The Fe(III complex is more active than the other complexes against the parasitic protozoa.

  11. Optical and Micro-Structural Characterization of MBE Grown Indium Gallium Nitride Polar Quantum Dots

    KAUST Repository

    El Afandy, Rami

    2011-07-07

    Gallium nitride and related materials have ushered in scientific and technological breakthrough for lighting, mass data storage and high power electronic applications. These III-nitride materials have found their niche in blue light emitting diodes and blue laser diodes. Despite the current development, there are still technological problems that still impede the performance of such devices. Three-dimensional nanostructures are proposed to improve the electrical and thermal properties of III-nitride optical devices. This thesis consolidates the characterization results and unveils the unique physical properties of polar indium gallium nitride quantum dots grown by molecular beam epitaxy technique. In this thesis, a theoretical overview of the physical, structural and optical properties of polar III-nitrides quantum dots will be presented. Particular emphasis will be given to properties that distinguish truncated-pyramidal III-nitride quantum dots from other III-V semiconductor based quantum dots. The optical properties of indium gallium nitride quantum dots are mainly dominated by large polarization fields, as well as quantum confinement effects. Hence, the experimental investigations for such quantum dots require performing bandgap calculations taking into account the internal strain fields, polarization fields and confinement effects. The experiments conducted in this investigation involved the transmission electron microscopy and x-ray diffraction as well as photoluminescence spectroscopy. The analysis of the temperature dependence and excitation power dependence of the PL spectra sheds light on the carrier dynamics within the quantum dots, and its underlying wetting layer. A further analysis shows that indium gallium nitride quantum dots through three-dimensional confinements are able to prevent the electronic carriers from getting thermalized into defects which grants III-nitrides quantum dot based light emitting diodes superior thermally induced optical

  12. Synthesis and characterization of Fe(III-piperazine-derived complexes encapsulated in zeolite Y

    Directory of Open Access Journals (Sweden)

    Márcio E. Berezuk

    2012-01-01

    Full Text Available Zeolite-encapsulated complexes have been widely applied in hydrocarbon oxidation catalysis. The "ship-in-a-bottle" encapsulation of iron(III complexes containing piperazine and piperazine-derivative ligands in zeolite-Y is described. The flexible ligand methodology was employed and the efficiency and reproducibility of the procedure was investigated. The catalysts were characterized employing several techniques and the results indicate the presence of coordinated and uncoordinated iron(III ions inside and outside the zeolitic cage.

  13. Cloning, overexpression, and characterization of recombinant heparinase III from Bacteroides stercoris HJ-15.

    Science.gov (United States)

    Hyun, Yang-Jin; Lee, Jeong Hoon; Kim, Dong-Hyun

    2010-04-01

    Recombinant heparinase III (rHepIII) from Bacteroides stercoris HJ-15 was cloned, expressed, and characterized. The full-length heparinase III gene from B. stercoris HJ-15 was identified by Southern blotting, and the sequence was deposited in GenBank. The heparinase III gene, which is 2,001-bp long, was cloned and overexpressed in Escherichia coli; highly active rHepIII was easily purified using only one step of immobilized Ni(2+) affinity column chromatography. Enzymatic properties and substrate specificities of rHepIII were assessed, and its kinetic constants were calculated. rHepIII was most active in 50 mM sodium phosphate buffer with 350 mM NaCl (pH 6.6) at 45 degrees C. Through amino acid modification studies and site-directed mutagenesis assay, cysteines and histidines were identified as crucial residues for enzymatic activity. Moreover, this enzyme digested not only heparan sulfate but also heparin and hyaluronic acid, and their degradation products were verified by strong anion exchange/high-performance liquid chromatography. These characteristics, including active residues and substrate specificities were interesting compared with those of existing heparinase III from other species. We anticipate that the convenience of purification and the characteristics of this enzyme will make it a powerful tool for studies of glycosaminoglycans and their lyases.

  14. Characterization of Water Extractable Arabinoxylans from a Spring Wheat Flour: Rheological Properties and Microstructure

    Directory of Open Access Journals (Sweden)

    Alma Campa-Mada

    2013-07-01

    Full Text Available In the present study water extractable arabinoxylans (WEAX from a Mexican spring wheat flour (cv. Tacupeto F2001 were isolated, characterized and gelled and the gel rheological properties and microstructure were investigated. These WEAX presented an arabinose to xylose ratio of 0.66, a ferulic acid and diferulic acid content of 0.526 and 0.036 µg/mg WEAX, respectively and a Fourier Transform Infra-Red (FT-IR spectrum typical of arabinoxylans. The intrinsic viscosity and viscosimetric molecular weight values for WEAX were 3.5 dL/g and 504 kDa, respectively. WEAX solution at 2% (w/v formed gels induced by a laccase as cross-linking agent. Cured WEAX gels registered storage (G’ and loss (G’’ modulus values of 31 and 5 Pa, respectively and a diferulic acid content of 0.12 µg/mg WEAX, only traces of triferulic acid were detected. Scanning electron microscopy analysis of the lyophilized WEAX gels showed that this material resembles that of an imperfect honeycomb.

  15. Microstructure characterization of high-purity aluminum processed by dynamic severe plastic deformation

    Energy Technology Data Exchange (ETDEWEB)

    Dirras, Guy; Chauveau, Thierry; Ramtani, Salah; Bui, Quang-Hien [LPMTM, CNRS, UPR 9001, Universite Paris 13, 99 avenue J. B. Clement, 93430 Villetaneuse (France); Abdul-Latif, Akrum [Laboratoire d' Ingenierie des Systemes Mecaniques et des Materiaux, 3 rue Fernand Hainaut, 93407 St Ouen Cedex (France)

    2010-10-15

    Fine-grained aluminum (700-1000 nm) was processed by dynamic severe plastic deformation of coarse-grained (3 mm) pure aluminum (99.999 wt.%). The resulting microstructure was characterized by transmission electron microscopy (TEM) and X-ray profile analyses. It is observed that the grain size determined by TEM departs from measurements made by X-ray profile analysis. In the latter case, the average crystallite size determined over the global crystallographic or on the deformation-induced texture components, namely {l_brace}123{r_brace} left angle 751 right angle, {l_brace}100{r_brace} left angle 011 right angle, and {l_brace}223{r_brace} left angle 154 right angle, yields similar values ({proportional_to}225 nm). By contrast, the dislocation density determined on these texture components is about two times higher than the one measured on the global texture. The difference might be related to the specificities of the induced crystallographic texture. (Abstract Copyright [2010], Wiley Periodicals, Inc.)

  16. Characterization the microstructure and defects of matrix graphite irradiated with Xe ions

    Science.gov (United States)

    Xu, H. X.; Lin, J.; Li, J. J.; Zhu, Z. Y.; Zeng, G. L.; Liu, J. D.; Gu, B. C.; Liu, B.

    2017-09-01

    The matrix graphite of pebble fuel elements was irradiated with 1 MeV Xe ions at room temperature to fluences of 5.8 × 1014 ions/cm2 and 2.9 × 1015 ions/cm2, respectively. The microstructure and defects of matrix graphite samples were characterized by using scanning electron microscopy (SEM), Raman spectroscopy and slow positron beam techniques. The SEM result reveals that hundred-nanometer sized pores appear at the surface after irradiation and the density of pore increases with fluence. Raman results show that D peak (1350 cm-1) and G peak (1580 cm-1) are broadened after irradiation. In addition, the G peak position shifts from 1580 cm-1 to 1560 cm-1 with the linewidth increases from 21 cm-1 to 132 cm-1, corresponding to the increase in bond-angle disorder as the matrix graphite transforms from microcrystalline to amorphous carbon(a-C). The slow positron beam study shows that the defects-trapped positron S parameter increases with fluence, suggesting that the vacancy-type defects concentration or size of open volume defects increases. The analysis of Raman and slow positron beam consistently conclude that the reason for the phase transition after irradiation is the increase in irradiation-induced vacancy defects accompanied by the overlap of disordered regions.

  17. Microstructural and mechanical characterization of alumina scales thermally developed on iron aluminide alloys

    Energy Technology Data Exchange (ETDEWEB)

    Natesan, K.; Renusch, D.; Veal, B.W.; Grimsditch, M. [and others

    1996-11-01

    To understand the underlying phenomena when characterizing material performance, we must know the chemistry and physics of the early stages of oxidation, chemistry, and bonding at the substrate/oxide interface, effect of segregants on the strength of bonding, transport processes through the scale formed during corrosion, mechanisms of residual stress generation and relief, and fracture behavior at the oxide/substrate interface. Specific objectives of the program described here are to (a) systematically investigate the relationships among substrate composition and properties and scale/coating adherence, damage tolerance, and micromechanical properties; (b) use results from the investigation to prevent scale/coating failure at elevated temperatures; and (c) identify conditions that lead to coatings that are more damage tolerant and scales that are amenable to legitimate synthesis routes. This report presents experimental data on the microstructural characteristics of alumina scales that have been thermally developed on several Fe-based alumina-forming intermetallic alloys. In addition, data are presented on scale adhesion, along with determinations of strain from data obtained by ruby fluorescence.

  18. Microstructural and Process Characterization of Conductive Traces Printed from Ag Particulate Inks

    Directory of Open Access Journals (Sweden)

    Eric MacDonald

    2011-05-01

    Full Text Available Conductive inks are key enablers for the use of printing techniques in the fabrication of electronic systems. Focus on the understanding of aspects controlling the electrical performance of conductive ink is paramount. A comparison was made between microparticle Ag inks and an Ag nanoparticle ink. The microstructures resulting from thermal cure processes were characterized morphologically and also in terms of their effect on the resistivity of printed traces. For microparticle inks, the variability of resistivity measurements between samples as defined by coefficient of variation (CV was greater than 0.1 when the resistivity was 10 to 50 times that of bulk Ag. When the resistivity was lower (~1.4 times that of bulk Ag the CV of sample sets was less than 0.1. In the case of the nanoparticle ink, resistivity was found to decrease by a factor ranging from 1.2 to 1.5 after doubling the amount of layers printed prior to curing though it was expected to remain the same. Increasing the amount of layers printed also enhanced the sintering process.

  19. Microstructural and Process Characterization of Conductive Traces Printed from Ag Particulate Inks.

    Science.gov (United States)

    Roberson, David A; Wicker, Ryan B; Murr, Lawrence E; Church, Ken; MacDonald, Eric

    2011-05-26

    Conductive inks are key enablers for the use of printing techniques in the fabrication of electronic systems. Focus on the understanding of aspects controlling the electrical performance of conductive ink is paramount. A comparison was made between microparticle Ag inks and an Ag nanoparticle ink. The microstructures resulting from thermal cure processes were characterized morphologically and also in terms of their effect on the resistivity of printed traces. For microparticle inks, the variability of resistivity measurements between samples as defined by coefficient of variation (CV) was greater than 0.1 when the resistivity was 10 to 50 times that of bulk Ag. When the resistivity was lower (~1.4 times that of bulk Ag) the CV of sample sets was less than 0.1. In the case of the nanoparticle ink, resistivity was found to decrease by a factor ranging from 1.2 to 1.5 after doubling the amount of layers printed prior to curing though it was expected to remain the same. Increasing the amount of layers printed also enhanced the sintering process.

  20. Shock and Microstructural Characterization of the α-ω Phase Transition in Titanium Crystals

    Science.gov (United States)

    Morrow, Benjamin M.; Rigg, Paulo A.; Jones, David R.; Addessio, Francis L.; Trujillo, Carl P.; Saavedra, Ramon A.; Martinez, Daniel T.; Cerreta, Ellen K.

    2017-12-01

    A multicrystal comprised of a small number of large crystals of high-purity titanium and a [0001] oriented high-purity single crystal titanium sample were shock loaded using gas gun plate impact experiments. Tests were performed at stresses above the α {-}ω phase transition stress (for high-purity polycrystalline specimens) to observe the behavior of oriented crystals under similar conditions. Post-mortem characterization of the shocked microstructure was conducted on the single crystal sample to measure textures, and quantify phases and twinning. The apparent activation of plastic and transformation mechanisms was dependent upon crystal orientation. Specifically, the [0001] crystal showed a higher Hugoniot elastic limit than the [10\\bar{1}0] or [3\\bar{1}\\bar{4}4] orientations. The slope of velocity as a function of time was lower in the [0001] orientation than the other orientations during plastic deformation, indicating sluggish transformation kinetics for the α to ω phase transition for the [0001] oriented crystal. Microtexture measurements of a recovered [0001] oriented single crystal revealed the presence of retained ω phase after unloading, with orientations of the constituent phase fractions indicative of the forward α → ω transition, rather than the reverse ω → α transition, suggesting that the material never achieved a state of 100% ω phase.

  1. Obtention of uranium-molybdenum alloy ingots microstructure and phase characterization

    Energy Technology Data Exchange (ETDEWEB)

    Pedrosa, Tercio A.; Braga, Daniel M.; Paula, Joao Bosco de; Brina, Jose Giovanni M.; Ferraz, Wilmar B., E-mail: tap@cdtn.b, E-mail: bragadm@cdtn.b, E-mail: jbp@cdtn.b, E-mail: jgmb@cdtn.b, E-mail: ferrazw@cdtn.b [Centro de Desenvolvimento da Tecnologia Nuclear (CDTN/CNEN-MG), Belo Horizonte, MG (Brazil)

    2011-07-01

    The replacement of high enriched uranium (U-{sup 235} > 85 wt%) by low enriched uranium (U-{sup 235} < 20 wt%) nuclear fuels in research and test reactors is being implemented as an initiative of the Reduced Enrichment for Research and Test Reactors (RERTR) program, conceived in the USA since mid-70s, in order to avoid nuclear weapons proliferation. Such replacement implies in the use of compounds or alloys with higher uranium densities. Several uranium alloys that fill this requirement has been investigated since then. Among these alloys, U-Mo presents great application potential due to its physical properties and good behavior during irradiation, which makes it an important option as a nuclear fuel material for the Brazilian Multipurpose Reactor - RMB. The development of the plate-type nuclear fuel based on U-Mo alloys is being performed at the Nuclear Technology Development Centre (CDTN) and also at the Institute of Energetic and Nuclear Research - IPEN. U-{sup 10}Mo ingots were melted in an induction furnace with protective argon atmosphere. The microstructure of the ingots were characterized through optical and scanning electronic microscopy in the as cast and heat treated conditions. Energy Dispersive Spectrometry and X-Ray Diffraction were used as characterization techniques for elemental analysis and phases determination. It was confirmed the presence of metastable gamma-phase in the as cast condition, surrounded by hypereutectoid alpha-phase (uranium-rich phase), as well as a pearlite-like constituent, composed by alternated lamellas of U{sub 2}Mo compound and alpha-phase, in the heat treated condition. (author)

  2. Deformation microstructures

    DEFF Research Database (Denmark)

    Hansen, N.; Huang, X.; Hughes, D.A.

    2004-01-01

    Microstructural characterization and modeling has shown that a variety of metals deformed by different thermomechanical processes follows a general path of grain subdivision, by dislocation boundaries and high angle boundaries. This subdivision has been observed to very small structural scales...... of the order of 10 nm, produced by deformation under large sliding loads. Limits to the evolution of microstructural parameters during monotonic loading have been investigated based on a characterization by transmission electron microscopy. Such limits have been observed at an equivalent strain of about 10...

  3. An Automated Multi-Modal Serial Sectioning System for Characterization of Grain-Scale Microstructures in Engineering Materials (Preprint)

    Science.gov (United States)

    2012-03-01

    ENGINEERING MATERIALS (PREPRINT) Michael Uchic, Michael Groeber , and Jonathan Spowart Metals Branch Metals, Ceramics & Nondestructive Evaluation...AUTHOR(S) Michael Uchic, Michael Groeber , and Jonathan Spowart (AFRL/RXLM) Megna Shah and Michael Scott (UES Inc.) Patrick Callahan (Carnegie...3D microstructural characterization of nickel superalloys via serial- sectioning using a dual beam FIB-SEM. Scripta Materialia 55:23-28 [7] Groeber MA

  4. Microstructure, characterizations, functionality and compressive strength of cement-based materials using zinc oxide nanoparticles as an additive

    Energy Technology Data Exchange (ETDEWEB)

    Nochaiya, Thanongsak [Department of Physics, Faculty of Science, Naresuan University, Phitsanulok 65000 (Thailand); Sekine, Yoshika [Department of Chemistry, School of Science, Tokai University, 4-1-1 Kitakaname, Hiratsuka, Kanagawa 259-1292 (Japan); Choopun, Supab [Applied Physics Research Laboratory, Department of Physics and Materials Science, Faculty of Science, Chiang Mai University, Chiang Mai 50200 (Thailand); Chaipanich, Arnon, E-mail: arnon.chaipanich@cmu.ac.th [Advanced Cement-Based Materials Research Unit, Department of Physics and Materials Science, Faculty of Science, Chiang Mai University, Chiang Mai 50200 (Thailand)

    2015-05-05

    Highlights: • Nano zinc oxide was used as an additive material. • Microstructure and phase characterization of pastes were characterized using SEM and XRD. • TGA and FTIR were also used to determine the hydration reaction. • Compressive strength of ZnO mixes was found to increase at 28 days. - Abstract: Zinc oxide nanoparticles as a nanophotocatalyst has great potential for self-cleaning applications in concrete structures, its effects on the cement hydration, setting time and compressive strength are also important when using it in practice. This paper reports the effects of zinc oxide nanoparticles, as an additive material, on properties of cement-based materials. Setting time, compressive strength and porosity of mortars were investigated. Microstructure and morphology of pastes were characterized using scanning electron microscope and X-ray diffraction (XRD), respectively. Moreover, thermal gravimetric analysis (TGA) and Fourier-transform infrared spectrometer (FTIR) were also used to determine the hydration reaction. The results show that Portland cement paste with additional ZnO was found to slightly increase the water requirement while the setting time presented prolongation period than the control mix. However, compressive strength of ZnO mixes was found to be higher than that of PC mix up to 15% (at 28 days) via filler effect. Microstructure, XRD and TGA results of ZnO pastes show less hydration products before 28 days but similar at 28 days. In addition, FTIR results confirmed the retardation when ZnO was partially added in Portland cement pastes.

  5. Microstructural characterization of Cu82.3Al8.3Mn9.4 shape memory alloy after rolling

    Directory of Open Access Journals (Sweden)

    Mirko Gojić

    2017-09-01

    Full Text Available In this paper, the microstructure of Cu82.3Al8.3Mn9.4 (in wt. % shape memory alloy after hot and cold rolling was investigated. The Cu82.3Al8.3Mn9.4 alloy was produced by a vertical continuous casting method in the form a cylinder rod of 8 mm in diameter. After the casting, hot and cold rolling was performed. By hot rolling a strip with a thickness of 1.75 mm was obtained, while by cold rolling a strip with a thickness of 1.02 mm was produced. After the rolling process, heat treatment was performed. Heat treatment was carried out by solution annealing at 900 °C held for 30 minutes and water quenched immediately after heating. The microstructure characterization of the investigated alloy was carried out by optical microscopy (OM, scanning electron microscopy (SEM equipped with a device for energy dispersive spectroscopy (EDS. Phase transformation temperatures and fusion enthalpies were determined by differential scanning calorimetry (DSC method. The homogenous martensite microstructure was confirmed by OM and SEM micrographs after casting. During rolling the two-phase microstructure occurred. Results of DSC analysis showed martensite start (Ms, martensite finish (Mf, austenite start (As and austenite finish (Af temperatures.

  6. Cloning and characterization of type III iodothyronine deiodinase from the fish Oreochromis niloticus

    NARCIS (Netherlands)

    J.P. Sanders (Jo); S. van der Geyten; E. Kaptein (Ellen); V.M. Darras (Veerle); E.R. Kuhn; J.L. Leonard; T.J. Visser (Theo)

    1999-01-01

    textabstractType III iodothyronine deiodinase (D3) catalyzes the inner ring deiodination (IRD) of T4 and T3 to the inactive metabolites rT3 and 3,3'-diiodothyronine (3,3'-T2), respectively. Here we describe the cloning and characterization of complementary DNA (cDNA)

  7. CLONING, EXPRESSION, AND CHARACTERIZATION OF RAT S-ADENOSYL-L-METHIONINE: ARSENIC (III) METHYLTRANSFERASE (CYT19)

    Science.gov (United States)

    CLONING, EXPRESSION, AND CHARACTERIZATION OF RAT S-ADENOSYL-L-METHIONINE: ARSENIC(III) METHYLTRANSFERASE (cyt19)Stephen B. Waters1 , Felicia Walton1 , Miroslav Styblo1 , Karen Herbin-Davis2, and David J. Thomas2 1 School of Medicine, University of North Carolina at Chape...

  8. Effects of Pulsed Nd:YAG Laser Welding Parameters on Penetration and Microstructure Characterization of a DP1000 Steel Butt Joint

    National Research Council Canada - National Science Library

    Xin Xue; António B Pereira; Jose Amorim; Juan Liao

    2017-01-01

    Of particular importance and interest are the effects of pulsed Nd:YAG laser beam welding parameters on penetration and microstructure characterization of DP1000 butt joint, which is widely used in the automotive industry nowadays...

  9. The Influence of Casting Conditions on the Microstructure of As-Cast U-10Mo Alloys: Characterization of the Casting Process Baseline

    Energy Technology Data Exchange (ETDEWEB)

    Nyberg, Eric A.; Joshi, Vineet V.; Lavender, Curt A.; Paxton, Dean M.; Burkes, Douglas

    2013-12-13

    Sections of eight plate castings of uranium alloyed with 10 wt% molybdenum (U-10Mo) were sent from Y-12 to the Pacific Northwest National Laboratory (PNNL) for microstructural characterization. This report summarizes the results from this study.

  10. Study of the microstructure and the hardness of PZT piezoelectric ceramics types I and III used in electro acoustic transducers; Estudo da microestrutura e da microdureza das ceramicas piezoeletricas tipos PZT I e III utilizadas em transdutores eletroacusticos

    Energy Technology Data Exchange (ETDEWEB)

    Cabral, Ricardo de Freitas; Itaboray, Lucas Mendes; Santos, Anna Paula de Oliveira [Centro Universitario de Volta Redonda (UNIFOA), Volta Redonda, RJ (Brazil)

    2015-12-15

    The field of electronic processing of the ceramic piezoelectric type imported powdered led to the production of ceramics with 97% of theoretical density, homogeneous microstructure with great potential for applications in piezoelectric devices such as electro acoustic transducers. However, the production of electronic ceramics National piezoelectric type is not yet able to have as raw material zirconate titanate Lead (PZT) 100% made in Brazil. Thus, this is used for supply of domestic production, the zirconium oxide. In this work, both post PZT types I and III, imported, were uniaxially pressed at 70 MPa and sintered at 1200 and 1250 deg C for 3 hours. Hardness measurements were performed by micro indentation, X-ray diffraction analysis and Scanning Electron Microscopy. The hardness of PZT I was 393 HV. (author)

  11. Crystallographic, Microstructural, and Mechanical Characterization of Dynamically Processed EP741NP Superalloy

    Science.gov (United States)

    Sharma, A. D.; Sharma, A. K.; Thakur, N.

    2016-08-01

    Considerable progress has been made for the solidification of metal powders with improved properties by using varieties of metallurgical methods. However, solidification of superalloy powders offers many difficulties under traditional processes. This article outlines an extensive program being undertaken to produce monoliths of superalloys with enhanced microstructural and mechanical properties. EP741NP superalloy has been subjected to explosive shock wave loading to obtain uniform and crack-free monoliths. An axisymmetric cylindrical configuration with a plastic explosive of high-detonation velocity has been used to consolidate the superalloy powder nearer to its theoretical density (~98 pct). By careful design of experiments, detonation velocity has been measured vis-à-vis compaction of metal powders in a single-shot experiment by employing instrumented detonics. The shock-processed specimens characterized for phase, lattice parameter, and structural variation by X-ray diffraction technique show intact crystalline structure. Results obtained from Williamson-Hall method indicate small micro-strain (2.8 × 10-3) and decreased crystallite size. Energy-dispersive spectroscopy suggests no segregation within the specimens. Scanning electron microscopy shows fracture-less and micro-cracks/void-free compacts of superalloy indicating satisfactory sub-structural strength. Indentation experiments with variable loads (1.96 N and 2.94 N) performed on the shock-processed specimen cut along transverse section show high order of Vicker's micro-hardness value up to 486 H v. The tensile and compressive strengths of the superalloy monoliths cut along the consolidation axes have been found to be 824 and 834 MPa, respectively.

  12. Microstructural characterization and chemical compatibility of pulsed laser deposited yttria coatings on high density graphite

    Energy Technology Data Exchange (ETDEWEB)

    Sure, Jagadeesh [Corrosion Science and Technology Group, Indira Gandhi Centre for Atomic Research, Kalpakkam — 603 102 (India); Mishra, Maneesha [Physical Metallurgy Group, Indira Gandhi Centre for Atomic Research, Kalpakkam-603 102 (India); Tarini, M. [SRM University, Kattankulathur-603 203 (India); Shankar, A. Ravi; Krishna, Nanda Gopala [Corrosion Science and Technology Group, Indira Gandhi Centre for Atomic Research, Kalpakkam — 603 102 (India); Kuppusami, P. [Physical Metallurgy Group, Indira Gandhi Centre for Atomic Research, Kalpakkam-603 102 (India); Mallika, C. [Corrosion Science and Technology Group, Indira Gandhi Centre for Atomic Research, Kalpakkam — 603 102 (India); Mudali, U. Kamachi, E-mail: kamachi@igcar.gov.in [Corrosion Science and Technology Group, Indira Gandhi Centre for Atomic Research, Kalpakkam — 603 102 (India)

    2013-10-01

    Yttria coatings were deposited on high density (HD) graphite substrate by pulsed laser deposition method and subsequently annealing in vacuum at 1373 K was carried out to evaluate the thermal stability of the coatings. Yttria deposited on HD graphite samples were exposed to molten LiCl–KCl salt at 873 K for 3 h to evaluate the corrosion behavior of the coating for the purpose of pyrochemical reprocessing applications. The microstructure and the corrosion behavior of the yttria coating deposited on HD graphite in molten LiCl–KCl salt were evaluated by several characterization techniques. X-ray diffraction and Laser Raman patterns confirmed the presence of cubic phase of yttria in the coating. The surface morphology of yttria coating on HD graphite examined by scanning electron microscope and atomic force microscopy revealed the agglomeration of oxide particles and formation of clusters. After annealing at 1373 K, no appreciable grain growth of yttria particles could be observed. X-ray photoelectron spectroscopy analysis was carried out for elemental analysis before and after chemical compatibility test of the coated samples in molten LiCl–KCl salt to identify the corrosive elements present on the yttria coatings. The chemical compatibility and thermal stability of the yttria coating on HD graphite in molten LiCl–KCl salt medium have been established. - Highlights: • Y{sub 2}O{sub 3} coating was deposited on graphite by pulsed laser deposition method. • Chemical compatibility of Y{sub 2}O{sub 3} coating in LiCl–KCl salt at 873 K was studied. • Gibbs free energy change was positive for Y{sub 2}O{sub 3} reaction with Cl{sub 2}, U and UCl{sub 3}. • Y{sub 2}O{sub 3} coating exhibited better corrosion performance in molten LiCl–KCl salt.

  13. Microstructure Characterization and Wear-Resistant Properties Evaluation of an Intermetallic Composite in Ni-Mo-Si System.

    Science.gov (United States)

    Huang, Boyuan; Song, Chunyan; Liu, Yang; Gui, Yongliang

    2017-02-04

    Intermetallic compounds have been studied for their potential application as structural wear materials or coatings on engineering steels. In the present work, a newly designed intermetallic composite in a Ni-Mo-Si system was fabricated by arc-melting process with commercially pure metal powders as starting materials. The chemical composition of this intermetallic composite is 45Ni-40Mo-15Si (at %), selected according to the ternary alloy diagram. The microstructure was characterized using optical microscopy (OM), scanning electron microscopy (SEM), X-ray diffraction (XRD), and energy dispersive spectroscopy (EDS), and the wear-resistant properties at room temperature were evaluated under different wear test conditions. Microstructure characterization showed that the composite has a dense and uniform microstructure. XRD results showed that the intermetallic composite is constituted by a binary intermetallic compound NiMo and a ternary Mo₂Ni₃Si metal silicide phase. Wear test results indicated that the intermetallic composite has an excellent wear-resistance at room-temperature, which is attributed to the high hardness and strong atomic bonding of constituent phases NiMo and Mo₂Ni₃Si.

  14. Gold(III) Complex of Caffeine: Synthesis, Isolation and Spectroscopic Characterization

    OpenAIRE

    IVANOVA, Bojidarka

    2014-01-01

    Au(III)-caffeine complex was synthesized and characterized by means of solid-state linear-dichroic infrared spectral analysis (IRLD), 1H-NMR, MS, DSC and TGA methods. The caffeine (I) is monodentate and coordinated with metal ion through its N9 atom at molar ratio metal to ligand 1:1. The other 3 positions in the Au(III) coordination sphere are occupied by Cl-, thus forming [Au3+(C8H10N4O2)Cl3] complex. IR-characteristic band assignment in the 4000-400 cm-1 IR region of pure ligand ...

  15. Microstructure Characterization and Hardness Evaluation of Alloy 52 Welded Stainless Steel 316 Subjected to Ultrasonic Nanocyrtal Surface Modification Technique

    Energy Technology Data Exchange (ETDEWEB)

    Kim, H. D.; Amanov, A.; Pyun, Y. S. [Sun Moon Univ., Asan (Korea, Republic of); Kim, Y. S.; Choi, Y. S. [Andong National Univ., Andong (Korea, Republic of)

    2015-10-15

    In this study, an ultrasonic nanocrystal surface modification (UNSM) technique was applied to dissimilar weld point between STS316L and Alloy 52. This UNSM technique is a patented technology, which can be described as a type of ultrasonic cold-forging technology. It has been demonstrated that the UNSM technique is a simple method to produce a nanocrystalline surface layer at the top surface of metallic materials. Microstructure and hardness of STS316L and Alloy 52 are investigated before and after UNSM treatment. It is expected according to the previous study that the UNSM technique is able to release the residual stress which delays PWSCC. In this study, microstructural characterization and hardness evaluation of STS316L and welded Alloy 52 subjected to UNSM technique were investigated.

  16. Ultrasonic Characterization of Cast Austenitic Stainless Steel Microstructure: Discrimination between Equiaxed- and Columnar-Grain Material – An Interim Study

    Energy Technology Data Exchange (ETDEWEB)

    Ramuhalli, Pradeep; Good, Morris S.; Diaz, Aaron A.; Anderson, Michael T.; Watson, Bruce E.; Peters, Timothy J.; Dixit, Mukul; Bond, Leonard J.

    2009-10-27

    Ultrasonic nondestructive evaluation (NDE) and inspection of cast austenitic stainless steel (CASS) components used in the nuclear power industry is neither as effective nor reliable as is needed due to detrimental effects upon the interrogating ultrasonic beam and interference from ultrasonic backscatter. The root cause is the coarse-grain microstructure inherent to this class of materials. Some ultrasonic techniques perform better for particular microstructural classifications and this has led to the hypothesis that an ultrasonic inspection can be optimized for a particular microstructural class, if a technique exists to reliably classify the microstructure for feedback to the inspection. This document summarizes scoping experiments of in-situ ultrasonic methods for classification and/or characterization of the material microstructures in CASS components from the outside surface of a pipe. The focus of this study was to evaluate ultrasonic methods and provide an interim report that documents results and technical progress. An initial set of experiments were performed to test the hypothesis that in-service characterization of cast austenitic stainless steel (CASS) is feasible, and that, if reliably performed, such data would provide real-time feedback to optimize in-service inspections in the field. With this objective in mind, measurements for the experiment were restricted to techniques that should be robust if carried forward to eventual field implementation. Two parameters were investigated for their ability to discriminate between different microstructures in CASS components. The first parameter was a time-of-flight ratio of a normal incidence shear wave to that of a normal incidence longitudinal wave (TOFRSL). The ratio removed dependency on component thickness which may not be accurately reported in the field. The second parameter was longitudinal wave attenuation. The selected CASS specimens provided five equiaxed-grain material samples and five columnar

  17. Synthesis, spectroscopic characterization and antibacterial studies of lanthanide(III) Schiff base complexes containing N, O donor atoms

    Science.gov (United States)

    Lekha, L.; Raja, K. Kanmani; Rajagopal, G.; Easwaramoorthy, D.

    2014-01-01

    A series of six Ln(III) Schiff base complexes, Pr(III), Sm(III), Gd(III), Tb(III), Er(III) and Yb(III), were synthesized using sodium salt of Schiff base, 2-[(5-bromo-2-hydroxy-benzylidene)-amino]-3-hydroxy-propionic acid, derived from L-serine and 5-bromosalicylaldehyde. These complexes having general formula [Ln(L)(NO3)2(H2O)]·NO3 were characterized by elemental analysis, conductivity measurements, UV-Vis, FT-IR, mass spectrometry and fluorescence studies. Elemental analysis and conductivity measurements suggest the complexes have a 1:1 stoichiometry. From the spectral studies it has been concluded that Ln(III) complexes display eight coordination. The Schiff base and its Ln(III) metal complexes have also been screened for their antibacterial activities by Agar diffusion method.

  18. A Neutrally Charged Trimethylmanganese(III) Complex: Synthesis, Characterization, and Disproportionation Chemistry

    Energy Technology Data Exchange (ETDEWEB)

    Stalzer, Madelyn M.; Telser, Joshua; Krzystek, Jurek; Motta, Alessandro; Delferro, Massimiliano; Marks, Tobin J.

    2016-08-22

    The synthesis and properties of an unusual, neutrally charged and volatile N,N,N',N'-tetramethylethylenediamine trimethyl manganese(III) complex, (TMEDA)MnMe3, are described, along with its facile disproportionation to the corresponding Mn(II) and Mn(IV) complexes. Characterization by single-crystal XRD, UV-vis spectroscopy, high-frequency and -field EPR (HFEPR), magnetic susceptibility, and density functional theory (DFT) computations indicate that the (TMEDA)MnMe3 electronic structure can be described as largely square pyramidal Mn(III) centered. The paucity of manganese(III) polyalkyls and the simplicity and reactivity of this compound implicate it as a potentially useful synthetic building block.

  19. TRLFS characterization of Eu(III)-doped synthetic organo-hectorite.

    Science.gov (United States)

    Finck, Nicolas; Stumpf, Thorsten; Walther, Clemens; Bosbach, Dirk

    2008-12-12

    Europium(III) was coprecipitated with the clay mineral hectorite, a magnesian smectite, following a multi-step synthesis procedure. Different Eu(III) species associated with the proceeding synthetic hectorite were characterized by selectively exciting the 5D0-->7F0 transition at low temperature (T < 20 K). Fluorescence decay times indicated that Eu(III) ions may be incorporated in the octahedral layer of the brucite precursor as well as in the octahedral sheet of the clay mineral. The excitation spectra indicated that the substitution of the divalent Mg by the trivalent Eu induced local structural deformation. This investigation implements the molecular-level understanding of the f element structural incorporation into the octahedral layer of sheet silicates by coprecipitation with clay minerals from salt solutions at 100 degrees C.

  20. Microstructure Characterization of WCCo-Mo Based Coatings Produced Using High Velocity Oxygen Fuel

    Directory of Open Access Journals (Sweden)

    Serkan Islak

    2015-12-01

    Full Text Available The present study has been carried out in order to investigate the microstructural properties of WCCo-Mo composite coatings deposited onto a SAE 4140 steel substrate by high velocity oxygen fuel (HVOF thermal spray. For this purpose, the Mo quantity added to the WCCo was changed as 10, 20, 30 and 40 wt. % percents. The coatings are compared in terms of their phase composition, microstructure and hardness. Phase compound and microstructure of coating layers were examined using X-ray diffractometer (XRD and scanning electron microscope (SEM. XRD results showed that WCCo-Mo composite coatings were mainly composed of WC, W2C, Co3W3C, Mo2C, MoO2, Mo and Co phases. The average hardness of the coatings increased with increasing Mo content.

  1. Isothermal Transformation of a Commercial Super-Bainitic Steel: Part I Microstructural Characterization and Hardness

    Science.gov (United States)

    Han, Ying; Xiu, Wencui; Liu, Cheng; Wu, Hua

    2017-02-01

    The effects of isothermal treatment on the microstructure and hardness of commercial super-bainitic steel were investigated. A series of isothermal treatments were carried out at temperatures of 210-250 °C for different time periods. The results indicate that the bainitic reaction and hardness were very sensitive to the isothermal transformation temperature. The fine super-bainitic microstructure, containing the carbide-free bainitic ferrite lath and the carbon-enriched retained austenite film, can be produced by heating to 210 °C for 30 h, resulting in a hardness of 662 HV. By increasing the isothermal transformation temperature, the bainitic transformation kinetic is accelerated; however, this is at the expense of coarsening bainitic ferrite laths and decreasing the bainitic ferrite quantity. The relationship between hardness and microstructures obtained under different isothermal treatments, which is correlated with the carbon concentration, dislocation density, bainitic amount and super-bainite size, is discussed in detail.

  2. Microstructural characterization of fly ash particulate reinforced AA6063 aluminium alloy for aerospace applications

    Science.gov (United States)

    Razzaq, A. M.; Majid, D. L. Abang Abdul; Ishak, M. R.; Uday, M. B.

    2017-12-01

    Aluminium-fly ash (FA) particulate reinforced composites (AA6063-FA) have been used in automotive and aerospace industries because of their low density and good mechanical properties. Three different weight fraction of FA: 2%, 4% and 6% are added to AA6063 alloy using compocasting method. The effect of FA particulates on microstructure, density and compression strength of AA6063- FA composites are investigated. Field Emission Scanning Electron Microscope (FESEM) micrographs reveal that the FA particulates are uniformly distributed in AA6063 alloy. The results also show that density, compression strength and microstructure of the AA6063-FA composites are significantly influenced by the FA amount. The increase in the weight fraction of FA will improve the microstructure and enhance the compression strength. The density of AA6063-FA composites decreases as the incorporation of FA increases.

  3. Triple phase boundary specific pathway analysis for quantitative characterization of solid oxide cell electrode microstructure

    DEFF Research Database (Denmark)

    Jørgensen, Peter Stanley; Ebbehøj, Søren Lyng; Hauch, Anne

    2015-01-01

    The density and percolation of Triple phase boundary sites are important quantities in analyzing microstructures of solid oxide fuel cell electrodes from tomography data. However, these measures do not provide descriptions of the quality of the TPB sites in terms of the length and radius of the p......The density and percolation of Triple phase boundary sites are important quantities in analyzing microstructures of solid oxide fuel cell electrodes from tomography data. However, these measures do not provide descriptions of the quality of the TPB sites in terms of the length and radius...

  4. Microstructure characterization of alloy 625 deposited on nickel foam using air plasma spraying

    Energy Technology Data Exchange (ETDEWEB)

    Azarmi, F.; Saaedi, J.; Coyle, T.W.; Mostaghimi, J. [Center for Advanced Coating Technologies, University of Toronto (Canada)

    2008-05-15

    Ni-based superalloy 625 has been deposited on nickel foam by air plasma spraying (APS) using an optimized set of spraying parameters under two different substrate conditions. For condition (i) the substrate was not cooled during spraying and for condition (ii) the substrate constantly cooled using air jets during spraying. Microstructural characteristics of the as-sprayed coating microstructure were examined by a combination of optical and scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), image analysis, and X-ray diffraction (XRD) analysis, and compared to those of the alloy 625 powder used for spraying. (Abstract Copyright [2008], Wiley Periodicals, Inc.)

  5. Single‐molecule mechanochemical characterization of E. coli pol III core catalytic activity

    Science.gov (United States)

    Naufer, M. Nabuan; Murison, David A.; Rouzina, Ioulia; Beuning, Penny J.

    2017-01-01

    Abstract Pol III core is the three‐subunit subassembly of the E. coli replicative DNA polymerase III holoenzyme. It contains the catalytic polymerase subunit α, the 3′ → 5′ proofreading exonuclease ε, and a subunit of unknown function, θ. We employ optical tweezers to characterize pol III core activity on a single DNA substrate. We observe polymerization at applied template forces F  30 pN. Both polymerization and exonucleolysis occur as a series of short bursts separated by pauses. For polymerization, the initiation rate after pausing is independent of force. In contrast, the exonucleolysis initiation rate depends strongly on force. The measured force and concentration dependence of exonucleolysis initiation fits well to a two‐step reaction scheme in which pol III core binds bimolecularly to the primer‐template junction, then converts at rate k 2 into an exo‐competent conformation. Fits to the force dependence of k init show that exo initiation requires fluctuational opening of two base pairs, in agreement with temperature‐ and mismatch‐dependent bulk biochemical assays. Taken together, our results support a model in which the pol and exo activities of pol III core are effectively independent, and in which recognition of the 3′ end of the primer by either α or ε is governed by the primer stability. Thus, binding to an unstable primer is the primary mechanism for mismatch recognition during proofreading, rather than an alternative model of duplex defect recognition. PMID:28263430

  6. Isolation, characterization, and stability of discretely-sized nanolipoprotein particles assembled with apolipophorin-III.

    Directory of Open Access Journals (Sweden)

    Nicholas O Fischer

    Full Text Available BACKGROUND: Nanolipoprotein particles (NLPs are discoidal, nanometer-sized particles comprised of self-assembled phospholipid membranes and apolipoproteins. NLPs assembled with human apolipoproteins have been used for myriad biotechnology applications, including membrane protein solubilization, drug delivery, and diagnostic imaging. To expand the repertoire of lipoproteins for these applications, insect apolipophorin-III (apoLp-III was evaluated for the ability to form discretely-sized, homogeneous, and stable NLPs. METHODOLOGY: Four NLP populations distinct with regards to particle diameters (ranging in size from 10 nm to >25 nm and lipid-to-apoLp-III ratios were readily isolated to high purity by size exclusion chromatography. Remodeling of the purified NLP species over time at 4 degrees C was monitored by native gel electrophoresis, size exclusion chromatography, and atomic force microscopy. Purified 20 nm NLPs displayed no remodeling and remained stable for over 1 year. Purified NLPs with 10 nm and 15 nm diameters ultimately remodeled into 20 nm NLPs over a period of months. Intra-particle chemical cross-linking of apoLp-III stabilized NLPs of all sizes. CONCLUSIONS: ApoLp-III-based NLPs can be readily prepared, purified, characterized, and stabilized, suggesting their utility for biotechnological applications.

  7. Microstructural and Mechanical Characterization of a Custom-Built Implant Manufactured in Titanium Alloy by Direct Metal Laser Sintering

    Directory of Open Access Journals (Sweden)

    Maria Aparecida Larosa

    2014-08-01

    Full Text Available Custom-built implants manufacture has always presented difficulties which result in high cost and complex fabrication, mainly due to patients’ anatomical differences. The solution has been to produce prostheses with different sizes and use the one that best suits each patient. Additive manufacturing technology, incorporated into the medical field in the late 80's, has made it possible to obtain solid biomodels facilitating surgical procedures and reducing risks. Furthermore, this technology has been used to produce implants especially designed for a particular patient, with sizes, shapes, and mechanical properties optimized, for different areas of medicine such as craniomaxillofacial surgery. In this work, the microstructural and mechanical properties of Ti6Al4V samples produced by direct metal laser sintering (DMLS are studied. The microstructural and mechanical characterizations have been made by optical and scanning electron microscopy, X-ray diffraction, and microhardness and tensile tests. Samples produced by DMLS have a microstructure constituted by hexagonal α′ martensite with acicular morphology. An average microhardness of 370 HV was obtained and the tensile tests showed ultimate strength of 1172 MPa, yield strength of 957 MPa, and elongation at rupture of 11%.

  8. Hybrid approach combining multiple characterization techniques and simulations for microstructural analysis of proton exchange membrane fuel cell electrodes

    Energy Technology Data Exchange (ETDEWEB)

    Cetinbas, Firat C.; Ahluwalia, Rajesh K.; Kariuki, Nancy; De Andrade, Vincent; Fongalland, Dash; Smith, Linda; Sharman, Jonathan; Ferreira, Paulo; Rasouli, Somaye; Myers, Deborah J.

    2017-03-01

    The cost and performance of proton exchange membrane fuel cells strongly depend on the cathode electrode due to usage of expensive platinum (Pt) group metal catalyst and sluggish reaction kinetics. Development of low Pt content high performance cathodes requires comprehensive understanding of the electrode microstructure. In this study, a new approach is presented to characterize the detailed cathode electrode microstructure from nm to μm length scales by combining information from different experimental techniques. In this context, nano-scale X-ray computed tomography (nano-CT) is performed to extract the secondary pore space of the electrode. Transmission electron microscopy (TEM) is employed to determine primary C particle and Pt particle size distributions. X-ray scattering, with its ability to provide size distributions of orders of magnitude more particles than TEM, is used to confirm the TEM-determined size distributions. The number of primary pores that cannot be resolved by nano-CT is approximated using mercury intrusion porosimetry. An algorithm is developed to incorporate all these experimental data in one geometric representation. Upon validation of pore size distribution against gas adsorption and mercury intrusion porosimetry data, reconstructed ionomer size distribution is reported. In addition, transport related characteristics and effective properties are computed by performing simulations on the hybrid microstructure.

  9. C-3 Substituted Lawsonemonoximates of Holmium(III): Synthesis, Characterization, and Antimicrobial Activity

    OpenAIRE

    S. B. Jagtap; S G Joshi; Litake, G. M.; Ghole, V. S.; Kulkarni, B. A.

    2000-01-01

    A series of five new metal complexes of Ho(III) with C-3 substituted derivatives of lawsonemonexime (2-hydroxy-1,4-naphthalenediene-1-oxime) were synthesized. The compounds were characterized by melting point, elemental analysis, IR spectroscopy and magnetic susceptibility. The antimicrobial activity of the compounds were determined by disk diffusion method and broth micro-dilution techniques using Mueller Hinton medium against the following organisms: S. aureus ATCC 6538P, Klebsiella pneumon...

  10. First structurally characterized mixed-halogen nickel(III) NCN-pincer complex.

    Science.gov (United States)

    Kozhanov, Konstantin A; Bubnov, Michael P; Cherkasov, Vladimir K; Fukin, Georgy K; Vavilina, Nina N; Efremova, Larisa Yu; Abakumov, Gleb A

    2009-03-01

    A square-pyramidal mixed-halogen nickel(III) NCN-pincer complex (PipeNCN)NiClBr (where PipeNCN=2,6-bis(piperidinomethyl)phenyl) was structurally characterized. Bromine occupies apical position; pincer ligand and chlorine atom are in the basal plane. EPR detects that complex in solution exists as a mixture of two structural isomers with bromine or chlorine atoms in the top of pyramid.

  11. Microstructure characterization of erosion resistant coatings on carbon-bonded carbon fibre composites.

    Science.gov (United States)

    Moskalewicz, T; Smeacetto, F; Salvo, M; Boccaccini, A R; Czyrska-Filemonowicz, A

    2010-03-01

    The microstructure of as received and surface treated carbon-bonded carbon fibre composites has been examined by light microscopy, scanning and transmission electron microscopy. The microstructure of the as received material consists of a bonded together layered carbon fiber network, identified as graphitic carbon (hexagonal close packed). To improve the erosion resistance of the carbon-bonded carbon fibre composites composite, the SiC and silicate glass-ceramic coatings from the system SiO(2)-Al(2)O(3)-Y(2)O(3) were produced on carbon-bonded carbon fibre composites composites by a low-cost slurry technique. Transmission electron microscopy investigations of cross-section thin foils allowed for detailed analysis of the coatings microstructure. It was found that the SiC coating was consisting mainly of a nanocrystalline SiC (fcc). The multilayered glass-ceramic coating showed a complex microstructure consisting of an external SiO(2)-Al(2)O(3)-Y(2)O(3) layer and an intermediate nanocrystalline SiC layer. The SiO(2)-Al(2)O(3)-Y(2)O(3) layer was composed of SiO(2) (fcc), Y(2)Si(2)O(7) (op) and Al(4.644)Si(1.357)O(9.68) (op).

  12. The analysis of bainitic ferrite microstructure in microalloyed plate steels through quantitative characterization of intervariant boundaries

    Energy Technology Data Exchange (ETDEWEB)

    Kang, Singon, E-mail: sikang@mines.edu [Advanced Steel Processing and Products Research Center, Colorado School of Mines, Golden, CO 80401 (United States); Speer, John G.; Regier, Ryan W. [Advanced Steel Processing and Products Research Center, Colorado School of Mines, Golden, CO 80401 (United States); Nako, Hidenori [Advanced Steel Processing and Products Research Center, Colorado School of Mines, Golden, CO 80401 (United States); Materials Research Laboratory, Kobe Steel Ltd., Kobe, Hyogo 651-2271 (Japan); Kennett, Shane C. [Advanced Steel Processing and Products Research Center, Colorado School of Mines, Golden, CO 80401 (United States); Exponent Failure Analysis Associates, Menlo Park, CA 94025 (United States); Findley, Kip O. [Advanced Steel Processing and Products Research Center, Colorado School of Mines, Golden, CO 80401 (United States)

    2016-07-04

    Electron backscatter diffraction (EBSD) measurements were performed to investigate the bainitic ferrite microstructure in low-carbon, microalloyed steels with varying C and Mn contents. Fully austenitized samples were isothermally heat treated at temperatures ranging from 450 to 550 °C to form bainitic ferrite. The bainitic ferrite microstructures and boundary characteristics obtained from the EBSD measurements were analyzed based on an inferred Kurdjumov-Sachs (K-S) orientation relationship. The heat treated samples exhibit a microstructure composed of laths and the lath aspect ratio tends to increase at lower isothermal heat treatment temperatures. High fractions of boundary misorientation angles below 5° are observed, which are due to lath boundaries in the microstructure. Additionally, misorientations of approximately 7°, 53° and 60° are observed, which are related to the sub-block, packet, and block boundaries, respectively. With decreasing isothermal heat treatment temperature, there is an increase of block boundaries; these boundaries are intervariant boundaries between different blocks within a packet, most of which have the misorientation angle of 60°. The specimens with a higher carbon level contained increased length of block boundaries, whereas the addition of Mn moderated the dependence of block boundary length on the heat treatment temperature within the experimental temperature range. Meanwhile, the length of intervariant boundaries of both packet and sub-block character did not vary much with heat treatment temperature and alloy composition.

  13. Microstructural characterization of autogenous laser welds on 316L stainless steel using EBSD and EDS.

    Science.gov (United States)

    Kell, J; Tyrer, J R; Higginson, R L; Thomson, R C

    2005-02-01

    This research is concerned with autogenous welding of 316L stainless steel and the microstructure generated by such a process. Autogenous welding does not require a filler material and in this case relies on an initial shallow melt phase to maintain a conduction limited weld. Essentially, a high power laser beam traverses the substrate, with the beam shaped by conventional optics, which produces a Gaussian irradiance distribution; or with a diffractive optical element, used to produce a uniform irradiance distribution. Initial results have shown that due to the nature of the heating cycle, complex microstructures are developed. These fine, complicated microstructures cannot be satisfactorily resolved and quantified using standard optical microscopy techniques. Electron backscatter diffraction (EBSD) and energy dispersive spectroscopy (EDS) have been carried out on a number of different microstructures prepared using a range of welding parameters. It is demonstrated that the simultaneous determination of the chemistry and crystallography is a very useful tool for rapid identification of the different phases formed on solidification as a consequence of varying welding procedures.

  14. Microstructural characterization of AISI 431 martensitic stainless steel laser-deposited coatings

    NARCIS (Netherlands)

    Hemmati, I.; Ocelik, V.; De Hosson, J. Th. M.

    High cooling rates during laser cladding of stainless steels may alter the microstructure and phase constitution of the claddings and consequently change their functional properties. In this research, solidification structures and solid state phase transformation products in single and multi layer

  15. Quantitative Microstructural Characterization of Thick Aluminum Plates Heavily Deformed Using Equal Channel Angular Extrusion

    DEFF Research Database (Denmark)

    Mishin, Oleg; Segal, V.M.; Ferrasse, S.

    2012-01-01

    A detailed quantitative analysis of the microstructure has been performed in three orthogonal planes of 15-mm-thick aluminum plates heavily deformed via two equal channel angular extrusion (ECAE) routes. One route was a conventional route A with no rotation between passes. Another route involved ...

  16. Microstructural characterization of Co-based coating deposited by low power pulse laser cladding

    NARCIS (Netherlands)

    Farnia, A.; Ghaini, F. Malek; Ocelik, V.; De Hosson, J. Th. M.

    A detailed microstructural study of Stellite 6 coating deposited on a low carbon ferritic steel substrate using preplaced powder method and low power Nd:YAG pulse laser is performed. The grain structure and solidification texture of the coating are investigated by orientation imaging microscopy

  17. Characterization of microstructures using contour tree connectivity for fluid flow analysis

    Science.gov (United States)

    Aydogan, Dogu Baran; Hyttinen, Jari

    2014-01-01

    Quantifying the connectivity of material microstructures is important for a wide range of applications from filters to biomaterials. Currently, the most used measure of connectivity is the Euler number, which is a topological invariant. Topology alone, however, is not sufficient for most practical purposes. In this study, we use our recently introduced connectivity measure, called the contour tree connectivity (CTC), to study microstructures for flow analysis. CTC is a new structural connectivity measure that is based on contour trees and algebraic graph theory. To test CTC, we generated a dataset composed of 120 samples and six different types of artificial microstructures. We compared CTC against the Euler parameter (EP), the parameter for connected pairs, the nominal opening dimension (dnom) and the permeabilities estimated using direct pore scale modelling. The results show that dnom is highly correlated with permeability (R2 = 0.91), but cannot separate the structural differences. The groups are best classified with feature combinations that include CTC. CTC provides new information with a different connectivity interpretation that can be used to analyse and design materials with complex microstructures. PMID:24671931

  18. [Microstructure morphology and flocculation mechanism of the decolorizing flocculant poly-aluminum (III)-magnesium (II)-sulfate].

    Science.gov (United States)

    Sang, Yi-min; Chang, Xue-hong; Che, Yue; Gu, Qing-bao

    2013-09-01

    Crystal structures and morphologic characteristics of poly-aluminum (III)-magnesium (II)-sulfate (PMAS) were discussed using X-radial diffraction and infrared spectrogram and the flocculation mechanism was explored here based on comparisons between decolorization effect of landfill leachate secondary effluent and the system Zeta potential. The results indicated that PMAS was a kind of macromolecular composite polymer of aluminum and magnesium based on -OH bonding. The flocculation mechanism of PMAS was mainly charge neutralization and co-precipitation netting. Charge neutralization was the main mechanism at low dose. Its flocculation behaviors were different along with different pH of wastewater at high doses, namely, it was mainly charge neutralization at low pH and co-precipitation netting at high pH and both of them work together at neutral condition.

  19. Nanoscale Three-Dimensional Microstructural Characterization of an Sn-Rich Solder Alloy Using High-Resolution Transmission X-Ray Microscopy (TXM)

    Energy Technology Data Exchange (ETDEWEB)

    Kaira, Chandrashekara S.; Mayer, Carl R.; De Andrade, V.; De Carlo, Francesco; Chawla, Nikhilesh

    2016-07-18

    Abstract

    Three-dimensional (3D) nondestructive microstructural characterization was performed using full-field transmission X-ray microscopy on an Sn-rich alloy, at a spatial resolution of 60 nm. This study highlights the use of synchrotron radiation along with Fresnel zone plate optics to perform absorption contrast tomography for analyzing nanoscale features of fine second phase particles distributed in the tin matrix, which are representative of the bulk microstructure. The 3D reconstruction was also used to quantify microstructural details of the analyzed volume.

  20. Characterizing the Effects of Washing by Different Detergents on the Wavelength-Scale Microstructures of Silk Samples Using Mueller Matrix Polarimetry

    Directory of Open Access Journals (Sweden)

    Yang Dong

    2016-08-01

    Full Text Available Silk fibers suffer from microstructural changes due to various external environmental conditions including daily washings. In this paper, we take the backscattering Mueller matrix images of silk samples for non-destructive and real-time quantitative characterization of the wavelength-scale microstructure and examination of the effects of washing by different detergents. The 2D images of the 16 Mueller matrix elements are reduced to the frequency distribution histograms (FDHs whose central moments reveal the dominant structural features of the silk fibers. A group of new parameters are also proposed to characterize the wavelength-scale microstructural changes of the silk samples during the washing processes. Monte Carlo (MC simulations are carried out to better understand how the Mueller matrix parameters are related to the wavelength-scale microstructure of silk fibers. The good agreement between experiments and simulations indicates that the Mueller matrix polarimetry and FDH based parameters can be used to quantitatively detect the wavelength-scale microstructural features of silk fibers. Mueller matrix polarimetry may be used as a powerful tool for non-destructive and in situ characterization of the wavelength-scale microstructures of silk based materials.

  1. Characterizing the Effects of Washing by Different Detergents on the Wavelength-Scale Microstructures of Silk Samples Using Mueller Matrix Polarimetry.

    Science.gov (United States)

    Dong, Yang; He, Honghui; He, Chao; Zhou, Jialing; Zeng, Nan; Ma, Hui

    2016-08-10

    Silk fibers suffer from microstructural changes due to various external environmental conditions including daily washings. In this paper, we take the backscattering Mueller matrix images of silk samples for non-destructive and real-time quantitative characterization of the wavelength-scale microstructure and examination of the effects of washing by different detergents. The 2D images of the 16 Mueller matrix elements are reduced to the frequency distribution histograms (FDHs) whose central moments reveal the dominant structural features of the silk fibers. A group of new parameters are also proposed to characterize the wavelength-scale microstructural changes of the silk samples during the washing processes. Monte Carlo (MC) simulations are carried out to better understand how the Mueller matrix parameters are related to the wavelength-scale microstructure of silk fibers. The good agreement between experiments and simulations indicates that the Mueller matrix polarimetry and FDH based parameters can be used to quantitatively detect the wavelength-scale microstructural features of silk fibers. Mueller matrix polarimetry may be used as a powerful tool for non-destructive and in situ characterization of the wavelength-scale microstructures of silk based materials.

  2. Design of an expert system based on neuro-fuzzy inference analyzer for on-line microstructural characterization using magnetic NDT method

    Energy Technology Data Exchange (ETDEWEB)

    Ghanei, S., E-mail: Sadegh.Ghanei@yahoo.com [Department of Materials Engineering, Faculty of Engineering, Ferdowsi University of Mashhad, Azadi Square, Mashhad (Iran, Islamic Republic of); Vafaeenezhad, H. [Centre of Excellence for High Strength Alloys Technology (CEHSAT), School of Metallurgical and Materials Engineering, Iran University of Science and Technology (IUST), Narmak, Tehran (Iran, Islamic Republic of); Kashefi, M. [Department of Materials Engineering, Faculty of Engineering, Ferdowsi University of Mashhad, Azadi Square, Mashhad (Iran, Islamic Republic of); Eivani, A.R. [Centre of Excellence for High Strength Alloys Technology (CEHSAT), School of Metallurgical and Materials Engineering, Iran University of Science and Technology (IUST), Narmak, Tehran (Iran, Islamic Republic of); Mazinani, M. [Department of Materials Engineering, Faculty of Engineering, Ferdowsi University of Mashhad, Azadi Square, Mashhad (Iran, Islamic Republic of)

    2015-04-01

    Tracing microstructural evolution has a significant importance and priority in manufacturing lines of dual-phase steels. In this paper, an artificial intelligence method is presented for on-line microstructural characterization of dual-phase steels. A new method for microstructure characterization based on the theory of magnetic Barkhausen noise nondestructive testing method is introduced using adaptive neuro-fuzzy inference system (ANFIS). In order to predict the accurate martensite volume fraction of dual-phase steels while eliminating the effect and interference of frequency on the magnetic Barkhausen noise outputs, the magnetic responses were fed into the ANFIS structure in terms of position, height and width of the Barkhausen profiles. The results showed that ANFIS approach has the potential to detect and characterize microstructural evolution while the considerable effect of the frequency on magnetic outputs is overlooked. In fact implementing multiple outputs simultaneously enables ANFIS to approach to the accurate results using only height, position and width of the magnetic Barkhausen noise peaks without knowing the value of the used frequency. - Highlights: • New NDT system for microstructural evaluation based on MBN using ANFIS modeling. • Sensitivity of magnetic Barkhausen noise to microstructure changes of the DP steels. • Accurate prediction of martensite by feeding multiple MBN outputs simultaneously. • Obtaining the modeled output without knowing the amount of the used frequency.

  3. Microstructural characterization, optical and photocatalytic properties of bilayered CuO and ZnO based thin films

    Energy Technology Data Exchange (ETDEWEB)

    Sáenz-Trevizo, A.; Amézaga-Madrid, P.; Pizá-Ruiz, P.; Solís-Canto, O.; Ornelas-Gutiérrez, C.; Pérez-García, S.; Miki-Yoshida, M., E-mail: mario.miki@cimav.edu.mx

    2014-12-05

    Highlights: • High quality bilayered Zn–Cu oxide thin films were deposited by aerosol assisted CVD. • Detailed microstructural characterization was performed by XRD and electron microscopy. • Absorbance of bilayered films shows a shift of absorption edge toward visible region. • Optical band gap or nearly 3.2 and 2 eV was determined for ZnO and Cu oxide. • High photocatalytic activity around 90% was obtained for bilayered samples. - Abstract: In this work, it is presented the synthesis, microstructural characterization and photocatalytic properties of bilayered CuO–ZnO/ZnO thin films onto borosilicate glass and fused silica substrates. The films were deposited by aerosol assisted chemical vapor deposition, using an experimental setup reported elsewhere. Deposition conditions were optimized to get high quality films; i.e. they were structurally uniform, highly transparent, non-light scattering, homogeneous, and well adhered to the substrate. Different Cu/Zn atomic ratios were tried for the upper layer. The microstructure of the films was characterized by grazing incidence X-ray diffraction (GIXRD), scanning electron microscopy (SEM), high resolution transmission electron microscopy (HRTEM) and X-ray photoelectron spectroscopy. GIXRD results indicate the presence of ZnO Wurzite and Cu oxide phases. Results of SEM and HRTEM analysis of the cross sectional microstructure showed that the films were composed of compact and dense layers with no visible evidence of an interfacial boundary or porosity. Optical absorbance of the bilayered films showed a clear shift of the absorption toward the visible range. Optical band gap was determined roughly at 3.2 and 2 eV for ZnO and Cu oxide, respectively. Photocatalytic activity of the samples, for the degradation of a 10{sup −5} mol dm{sup −3} solution of methylene blue (MB), was determined after 120 and 240 min of irradiation with an UV-A source. Around 90% of MB degradation was reached by bilayered films with

  4. Early Age Characterization and Microstructural Features of Sustainable Binder Systems for Concrete

    Science.gov (United States)

    Vance, Kirk

    Concrete is the most widely used infrastructure material worldwide. Production of Portland cement, the main binding component in concrete, has been shown to require significant energy and account for approximately 5-7% of global carbon dioxide production. The expected continued increased use of concrete over the coming decades indicates this is an ideal time to implement sustainable binder technologies. The current work aims to explore enhanced sustainability concretes, primarily in the context of limestone and flow. Aspects such as hydration kinetics, hydration product formation and pore structure add to the understanding of the strength development and potential durability characteristics of these binder systems. Two main strategies for enhancing this sustainability are explored in this work: (i) the use of high volume limestone in combination with other alternative cementitious materials to decrease the Portland cement quantity in concrete and (ii) the use of geopolymers as the binder phase in concrete. The first phase of the work investigates the use of fine limestone as cement replacement from the perspective of hydration, strength development, and pore structure. The nature of the potential synergistic benefit of limestone and alumina will be explored. The second phase will focus on the rheological characterization of these materials in the fresh state, as well as a more general investigation of the rheological characterization of suspensions. The results of this work indicate several key ideas. (i) There is a potential synergistic benefit for strength, hydration, and pore structure by using alumina and in Portland limestone cements, (ii) the limestone in these systems is shown to react to some extent, and fine limestone is shown to accelerate hydration, (iii) rheological characteristics of cementitious suspensions are complex, and strongly dependent on several key parameters including: the solid loading, interparticle forces, surface area of the particles

  5. Synthesis, microstructural characterization and optical properties of CuO nanorods and nanowires obtained by aerosol assisted CVD

    Energy Technology Data Exchange (ETDEWEB)

    Lugo-Ruelas, M. [Centro de Investigación en Materiales Avanzados S.C., Laboratorio Nacional de Nanotecnología, Miguel de Cervantes No. 120, Chihuahua, Chih. C.P. 31109 (Mexico); Universidad Autónoma de Chihuahua, Facultad de Ingeniería, Circuito No. 1, Nuevo Campus Universitario, Apdo. Postal 1552, Chihuahua, Chih. C.P. 31240 (Mexico); Amézaga-Madrid, P. [Centro de Investigación en Materiales Avanzados S.C., Laboratorio Nacional de Nanotecnología, Miguel de Cervantes No. 120, Chihuahua, Chih. C.P. 31109 (Mexico); Esquivel-Pereyra, O. [Centro de Investigación en Materiales Avanzados S.C., Laboratorio Nacional de Nanotecnología, Miguel de Cervantes No. 120, Chihuahua, Chih. C.P. 31109 (Mexico); Universidad Autónoma de Chihuahua, Facultad de Ingeniería, Circuito No. 1, Nuevo Campus Universitario, Apdo. Postal 1552, Chihuahua, Chih. C.P. 31240 (Mexico); Antúnez-Flores, W.; Pizá-Ruiz, P.; Ornelas-Gutiérrez, C. [Centro de Investigación en Materiales Avanzados S.C., Laboratorio Nacional de Nanotecnología, Miguel de Cervantes No. 120, Chihuahua, Chih. C.P. 31109 (Mexico); Miki-Yoshida, M., E-mail: mario.miki@cimav.edu.mx [Centro de Investigación en Materiales Avanzados S.C., Laboratorio Nacional de Nanotecnología, Miguel de Cervantes No. 120, Chihuahua, Chih. C.P. 31109 (Mexico)

    2015-09-15

    Highlights: • Nanorods and nanowires of CuO were successfully synthesized by AACVD technique. • The carrier gas velocity was a determinant factor for the growth of nanorods or nanowires. • The increase of deposition time generates the reduction in the evenness and distribution density. • The crystalline phase of nanorods and nanowires was monoclinic tenorite. - Abstract: Copper oxide is a particularly interesting material because it presents photovoltaic, electrochemical and catalytic properties. Its unique properties are very important in the area of nanotechnology and may be an advantage because these nanomaterials can be applied in the design and manufacture of nanosensors, photocatalysis area, nanolasers switches and transistors. Nowadays one-dimensional nanostructures as nanorods, nanowires, etc., have generated a great importance and have received considerable attention and study due to their unique physical and chemical properties. In this work we report the synthesis, microstructural characterization and optical properties of CuO nanorods and nanowires grown by aerosol assisted chemical vapor deposition onto a CuO, ZnO and TiO{sub 2} thin film covered and bare borosilicate glass substrate. Concentration of the precursor solution and carrier gas flux were previously optimized and fixed at 0.1 mol dm{sup −3} and 5 L min{sup −1}, respectively. Other deposition parameters such as substrate temperature, as well the carrier gas velocity and deposition time were varied from 623 to 973 K, 0.88 to 1.77 m s{sup −1} and 11 to 16 min, respectively. Their influence on the morphology, microstructure and optical properties of the nanorods and nanowires were analyzed. The crystalline structure of the materials was characterized by grazing incidence X-ray diffraction; results indicate the presence of the tenorite phase. Surface morphology and microstructure were studied by field emission scanning electron microscopy, and high resolution transmission electron

  6. Microstructural Characterization for Structural Health Monitoring of Heat-Resisting Rotor Steels

    Energy Technology Data Exchange (ETDEWEB)

    Kim, C. S.; Byeon, J. W.; Park, I. K. [Seoul National University of Technology, Seoul (Korea, Republic of)

    2008-04-15

    The typical heat-resisting rotor steels such as 2.25CrMo, 9CrMo and 12CrW steel were experimentally studied in order to understand their materials degradation under high temperature and pressure during the long-term service, and then use the basic studies for the structural health monitoring. In order to monitor the materials degradation, it was conducted by the isothermal aging for 2.25CrMo steel, creep-fatigue for 9CrMo steel and creep for 12Cr steel with the incremental step test. The ultrasonic wave properties, electrical resistivity and coercivity were interpreted in relation to microstructural changes at each material and showed strong sensitivity to the specific microstructural evolution

  7. Mueller matrix polarimetry for characterizing microstructural variation of nude mouse skin during tissue optical clearing.

    Science.gov (United States)

    Chen, Dongsheng; Zeng, Nan; Xie, Qiaolin; He, Honghui; Tuchin, Valery V; Ma, Hui

    2017-08-01

    We investigate the polarization features corresponding to changes in the microstructure of nude mouse skin during immersion in a glycerol solution. By comparing the Mueller matrix imaging experiments and Monte Carlo simulations, we examine in detail how the Mueller matrix elements vary with the immersion time. The results indicate that the polarization features represented by Mueller matrix elements m22&m33&m44 and the absolute values of m34&m43 are sensitive to the immersion time. To gain a deeper insight on how the microstructures of the skin vary during the tissue optical clearing (TOC), we set up a sphere-cylinder birefringence model (SCBM) of the skin and carry on simulations corresponding to different TOC mechanisms. The good agreement between the experimental and simulated results confirm that Mueller matrix imaging combined with Monte Carlo simulation is potentially a powerful tool for revealing microscopic features of biological tissues.

  8. Microstructural Characterization of Melt Extracted High-Nb-Containing TiAl-Based Fiber

    Directory of Open Access Journals (Sweden)

    Shuzhi Zhang

    2017-02-01

    Full Text Available The microstructure of melt extracted Ti-44Al-8Nb-0.2W-0.2B-1.5Si fiber were investigated. When the rotation speed increased from 2000 to 2600 r/min, the appearance of the wire was uniform with no Rayleigh-wave default. The structure was mainly composed of fine α2 (α phase dendritic crystal and a second phase between dendrite arms and grain boundaries. The precipitated second phases were confirmed to be Ti5Si3 from the eutectic reaction L→Ti5Si3 + α and TiB. As the lower content of Si and higher cooling rate, a divorced eutectic microstructure was obtained. Segregation of Ti, Nb, B, Si, and Al occurred during rapid solidification.

  9. Microstructural Characterization Of Laser Heat Treated AISI 4140 Steel With Improved Fatigue Behavior

    Directory of Open Access Journals (Sweden)

    Oh M.C.

    2015-06-01

    Full Text Available The influence of surface heat treatment using laser radiation on the fatigue strength and corresponding microstructural evolution of AISI 4140 alloy steel was investigated in this research. The AISI 4140 alloy steel was radiated by a diode laser to give surface temperatures in the range between 600 and 800°C, and subsequently underwent vibration peening. The fatigue behavior of surface-treated specimens was examined using a giga-cycle ultrasonic fatigue test, and it was compared with that of non-treated and only-peened specimens. Fatigue fractured surfaces and microstructural evolution with respect to the laser treatment temperatures were investigated using an optical microscope. Hardness distribution was measured using Vickers micro-hardness. Higher laser temperature resulted in higher fatigue strength, attributed to the phase transformation.

  10. Characterization of hot spots in microstructured reactors for fast and exothermic reactions in mixing regime

    OpenAIRE

    Haber, Julien; Kashid, Madhavanand N.; Borhani, Navid; Jiang, Bo; Maeder, Thomas; Thome, John Richard; Renken, Albert; Kiwi-Minsker, Lioubov

    2012-01-01

    The intensification of fast exothermic reactions can be achieved by using microstructured reactors (MSR) which provide improved mass & heat transfer rates leading to higher overall reaction kinetics. But for highly exothermic reactions the heat evacuation becomes not efficient enough and unwanted hot spots are formed. In this study, first the mixing in MSR is quantified for different geometries and then temperature profiles are measured using a novel quantitative IR-thermometry method. The re...

  11. Phase and Micro-Structural Characterization of Sanitary-Ware Fired at Different Temperature

    OpenAIRE

    ATHER HASSAN; YASEEN IQBAL; SYED ZAFAR ILYAS

    2017-01-01

    The three main ingredients of sanitary-ware are clay, feldspar and quartz. This ware is being widely used and has therefore, attracted the attention of researchers from time to time. Consequently, it has been extensively investigated. The present study describes the phase and micro-structural analysis of sanitary-ware samples collected from local (Durr Ceramics Peshawar) industry. XRD (X-Ray Diffraction) of samples fired at 1100oC reveals the presence of ? ? ? ? ?-quartz and primary mullite o...

  12. Synthesis, characterization, hydrolase and catecholase activity of a dinuclear iron(III) complex: Catalytic promiscuity.

    Science.gov (United States)

    Camargo, Tiago P; Maia, Fernanda F; Chaves, Cláudia; de Souza, Bernardo; Bortoluzzi, Adailton J; Castilho, Nathalia; Bortolotto, Tiago; Terenzi, Hernán; Castellano, Eduardo E; Haase, Wolfgang; Tomkowicz, Zbigniew; Peralta, Rosely A; Neves, Ademir

    2015-05-01

    Herein, we report the synthesis and characterization of the new di-iron(III) complex [(bbpmp)(H2O)(Cl)Fe(III)(μ-Ophenoxo)Fe(III)(H2O)Cl)]Cl (1), with the symmetrical ligand 2,6-bis{[(2-hydroxybenzyl)(pyridin-2-yl)methylamino]methyl}-4-methylphenol (H3bbpmp). Complexes 2 with the unsymmetrical ligand H2bpbpmp - {2-[[(2-hydroxybenzyl)(2-pyridylmethyl)]aminomethyl]-6-bis(pyridylmethyl) aminomethyl}-4-methylphenol and 3 with the ligand L(1)=4,11-dimethyl-1,8-bis{2-[N-(di-2-pyridylmethyl)amino]ethyl}cyclam were included for comparison purposes. Complex 1 was characterized through elemental analysis, X-ray crystallography, magnetochemistry, electronic spectroscopy, electrochemistry, mass spectrometry and potentiometric titration. The magnetic data show a very weak antiferromagnetic coupling between the two iron centers of the dinuclear complex 1 (J=-0.29cm(-1)). Due to the presence of labile coordination sites in both iron centers the hydrolysis of both the diester model substrate 2,4-BDNPP and DNA was studied in detail. Complex 1 was also able to catalyze the oxidation of the substrate 3,5-di-tert-butylcatechol (3,5-DTBC) to give the corresponding quinone, and thus it can be considered as a catalytically promiscuous system. Copyright © 2015 Elsevier Inc. All rights reserved.

  13. Microstructural characterization of alumina-zirconia layered ceramics using positron annihilation spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Parente, P., E-mail: pparente@fis.uc3m.es [Departamento de Fisica, Universidad Carlos III de Madrid, 28911 Leganes (Spain); Ortega, Y. [Departamento de Fisica de Materiales, Facultad de Ciencias Fisicas, Univ. Complutense de Madrid, 28040 Madrid (Spain); Savoini, B.; Monge, M.A. [Departamento de Fisica, Universidad Carlos III de Madrid, 28911 Leganes (Spain); Tucci, A.; Esposito, L. [Centro Ceramico Bologna, 40128 Bologna (Italy); Sanchez-Herencia, A.J. [Instituto de Ceramica y Vidrio, Consejo Superior de Investigaciones Cientificas, 28049 Madrid (Spain)

    2010-05-15

    Positron annihilation spectroscopy (PAS), indentation, nanoindentation experiments and scanning electron microscopy (SEM) observations were performed on Al{sub 2}O{sub 3}-ZrO{sub 2} laminates samples to assess the effect of residual stresses on their mechanical and microstructural properties. Layered samples were implemented by slip-casting, constituted by two thin Al{sub 2}O{sub 3} external layers and an intermediate thick one, consisting of a mixture of Al{sub 2}O{sub 3} and monoclinic ZrO{sub 2} in the range 0-30 vol.%. In these systems residual tensile stresses fields were generated inside the external layers during cooling from the sintering temperature, by the expansion of the adjacent ZrO{sub 2}-containing layer. SEM observations showed the microstructural effects due to the level of tension related to the zirconia content. A correlation between the PAS parameters and the microstructural changes caused by the presence of residual stresses was found. Nanoindentation measurements were used to trace the sign and magnitude of the residual stress gradient across the interface between the layers.

  14. Microstructure characterization of oxidation of aluminized coating prepared by a combined process

    Science.gov (United States)

    Liu, H. B.; Tao, J.; Xu, J.; Chen, Z. F.; Sun, X. J.; Xu, Z.

    2008-08-01

    Alumina layer is a good candidate for the tritium penetration barrier that is important in the control of tritium losses due to permeation through structural materials used in high-temperature gas-cooled reactors and in fusion reactors. This paper describes the microstructure of the oxide film of the tritium penetration barrier formed on 316L stainless steel, which was prepared by a combined process, namely, aluminizing and oxidizing treatments using a double glow plasma technology. Microstructure and phase structure of the coatings investigated were examined by scanning electronic microscope (SEM), X-ray diffraction analysis (XRD) and transmission electron microscopy (TEM), respectively. The chemical composition and the chemical states of Al, O elements in the oxidation film were identified by X-ray photoelectron spectroscopy (XPS). After aluminization, the typical microstructure of the coating mainly consisted of an outer high aluminum-containing intermetallic compound layer (Fe 2Al 5 and FeAl) and intermediate ferritic stainless steel (α Fe(Al))layer followed by the austenitic substrate. After the combined process, an oxide layer that consisted of Al 2O 3 and spinel FeAl 2O 4 had been successfully formed on the aluminizing coating surface, with an amorphous outmost surface and an underlying subsurface nanocrystalline structure.

  15. Mechanical properties, fracture surface characterization, and microstructural analysis of six noble dental casting alloys.

    Science.gov (United States)

    Ucar, Yurdanur; Brantley, William A; Johnston, William M; Dasgupta, Tridib

    2011-06-01

    Because noble dental casting alloys for metal ceramic restorations have a wide range of mechanical properties, knowledge of these properties is needed for rational alloy selection in different clinical situations where cast metal restorations are indicated. The purpose of this study was to compare the mechanical properties and examine both the fracture and polished surfaces of 6 noble casting alloys that span many currently marketed systems. Five alloys were designed for metal ceramic restorations, and a sixth Type GPT has Type IV alloy for fixed prosthodontics (Maxigold KF) was included for comparison. Specimens (n=6) meeting dimensional requirements for ISO Standards 9693 and 8891 were loaded to failure in tension using a universal testing machine at a crosshead speed of 2 mm/min. Values of 0.1% and 0.2% yield strength, ultimate tensile strength, elastic modulus, and percentage elongation were obtained. Statistical comparisons of the alloy mechanical properties were made using 1-way ANOVA and the REGW multiple-range test (α=.05). Following fracture surface characterization using scanning electron microscopy (SEM), specimens were embedded in epoxy resin, polished, and again, examined with the SEM. When the multiple comparisons were considered, there were generally no significant differences in the elastic modulus, 0.1% and 0.2% offset yield strength, and ultimate tensile strength for the d.SIGN 91 (Au-Pd), d.SIGN 59 (Pd-Ag), Capricorn 15 (Pd-Ag-Au) and Maxigold KF (Au-Ag-Pd) alloys, except that the ultimate tensile strength was significantly lower (PGold XH (Au-Pt). The d.SIGN 59 (14.6%) and Capricorn 15 (13.8%) alloys had the highest values of mean percentage elongation, which were not significantly different. Aquarius XH (6.0%) and Maxigold KF (4.2%) had the lower mean values of percentage elongation, which were also not significantly different. The polished and etched surfaces for all alloys revealed equiaxed, fine-grain microstructures, and all fracture

  16. Characterization of the lanthanum(III) and europium(III) trichloroacetate complexes extracted with 18-crown-6

    Energy Technology Data Exchange (ETDEWEB)

    Imura, H.; Saito, Y.; Ohashi, K. [Ibaraki Univ., Mito (Japan); Meguro, Y.; Yoshida, Z. [Japan Atomic Energy Research Inst., Tokai (Japan); Choppin, G.R. [Florida State Univ., Tallahassee, FL (United States)

    1996-08-01

    Extraction of lanthanide(III) ions with 18-crown-6 (18C6) and trichloroacetate (tca) has been studied. The composition, hydration, and structure of the La(III) and Eu(III) complexes extracted into 1,2-dichloroethane were investigated by using several methods such as the liquid-liquid distribution technique, conductimetry, Karl Fisher titration, laser luminescence spectroscopy, and {sup 1}H NMR. The La(III) complex was found to be a monohydrate, La(tca){sub 3}(18C6)(H{sub 2}O), while that of Eu(III) was a mixture of a monohydrate and a dihydrate, i.e., Eu(tca){sub 3}(18C6)(H{sub 2}O) and Eu(tca){sub 3}(18C6)(H{sub 2}O){sub 2}. The origin of the selectivity by 18C6 which gives much higher extractability of La(III) than of Eu(III) is explained by considering the hydration and probable structure of their complexes. 12 refs., 5 figs., 4 tabs.

  17. Synthesis and characterization of dihexyldithiocarbamate as a chelating agent in extraction of gold(III)

    Energy Technology Data Exchange (ETDEWEB)

    Fatimah, Soja Siti, E-mail: soja-sf@upi.edu [Departemen Pendidikan Kimia, Universitas Pendidikan Indonesia, Jl. Dr. Setiabudhi No. 229, Bandung 40154 (Indonesia); Department of Chemistry, Faculty of Mathematics and Natural Sciences, Padjadjaran University, Jl. Raya Bandung-Sumedang, Km. 21, Jatinangor (Indonesia); Bahti, Husein H.; Hastiawan, Iwan [Department of Chemistry, Faculty of Mathematics and Natural Sciences, Padjadjaran University, Jl. Raya Bandung-Sumedang, Km. 21, Jatinangor (Indonesia); Permanasari, Anna [Departemen Pendidikan Kimia, Universitas Pendidikan Indonesia, Jl. Dr. Setiabudhi No. 229, Bandung 40154 (Indonesia)

    2016-02-08

    The use of dialkyldithiocarbamates as chelating agents of transition metals have been developing for decades. Many chelating agents have been synthesized and used in the extraction of the metals. Studies on particular aspects of extraction of the metals, such as the effect of increasing hydrophobicity of chelating agents on the effectiveness of the extraction, have been done. However, despite the many studies on the synthesis and applications of this type of chelating agents, interests in the aspect of molecular structure of the synthesized ligands and of their complexes, have been limited. This study aimed at synthesizing and characterizing dihexylthiocarbamate, and using the ligand for the extraction of gold III). Characterization of the ligand and of its metal complex were done by using elemental analysis, DTG, and spectroscopic methods to include NMR, ({sup 1}H, and {sup 13}C), FTIR, and MS-ESI. Data on the synthesis, characterization, and the application of the ligand as a chelating agent are presented.

  18. Threading dislocation density characterization in III-V photovoltaic materials by electron channeling contrast imaging

    Science.gov (United States)

    Yaung, Kevin Nay; Kirnstoetter, Stefan; Faucher, Joseph; Gerger, Andy; Lochtefeld, Anthony; Barnett, Allen; Lee, Minjoo Larry

    2016-11-01

    Accurate and rapid threading dislocation density (TDD) characterization of III-V photovoltaic materials using electron channeling contrast imaging (ECCI) is demonstrated. TDDs measured using ECCI showed close agreement with those from electron beam-induced current mapping (EBIC) and defect selective etching (DSE). ECCI is shown to be well-suited for measuring TDD values over a range of 5×106-5×108 cm-2. ECCI can distinguish individual dislocations in clusters closer than 0.2 μm, highlighting its excellent spatial resolution compared to DSE and EBIC. Taken together, ECCI is shown to be a versatile and complementary method to rapidly quantify TDD in III-V solar cells.

  19. Fractal analysis of SEM images and mercury intrusion porosimetry data for the microstructural characterization of microcrystalline cellulose-based pellets

    Energy Technology Data Exchange (ETDEWEB)

    Gomez-Carracedo, A.; Alvarez-Lorenzo, C.; Coca, R.; Martinez-Pacheco, R.; Concheiro, A. [Departamento de Farmacia y Tecnologia Farmaceutica, Universidad de Santiago de Compostela, Santiago de Compostela 15782 (Spain); Gomez-Amoza, J.L. [Departamento de Farmacia y Tecnologia Farmaceutica, Universidad de Santiago de Compostela, Santiago de Compostela 15782 (Spain)], E-mail: joseluis.gomez.amoza@usc.es

    2009-01-15

    The microstructure of theophylline pellets prepared from microcrystalline cellulose, carbopol and dicalcium phosphate dihydrate, according to a mixture design, was characterized using textural analysis of gray-level scanning electron microscopy (SEM) images and thermodynamic analysis of the cumulative pore volume distribution obtained by mercury intrusion porosimetry. Surface roughness evaluated in terms of gray-level non-uniformity and fractal dimension of pellet surface depended on agglomeration phenomena during extrusion/spheronization. Pores at the surface, mainly 1-15 {mu}m in diameter, determined both the mechanism and the rate of theophylline release, and a strong negative correlation between the fractal geometry and the b parameter of the Weibull function was found for pellets containing >60% carbopol. Theophylline mean dissolution time from these pellets was about two to four times greater. Textural analysis of SEM micrographs and fractal analysis of mercury intrusion data are complementary techniques that enable complete characterization of multiparticulate drug dosage forms.

  20. Characterization of Co(III) EDTA-Reducing Bacteria in Metal- and Radionuclide-Contaminated Groundwater

    Energy Technology Data Exchange (ETDEWEB)

    Gao, Weimin [Arizona State University; Gentry, Terry J [ORNL; Mehlhorn, Tonia L [ORNL; Carroll, Sue L [ORNL; Jardine, Philip M [ORNL; Zhou, Jizhong [University of Oklahoma, Norman

    2010-01-01

    The Waste Area Grouping 5 (WAG5) site at Oak Ridge National Laboratory has a potential to be a field site for evaluating the effectiveness of various bioremediation approaches and strategies. The site has been well studied in terms of its geological and geochemical properties over the past decade. However, despite the importance of microorganisms in bioremediation processes, the microbiological populations at the WAG5 site and their potential in bioremediation have not been similarly evaluated. In this study, we initiated research to characterize the microbial populations in WAG5 groundwater. Approximately 100 isolates from WAG5 groundwater were isolated and selected based on colony morphology. Fifty-five unique isolates were identified by BOX-PCR and subjected to further characterization. 16S rRNA sequences indicated that these isolates belong to seventeen bacterial genera including Alcaligenes (1 isolate), Aquamonas (1), Aquaspirillum (1), Bacillus (10), Brevundimonas (5), Caulobacter (7), Dechloromonas (2), Janibacter (1), Janthinobacterium (2), Lactobacillus (1), Paenibacillus (4), Pseudomonas (9), Rhodoferax (1), Sphingomonas (1), Stenotrophomonas (6), Variovorax (2), and Zoogloea (1). Metal respiration assays identified several isolates, which phylogenically belong or are close to Caulobacter, Stenotrophomonas, Bacillus, Paenibacillus and Pseudomonas, capable of reducing Co(III)EDTA- to Co(II)EDTA{sup 2-} using the defined M1 medium under anaerobic conditions. In addition, using WAG5 groundwater directly as the inoculants, we found that organisms associated with WAG5 groundwater can reduce both Fe(III) and Co(III) under anaerobic conditions. Further assays were then performed to determine the optimal conditions for Co(III) reduction. These assays indicated that addition of various electron donors including ethanol, lactate, methanol, pyruvate, and acetate resulted in metal reduction. These experiments will provide useful background information for future

  1. Characterization of competitive binding of Eu(III)/Cu(II) and Eu(III)/Ca(II) to Gorleben humic acid

    Energy Technology Data Exchange (ETDEWEB)

    Marang, L.; Reiller, P.E. [CEA Saclay, Lab Speciat Radionucledies and Mol, DEN, DANS, DPC, SECR, 91 - Gif sur Yvette (France); Marang, L.; Benedetti, M.F. [Univ Paris Diderot, Lab Geochim Eaux, IPGP, F-75251 Paris 05 (France); Marang, L.; Benedetti, M.F. [CNRS, UMR 71574, F-75251 Paris 05 (France); Eidner, S.; Kumke, M. [Univ Potsdam, Inst Chem, D-14476 Potsdam (Germany)

    2009-06-15

    Complete text of publication follows: In an area that contains high concentrations of natural organic matter, it is expected to play an important role on the speciation of trivalent radionuclides. Competitive interactions with H{sup +} and major cations, e.g. Ca{sup 2+} or Mg{sup 2+}, could influence these metals transport and bioavailability. Competitive experiments between Eu{sup 3+} and cations which can bind differently to humic substances, would bring an improved understanding of the competitive mechanisms. The aim of this study is to acquire data for Eu(III)/Cu(II) and Eu(III)/Ca(II) competitive binding to a sedimentary-originated humic acid (Gorleben, Germany). The NICA-Donnan parameters [1] for Ca(II), Cu(II), and Eu(III) obtained from competitive binding experiments using Ca{sup 2+} or Cu{sup 2+} ion selective electrodes (ISE), were used to model time-resolved luminescence spectroscopy (TRLS) measurements. Then the TRL spectra and decay times were interpreted to check the consistency of the modelling. From ISE data, Eu(III) and Cu(II) are in direct competition for the same type of sites, whereas Ca(II) has an indirect influence through electrostatic binding. The spectroscopic interpretation of the competition experiments showed two strikingly different environments for the Eu(III)/Cu(II) and Eu(III)/Ca(II) systems. Cu(II) seems to expel more effectively Eu(III) into an aqueous like environment within the humic acid structure, i.e., the Donnan phase, and to the aqueous phase as free Eu{sup 3+}. This is evidenced both from the spectra as well as from the decrease in the luminescence decay times. Moreover, Ca(II) causes a slighter modification of the chemical environment of the humic-complexed Eu(III). [1] Kinniburgh et al. (1999) Colloids Surf. A 151, 147-166

  2. Growth and characterization of manganese doped III-V heterostructures; Herstellung und Charakterisierung von Mangan dotierten III-V Halbleiterheterostrukturen

    Energy Technology Data Exchange (ETDEWEB)

    Wurstbauer, Ursula

    2008-04-15

    Subject of this thesis is the growth of III-V heterostructures doped with manganese by means of molecular beam epitaxy (MBE). The characterization was done primarily by magnetotransport measurements in the temperature range from 300 K to 20 mK and fields up to 19 T. Two different kind of Mn doped materials, ferromagnetic GaMnAs layers and Mn modulation doped magnetic two dimensional hole systems were studied. The first part focuses on the enhancement of the electric and magnetic properties of ferromagnetic properties and the integration of GaMnAs layers in more sophisticated heterostructures. Therefore, the crystal quality and the influence of the buffer layer beneath the magnetic layer are crucial. The MBE-growth of ferromagnetic GaMnAs layers on (001), (311)A and (311)A was successfully achieved with present values of the Curie-temperature (TC). Additionally, the growth of ferromagnetic GaMnAs layers on nonpolar (110) substrates and on cleaved [110] edges was established. An application of the latter was the investigation of magnetic bipolar junctions. Magnetic two dimensional hole gases (M2DHG) has been realized by the use of In0.75Al0.25As/In0.75Ga0.25As/InAs quantum well (QW) structures. It is necessary to grow a buffer layer for strain relaxation due to the lattice mismatch by gradually increasing the In mole fraction. Magnetotransport measurements were carried out on Si doped two-dimensional electron gases (2DEG) and on Mn doped M2DHGs. From magnetotransport measurements on the M2DHGs we see some interesting features, in particular in the mK region. From the 2DEGs and all non inverted doped M2DEGs weak localization and weak antilocalization effects can be observed in the low field region. Whereas all M2DHGs with an inverted doping layer show strong localization effects and a metal insulator transition dependent on the applied magnetic field perpendicular to the QW. In the high field region Shubnikov-de-Haas oscillations in the longitudinal resistance and

  3. Electrical properties and microstructural characterization of Ni/Ta contacts to n-type 6H-SiC

    Science.gov (United States)

    Zhou, Tian-Yu; Liu, Xue-Chao; Huang, Wei; Zhuo, Shi-Yi; Zheng, Yan-Qing; Shi, Er-Wei

    2015-12-01

    A Ni/Ta bilayer is deposited on n-type 6H-SiC and then annealed at different temperatures to form an ohmic contact. The electrical properties are characterized by I-V curve measurement and the specific contact resistance is extracted by the transmission line method. The phase formation and microstructure of the Ni/Ta bilayer are studied after thermal annealing. The crystalline and microstructure properties are analyzed by using glance incident x-ray diffraction (GIXRD), Raman spectroscopy, and transmission electron microscopy. It is found that the transformation from the Schottky to the Ohmic occurs at 1050 °C and the GIXRD results show a distinct phase change from Ta2C to TaC at this temperature. A specific contact resistance of 6.5× 10-5 Ω·cm2 is obtained for sample Ni(80 nm)/Ta(20 nm)/6H-SiC after being annealed at 1050 °C. The formation of the TaC phase is regarded as the main reason for the excellent Ohmic properties of the Ni/Ta contacts to 6H-SiC. Raman and TEM data reveal that the graphite carbon is drastically consumed by the Ta element, which can improve the contact thermal stability. A schematic diagram is proposed to illustrate the microstructural changes of Ni/Ta/6H-SiC when annealed at different temperatures. Project supported by the Innovation Program of the Chinese Academy of Sciences (Grant No. KJCX2-EW-W10), the Shanghai Rising-star Program, China (Grant No. 13QA1403800), the Industry-Academic Joint Technological Innovations Fund Project of Jiangsu Province, China (Grant No. BY2011119), and the National High-tech Research and Development Program of China (Grant Nos. 2013AA031603 and 2014AA032602).

  4. Characterization of the microstructure in random and textured polycrystals and single crystals by diffraction line profile analysis

    Energy Technology Data Exchange (ETDEWEB)

    Ribarik, Gabor [Department of Materials Physics, Eoetvoes University Budapest, Pazmany Peter setany 1/A, H-1117 Budapest (Hungary); Ungar, Tamas, E-mail: ungar@ludens.elte.hu [Department of Materials Physics, Eoetvoes University Budapest, Pazmany Peter setany 1/A, H-1117 Budapest (Hungary)

    2010-11-25

    Research highlights: {yields} X-ray or neutron line profile analysis becomes a powerful tool to characterize dislocation structures, crystallite size, size-distribution and planar faults when diffraction patterns are constructed by the bottom-up approach following physical principles. {yields} The microstructure of archaeological specimens can tell about the manufacturing technologies used by our ancestors. {yields} Burger vector and slip system types operating in grains of polycrystal enable to understand plastic response in structural materials and geological minerals. {yields} The type and frequency of twinning in hexagonal materials is essential to understand the durability of key engineering materials in energy production. - Abstract: X-ray or neutron diffraction patterns are simulated by convoluting defect specific profile functions based on continuum theory of elasticity. The defect related profile functions are controlled by the physically mandatory minimum number of parameters: the dislocation density, {rho}, the dislocation arrangement parameter, M, one or more parameters describing strain anisotropy where their number depends on the crystal symmetry, the median, m and the logarithmic variance, {sigma} of the log-normal size distribution function, and finally the density of stacking faults, {alpha} or the frequency of twin boundaries, {beta}. These parameters are, at the same time, among the most relevant physical parameters describing the microstructure of crystalline materials. The theoretical diffraction patterns are produced by the convolution of the defect related, physically based profile functions in the 'extended Convolutional Multiple Whole Profile' (eCMWP) software package. The usage of the software package is demonstrated by the microstructure determination in randomly-textured and textured polycrystalline and single crystals specimens of different materials.

  5. Advanced Microstructural Characterization for Development of Improved HgCdTe Detectors and Devices

    Science.gov (United States)

    2014-09-21

    used, bulk CdZnTe substrates. Initiation of ZnTe growth on the Si(211) substrates, as well as the microstructure of the CdTe(211)B/ ZnTe/ Si(211... CdZnTe substrates. It has been proposed that HgCdSe could provide performance similar to HgCdTe in terms of its IR material properties, with the added...using molecular beam epitaxy (MBE) because Si-based substrates offer several strategic advantages relative to the commonly-used, bulk CdZnTe

  6. Spectroscopic approach in characterization of chromium(III), manganese(II), iron(III) and copper(II) complexes with a nitrogen donor tetradentate, 14-membered azamacrocyclic ligand.

    Science.gov (United States)

    Chandra, Sulekh; Gupta, Lokesh Kumar

    2005-07-01

    The complexes of Cr(III), Mn(II), Fe(III) and Cu(II) were synthesized with the macrocyclic ligand i.e. 2,3,9,10-tetraketo-1,4,8,11-tetraazacyclotetradecane. The ligand was prepared by the [2 + 2] condensation reaction of diethyloxalate and 1,3-diamino propane. These complexes were found to have the general composition M(L)X3 and M'(L)X2 [where M = Mn(II) and Cu(II), M' = Cr(III) and Fe(III), L = ligand (N4) and X = Cl-, NO3-, 1/2SO4(2-) and [CH3COO-]. The ligand and its transition metal complexes were characterized by the elemental analyses, molar conductance, magnetic susceptibility, mass, IR, electronic, and EPR spectral studies. On the basis of IR, electronic and EPR spectral studies an octahedral geometry has been assigned for Cr(III), Mn(II) and Fe(III) and a tetragonal geometry for Cu(II) complexes.

  7. Spectroscopic approach in characterization of chromium(III), manganese(II), iron(III) and copper(II) complexes with a nitrogen donor tetradentate, 14-membered azamacrocyclic ligand

    Science.gov (United States)

    Chandra, Sulekh; Gupta, Lokesh Kumar

    2005-07-01

    The complexes of Cr(III), Mn(II), Fe(III) and Cu(II) were synthesized with the macrocyclic ligand i.e. 2,3,9,10-tetraketo-1,4,8,11-tetraazacyclotetradecane. The ligand was prepared by the [2 + 2] condensation reaction of diethyloxalate and 1,3-diamino propane. These complexes were found to have the general composition M(L)X 3 and M'(L)X 2 [where M = Mn(II) and Cu(II), M' = Cr(III) and Fe(III), L = ligand (N 4) and X = Cl -, NO 3-, 1/2SO 42- and [CH 3COO -]. The ligand and its transition metal complexes were characterized by the elemental analyses, molar conductance, magnetic susceptibility, mass, IR, electronic, and EPR spectral studies. On the basis of IR, electronic and EPR spectral studies an octahedral geometry has been assigned for Cr(III), Mn(II) and Fe(III) and a tetragonal geometry for Cu(II) complexes.

  8. Thermo-mechanical and micro-structural characterization of shape memory polymer foams

    Science.gov (United States)

    di Prima, Matthew Allen

    The need for a set of design criteria, models, and limits for the use of shape memory polymer foams was proposed. The effect of temperature and strain on the mechanical behavior; compression, tensile, cyclic compression, constrained recovery, and free strain recovery of the material was used to determine the operational limits of the material. Next, the damage mechanism and viscoelastic effects in compressive cycling were determined through further mechanical testing and with the incorporation of three dimensional structure mapping via micro-CT scanning. The influence of microstructure was determined by testing the basic thermomechanical, viscoelactic, and shape recovery behavior of foams with relative densities of 20, 30, and 40 percent. A similar suite of tests were then performed with the base epoxy material to generate the material properties for computational modeling. This data was then combined with three dimensional microstructures generated from micro-CT scans to develop material models for shape memory foams. These models were then validated by comparing model results to the experimental results under similar conditions.

  9. Fabrication, microstructural characterization and wear characteristics of A380 alloy-alumina composites

    KAUST Repository

    Nurani, Sheikh Jaber

    2016-03-10

    To obtain better mechanical and tribological properties than aluminium alloys aluminium is reinforced with alumina particles making aluminium metal matrix composites. In this work scrap piston A380 alloy was used as the matrix alloy. Alumina particles were added by 5%, 10% and 15% into matrix alloy respectively to form desired composites by stir casting technique. Pin on disc wear testing machine with counter surface as steel disc of hardness HRC 32 and surface roughness of 0.62 μm was used to conduct the wear test. In result composites showed superior wear resistance property over A380 alloy. The effect of load, sliding speed and sliding distance on wear behaviour were also examined in this study. Wear mechanism was identified from the worn surface. Both optical and scanning electron microscope (SEM) of the composites was performed to determine the microstructures. Optical micrograph shows grain size decreases with addition of alumina particles. EDS analysis was performed to confirm the presence of α-Al matrix, primary Si particles and intermetallic. As a general method, phase compositions were analyzed by using a scanning electron microscope (SEM) equipped with an energy dispersive spectroscopy (EDS). Optical microstructures were consistent with the SEM micrographs. © 2015 IEEE.

  10. Characterizing microstructural changes of skeletal muscle tissues using spectral transformed Mueller matrix polarization parameters

    Science.gov (United States)

    He, Chao; He, Honghui; Chang, Jintao; Ma, Hui

    2016-03-01

    Polarization imaging techniques are recognized as potentially powerful tools to detect the structural changes of biological tissues. Meanwhile, spectral features of the scattered light can also provide abundant microstructural information, therefore can be applied in biomedical studies. In this paper, we adopt the polarization reflectance spectral imaging to analyze the microstructural changes of hydrolyzing skeletal muscle tissues. We measure the Mueller matrix, which is a comprehensive description of the polarization properties, of the bovine skeletal muscle samples in different periods of time, and analyze its behavior using the multispectral Mueller matrix transformation (MMT) technique. The experimental results show that for bovine skeletal muscle tissues, the backscattered spectral MMT parameters have different values and variation features at different stages. We can also find the experimental results indicate that the stages of hydrolysis for bovine skeletal muscle samples can be judged by the spectral MMT parameters. The results presented in this work show that combining with the spectral technique, the MMT parameters have the potential to be used as tools for meat quality detection and monitoring.

  11. Microstructural Characterization of Red Mud as Affected by Inorganic and Organic Chemicals Permeation

    Science.gov (United States)

    Rubinos, David A.; Valcárcel, Víctor; Spagnoli, Giovanni; Barral, María Teresa

    2017-09-01

    The microstructural characteristics of red mud (RM), especially specific surface area (SSA) and mesoporosity, and the effects of various representative fluids, namely methanol (80% v/v), trichloroethylene (TCE) (1100 mg/L), acetic acid (pH 2), and CaCl2 (5% w/v) aqueous solutions, were studied using N2-gas adsorption. The effect of compaction was also assessed. RM powder exhibited a moderate Brunauer-Emmet-Teller (BET)-SSA and is mostly a mesoporous (large mesopores, 200-500 Å) and a macroporous material. Compaction affected the macro and large, but not the fine, mesopores. Among the fluids, CaCl2 and acetic acid induced notable and opposing changes in RM microstructural characteristics. CaCl2 decreased SSA and suppressed fine mesoporosity, whereas acetic acid greatly enhanced them. Fractal analysis further indicated increasing surface roughness and heterogeneity of pore structure during acid exposure, altogether envisaging an improvement of adsorption capacity and a decrease of permeability of the RM.

  12. Microstructure and Corrosion Characterization of Squeeze Cast AM50 Magnesium Alloys

    Science.gov (United States)

    Sachdeva, Deepika; Tiwari, Shashank; Sundarraj, Suresh; Luo, Alan A.

    2010-12-01

    Squeeze casting of magnesium alloys potentially can be used in lightweight chassis components such as control arms and knuckles. This study documents the microstructural analysis and corrosion behavior of AM50 alloys squeeze cast at different pressures between 40 and 120 MPa and compares them with high-pressure die cast (HPDC) AM50 alloy castings and an AM50 squeeze cast prototype control arm. Although the corrosion rates of the squeeze cast samples are slightly higher than those observed for the HPDC AM50 alloy, the former does produce virtually porosity-free castings that are required for structural applications like control arms and wheels. This outcome is extremely encouraging as it provides an opportunity for additional alloy and process development by squeeze casting that has remained relatively unexplored for magnesium alloys compared with aluminum. Among the microstructural parameters analyzed, it seems that the β-phase interfacial area, indicating a greater degree of β network, leads to a lower corrosion rate. Weight loss was the better method for determining corrosion behavior in these alloys that contain a large fraction of second phase, which can cause perturbations to an overall uniform surface corrosion behavior.

  13. Characterization of the Microstructures and the Cryogenic Mechanical Properties of Electron Beam Welded Inconel 718

    Science.gov (United States)

    Kwon, Soon Il; Bae, Sang Hyun; Do, Jeong Hyeon; Jo, Chang Yong; Hong, Hyun Uk

    2016-02-01

    The microstructures and the cryogenic mechanical properties of electron beam (EB) welds between cast and forged Inconel 718 superalloys with a thickness of 10 mm were investigated in comparison with gas tungsten arc (GTA) welds. EB welding with a heat input lower than 250 J/mm caused the formation of liquation microfissuring in the cast-side heat-affected-zone (HAZ) of the EB welds. HAZ liquation microfissuring appeared to be associated with the constitutional liquation of primary NbC carbides at the grain boundaries. Compared with the GTA welding process, the EB welding produced welds with superior microstructure, exhibiting fine dendritic structure associated with the reduction in size and fraction of the Laves phase due to the rapid cooling rate. This result was responsible for the superior mechanical properties of the EB welds at 77 K (-196 °C). Laves particles in both welds were found to provide the preferential site for the crack initiation and propagation, leading to a significant decrease in the Charpy impact toughness at 77 K (-196 °C). Crack initiation and propagation induced by Charpy impact testing were discussed in terms of the dendrite arm spacing, the Laves size and the dislocation structure ahead of the crack arisen from the fractured Laves phase in the two welds.

  14. Characterizing microstructural features of biomedical samples by statistical analysis of Mueller matrix images

    Science.gov (United States)

    He, Honghui; Dong, Yang; Zhou, Jialing; Ma, Hui

    2017-03-01

    As one of the salient features of light, polarization contains abundant structural and optical information of media. Recently, as a comprehensive description of polarization property, the Mueller matrix polarimetry has been applied to various biomedical studies such as cancerous tissues detections. In previous works, it has been found that the structural information encoded in the 2D Mueller matrix images can be presented by other transformed parameters with more explicit relationship to certain microstructural features. In this paper, we present a statistical analyzing method to transform the 2D Mueller matrix images into frequency distribution histograms (FDHs) and their central moments to reveal the dominant structural features of samples quantitatively. The experimental results of porcine heart, intestine, stomach, and liver tissues demonstrate that the transformation parameters and central moments based on the statistical analysis of Mueller matrix elements have simple relationships to the dominant microstructural properties of biomedical samples, including the density and orientation of fibrous structures, the depolarization power, diattenuation and absorption abilities. It is shown in this paper that the statistical analysis of 2D images of Mueller matrix elements may provide quantitative or semi-quantitative criteria for biomedical diagnosis.

  15. Characterization of microstructure and properties of AlCuMg alloys

    Directory of Open Access Journals (Sweden)

    Zlatičanin Biljana V.

    2003-01-01

    Full Text Available The effect of magnesium content, in the interval range from 1 mass.% to 5 mass.%, on the microstructure and properties of aluminium - copper magnesium alloys was examined. The as-cast structure was modified by the addition of the AlTi5B1 to give alloys containing 0 to 0.25 mass. % titanium. Using X-ray powder diffraction we established that the tetragonal intermetallic compound Al2Cu and orthorhombic intermetallic compound Al2CuMg are formed across the whole range of magnesium additions. The effect of the magnesium and titanium content on the microstructure was monitored quantitatively. Using automatic image analysis we were able to measure the linear intercept grain size, the secondary dendrite arm spacing (DAS, the size of eutectic cells (Le, as well as the size distribution and volume fractions of the α-solid solution and the eutectic. In alloys containing high magnesium the average values of the DAS and grain size were found to decrease. Also, in alloys containing high magnesium the average values of the eutectic cell length and volume fractions of the eutectic were found to increase. The changes in chemical composition of the alloy cause changes in the structure that are reflected in the Brinell hardness and the compression strength. Compression strength and hardness increase with the content of magnesium and titanium.

  16. Microstructural characterization of Y{sub 2}O{sub 3} ODS-Fe-Cr model alloys

    Energy Technology Data Exchange (ETDEWEB)

    Castro, V. de [Department of Materials, University of Oxford, Oxford OX1 3PH (United Kingdom)], E-mail: vanessa.decastro@materials.ox.ac.uk; Leguey, T.; Munoz, A.; Monge, M.A.; Pareja, R. [Departamento de Fisica, Universidad Carlos III de Madrid, 28911 Leganes (Spain); Marquis, E.A.; Lozano-Perez, S.; Jenkins, M.L. [Department of Materials, University of Oxford, Oxford OX1 3PH (United Kingdom)

    2009-04-30

    Two Fe-12 wt% Cr alloys, one containing 0.4 wt% Y{sub 2}O{sub 3} and the other Y{sub 2}O{sub 3}-free, have been produced by mechanical alloying followed by hot isostatic pressing. These oxide dispersion strengthened and reference alloys were characterized both in the as-HIPed state and after tempering by transmission electron microscopy and atom-probe tomography. The as-HIPed alloys exhibited the characteristic microstructure of lath martensite and contained a high density of dislocations. Small voids with sizes <10 nm were also observed. Both alloys also contained M{sub 3}C and M{sub 23}C{sub 6} carbides (M = Cr, Fe) probably as a result of C ingress during milling. After tempering at 1023 K for 4 h the microstructures had partially recovered. In the recovered regions, martensite laths were replaced by equiaxed grains in which M{sub 23}C{sub 6} carbides decorated the grain boundaries. In the ODS alloy nanoparticles containing Y were commonly observed within grains, although they were also present at grain boundaries and adjacent to large carbides.

  17. Microstructural and Microchemical Characterization of Dual Step Aged Alloy X-750 and its Relationship to Environmentally Assisted Cracking

    Energy Technology Data Exchange (ETDEWEB)

    G.A. Young; N. Lewis; M. Hanson; W. Matuszyk; B. Wiersma; S. Gonzalez

    2001-05-08

    When exposed to deaerated high purity water, Alloy X-750 is susceptible to both high temperature (> 249 C) intergranular stress corrosion cracking (IGSCC) and intergranular low temperature (< 149 C) fracture (LTF). However, the microstructural and microchemical factors that govern environmentally assisted cracking (EAC) susceptibility are poorly understood. The present study seeks to characterize the grain boundary microstructure and microchemistry in order to gain a better mechanistic understanding of stress corrosion crack initiation, crack growth rate, and low temperature fracture. Light microscopy, scanning electron microscopy, transmission electron microscopy, orientation imaging microscopy, scanning Auger microscopy, and thermal desorption spectroscopy were performed on selected heats of Alloy X-750 AH. These data were correlated to EAC tests performed in 338 C deaerated water. Results show that grain boundary MC-type [(Ti,Nb)C] carbides and increased levels of grain boundary phosphorus correlate with an increase in LTF susceptibility but have little effect on the number of initiation sites or the SCC crack growth rate. Thermal desorption data show that multiple hydrogen trapping states exist in Alloy X-750 condition AH. Moreover, it appears that exposure to high temperature (> 249 C), hydrogen deaerated water increases the hydrogen concentration in strong hydrogen trap states and degrades the resistance of the material to low temperature fracture. These findings are consistent with a hydrogen embrittlement based mechanism of LTF where intergranular fracture occurs ahead of a crack tip and is exacerbated by phosphorus segregation to grain boundaries and grain boundary hydrogen trap states.

  18. Use of Vegetable Waste Extracts for Controlling Microstructure of CuO Nanoparticles: Green Synthesis, Characterization, and Photocatalytic Applications

    Directory of Open Access Journals (Sweden)

    Hameed Ullah

    2017-01-01

    Full Text Available Chemical syntheses involve either hazardous reactants or byproducts which adversely affect the environment. It is, therefore, desirable to develop synthesis processes which either do not involve hazardous reactants or consume all the reactants giving no byproducts. We have synthesized CuO nanoparticles (NPs adhering to some of the principles of green chemistry. The CuO NPs have been synthesized exploiting extracts of vegetable wastes, that is, Cauliflower waste and Potatoes and Peas peels. The extracts were aimed to work as capping agents to get control over the microstructure and morphology of the resulting CuO NPs. The green synthesized CuO NPs were characterized to explore the microstructure, morphology, optical bandgaps, and photocatalytic performances. XRD revealed that the CuO NPs of all the samples crystallized in a single crystal system, that is, monoclinic. However, the morphologies and the optical bandgaps energies varied as a function of the extract of vegetable waste. Similarly, the CuO NPs obtained through different extracts have shown different photocatalytic activities. The CuO NPs produced with extract of Cauliflower have shown high degradation of MB (96.28% compared to obtained with Potatoes peels (87.37% and Peas peels (79.11%.

  19. Ultrasonic Sensor Signals and Optimum Path Forest Classifier for the Microstructural Characterization of Thermally-Aged Inconel 625 Alloy

    Directory of Open Access Journals (Sweden)

    Victor Hugo C. de Albuquerque

    2015-05-01

    Full Text Available Secondary phases, such as laves and carbides, are formed during the final solidification stages of nickel-based superalloy coatings deposited during the gas tungsten arc welding cold wire process. However, when aged at high temperatures, other phases can precipitate in the microstructure, like the γ'' and δ phases. This work presents an evaluation of the powerful optimum path forest (OPF classifier configured with six distance functions to classify background echo and backscattered ultrasonic signals from samples of the inconel 625 superalloy thermally aged at 650 and 950 \\(^\\circ\\C for 10, 100 and 200 h. The background echo and backscattered ultrasonic signals were acquired using transducers with frequencies of 4 and 5 MHz. The potentiality of ultrasonic sensor signals combined with the OPF to characterize the microstructures of an inconel 625 thermally aged and in the as-welded condition were confirmed by the results. The experimental results revealed that the OPF classifier is sufficiently fast (classification total time of 0.316 ms and accurate (accuracy of 88.75% and harmonic mean of 89.52 for the application proposed.

  20. Ultrasonic sensor signals and optimum path forest classifier for the microstructural characterization of thermally-aged inconel 625 alloy.

    Science.gov (United States)

    de Albuquerque, Victor Hugo C; Barbosa, Cleisson V; Silva, Cleiton C; Moura, Elineudo P; Filho, Pedro P Rebouças; Papa, João P; Tavares, João Manuel R S

    2015-05-27

    Secondary phases, such as laves and carbides, are formed during the final solidification stages of nickel-based superalloy coatings deposited during the gas tungsten arc welding cold wire process. However, when aged at high temperatures, other phases can precipitate in the microstructure, like the γ'' and δ phases. This work presents an evaluation of the powerful optimum path forest (OPF) classifier configured with six distance functions to classify background echo and backscattered ultrasonic signals from samples of the inconel 625 superalloy thermally aged at 650 and 950 °C for 10, 100 and 200 h. The background echo and backscattered ultrasonic signals were acquired using transducers with frequencies of 4 and 5 MHz. The potentiality of ultrasonic sensor signals combined with the OPF to characterize the microstructures of an inconel 625 thermally aged and in the as-welded condition were confirmed by the results. The experimental results revealed that the OPF classifier is sufficiently fast (classification total time of 0.316 ms) and accurate (accuracy of 88.75%" and harmonic mean of 89.52) for the application proposed.

  1. Microstructural characterization of welded zone for Fe{sub 3}Al/Q235 fusion-bonded joint

    Energy Technology Data Exchange (ETDEWEB)

    Ma Haijun [Key Lab of Liquid Structure and Heredity of Materials, Ministry of Education, Shandong University, Jinan 250061, Shandong Province, Jing Shi Road 73, Shandong (China)], E-mail: hjma123@mail.sdu.edu.cn; Li Yajiang [Key Lab of Liquid Structure and Heredity of Materials, Ministry of Education, Shandong University, Jinan 250061, Shandong Province, Jing Shi Road 73, Shandong (China); Material Science Department, Bauman Moscow State Technical University, Moscow 105005 (Russian Federation); Puchkov, U.A. [Material Science Department, Bauman Moscow State Technical University, Moscow 105005 (Russian Federation); Wang Juan [Key Lab of Liquid Structure and Heredity of Materials, Ministry of Education, Shandong University, Jinan 250061, Shandong Province, Jing Shi Road 73, Shandong (China)

    2008-12-20

    The microstructural characterization of Fe{sub 3}Al/Q235 welded zone were analysed to investigate the welding behavior of Fe{sub 3}Al intermetallic. The results indicated that a crack-free Fe{sub 3}Al/Q235 joint was obtained when Cr25-Ni13 alloy was adopted as the filler metal. The microstructure of the welded zone presented different morphology due to the severe fluctuation of Al, Ni, Mn and Cr elements near the fusion zone. The fish-bone like structures in Q235 side fusion zone were composed of {alpha}-Fe(Cr, Al, Ni) solid solutions. Fe{sub 3}Al/Q235 joint fractured in the Fe{sub 3}Al HAZ, and shear strength of 533.33 MPa was achieved. The fracture mode of Fe{sub 3}Al side fracture surface was mainly transgranular cleavage, occured along [1 1 1] orientation on {l_brace}1 1 0{r_brace} planes. And the Q235 side fracture surface was in intergranular and quasi-cleavage mode. The phase relations of {gamma} and {alpha} in Fe{sub 3}Al side fusion zone, constituent of lower bainite in the weld and the Fe{sub 3}Al ordered transformation in HAZ were also determined.

  2. Synthesis, Characterization, and Antimicrobial and Antispermatogenic Activity of Bismuth(III) and Arsenic(III) Derivatives of Biologically Potent Nitrogen and Sulfur Donor Ligands

    OpenAIRE

    Latika Dawara; S. C. Joshi; Singh, R. V.

    2012-01-01

    A series of Bi(III) and As(III) complexes with two N∩S donor ligands, 1-(4-chloro-2-oxo-2H-chromen-3-yl)-methylene)-thiosemicarbazide (L1H) and N′-[1-(2-oxo-2H-chrome-3yl-ethylidene]-hydrazinecarbodithionic acid benzyl ester (L2H) have been synthesized by the reaction of BiCl3 and Ph3As with ligands in 1 : 1 and 1 : 2 molar ratios. All the synthesized compounds were characterized by elemental analyses, melting point determinations, and a combination of electronic, IR, 1H NMR, 13C NMR spectro...

  3. Synthesis, Characterization, and Antimicrobial and Antispermatogenic Activity of Bismuth(III) and Arsenic(III) Derivatives of Biologically Potent Nitrogen and Sulfur Donor Ligands

    OpenAIRE

    Dawara, Latika; S. C. Joshi; Singh, R. V.

    2012-01-01

    A series of Bi(III) and As(III) complexes with two N∩S donor ligands, 1-(4-chloro-2-oxo-2H-chromen-3-yl)-methylene)-thiosemicarbazide (L1H) and N′-[1-(2-oxo-2H-chrome-3yl-ethylidene]-hydrazinecarbodithionic acid benzyl ester (L2H) have been synthesized by the reaction of BiCl3 and Ph3As with ligands in 1 : 1 and 1 : 2 molar ratios. All the synthesized compounds were characterized by elemental analyses, melting point determinations, and a combination of electronic, IR, 1H NMR, 13C NMR spectros...

  4. Reductive reactivity of iron(III oxides in the east china sea sediments: characterization by selective extraction and kinetic dissolution.

    Directory of Open Access Journals (Sweden)

    Liang-Jin Chen

    Full Text Available Reactive Fe(III oxides in gravity-core sediments collected from the East China Sea inner shelf were quantified by using three selective extractions (acidic hydroxylamine, acidic oxalate, bicarbonate-citrate buffered sodium dithionite. Also the reactivity of Fe(III oxides in the sediments was characterized by kinetic dissolution using ascorbic acid as reductant at pH 3.0 and 7.5 in combination with the reactive continuum model. Three parameters derived from the kinetic method: m 0 (theoretical initial amount of ascorbate-reducible Fe(III oxides, k' (rate constant and γ (heterogeneity of reactivity, enable a quantitative characterization of Fe(III oxide reactivity in a standardized way. Amorphous Fe(III oxides quantified by acidic hydroxylamine extraction were quickly consumed in the uppermost layer during early diagenesis but were not depleted over the upper 100 cm depth. The total amounts of amorphous and poorly crystalline Fe(III oxides are highly available for efficient buffering of dissolved sulfide. As indicated by the m 0, k' and γ, the surface sediments always have the maximum content, reactivity and heterogeneity of reactive Fe(III oxides, while the three parameters simultaneously downcore decrease, much more quickly in the upper layer than at depth. Albeit being within a small range (within one order of magnitude of the initial rates among sediments at different depths, incongruent dissolution could result in huge discrepancies of the later dissolution rates due to differentiating heterogeneity, which cannot be revealed by selective extraction. A strong linear correlation of the m 0 at pH 3.0 with the dithionite-extractable Fe(III suggests that the m 0 may represent Fe(III oxide assemblages spanning amorphous and crystalline Fe(III oxides. Maximum microbially available Fe(III predicted by the m 0 at pH 7.5 may include both amorphous and a fraction of other less reactive Fe(III phases.

  5. Reductive reactivity of iron(III) oxides in the east china sea sediments: characterization by selective extraction and kinetic dissolution.

    Science.gov (United States)

    Chen, Liang-Jin; Zhu, Mao-Xu; Yang, Gui-Peng; Huang, Xiang-Li

    2013-01-01

    Reactive Fe(III) oxides in gravity-core sediments collected from the East China Sea inner shelf were quantified by using three selective extractions (acidic hydroxylamine, acidic oxalate, bicarbonate-citrate buffered sodium dithionite). Also the reactivity of Fe(III) oxides in the sediments was characterized by kinetic dissolution using ascorbic acid as reductant at pH 3.0 and 7.5 in combination with the reactive continuum model. Three parameters derived from the kinetic method: m 0 (theoretical initial amount of ascorbate-reducible Fe(III) oxides), k' (rate constant) and γ (heterogeneity of reactivity), enable a quantitative characterization of Fe(III) oxide reactivity in a standardized way. Amorphous Fe(III) oxides quantified by acidic hydroxylamine extraction were quickly consumed in the uppermost layer during early diagenesis but were not depleted over the upper 100 cm depth. The total amounts of amorphous and poorly crystalline Fe(III) oxides are highly available for efficient buffering of dissolved sulfide. As indicated by the m 0, k' and γ, the surface sediments always have the maximum content, reactivity and heterogeneity of reactive Fe(III) oxides, while the three parameters simultaneously downcore decrease, much more quickly in the upper layer than at depth. Albeit being within a small range (within one order of magnitude) of the initial rates among sediments at different depths, incongruent dissolution could result in huge discrepancies of the later dissolution rates due to differentiating heterogeneity, which cannot be revealed by selective extraction. A strong linear correlation of the m 0 at pH 3.0 with the dithionite-extractable Fe(III) suggests that the m 0 may represent Fe(III) oxide assemblages spanning amorphous and crystalline Fe(III) oxides. Maximum microbially available Fe(III) predicted by the m 0 at pH 7.5 may include both amorphous and a fraction of other less reactive Fe(III) phases.

  6. Generation and characterization of anisotropic microstructures in rare earth-iron-boron alloys

    Science.gov (United States)

    Oster, Nathaniel

    The automotive industry is currently being directed toward electrification of their fleets. In order to provide these hybrid or electric vehicles, lightweight high torque electric motors are needed. Permanent magnet (PM) brushless motors have been identified as the preferred motors for these applications. In order to effectively provide these motors, cost-effective high strength PMs are needed. The use of polymer bonded PMs is one method to reduce processing costs, but performance is decreased unless anisotropic PMs can be formed. New processing methods to form anisotropic mixed rare earth (MRE)-iron-boron PM particulate were studied in this work. Two primary processing routes were identified and investigated: controlled devitrification through application of uniaxial pressure and rapid directional solidification utilizing a segregating additive. In addition, further control of the melt-spinning process was achieved through control of wheel surface temperature and finish. Controlled devitrification was found to produce an anisotropic, nanocrystalline microstructure, as observed through TEM and XRD studies. A high defect density within the structure, unprecedented in RE2Fe14B microstructures, was observed. It is surmised that the defects cause soft magnetic behavior. Stabilization of a columnar, textured microstructure was achieved through the utilization of moderate wheel speeds during melt-spinning, in combination with minor additions of Ag to the alloy. The texture was seen to be altered from that typically seen in RE2Fe14B alloys melt-spun at low-to-moderate wheel speeds. It was observed that this occurs through a modification in the solidification pathway, catalyzed by the addition of Ag. In addition to the altered texture, the presence of fine precipitates within the matrix and varying interdendritic phases was observed. Alteration of wheel surface temperature and surface finish was seen to have significant effects on the ability to form amorphous material in

  7. Characterization of Carbon-Rich Phases in a Complex Microstructure of a Commercial X80 Pipeline Steel

    Science.gov (United States)

    Morales, E. V.; Bott, I. S.; Silva, R. A.; Morales, A. M.; de Souza, L. F. G.

    2016-07-01

    The wide use of the term M/A constituent conceals many complexities about shape, size, and composition. This work uses metallographic techniques and transmission electron microscopy to characterize the entire microstructure development which is observed during continuous cooling in a commercial X80 pipeline steel. A general model is presented which allows calculating the volume fractions of martensite and retained austenite, as well as their compositions in these carbon-rich phases of the M/A constituent for this commercial pipeline steel. This approach takes into account the allotriomorphic ferrite formation and the massive alloyed carbide precipitation before the acicular ferrite formation. Two morphologies (in the film and blocky forms) of the M/A constituent were registered. The calculated M/A volume fraction resulted in agreement with the fraction of this constituent experimentally obtained through the optical microscopy observations. This allowed the justification of the very small volumetric fraction of the M/A constituent with the film morphology.

  8. Quantitatively characterizing the microstructural features of breast ductal carcinoma tissues in different progression stages by Mueller matrix microscope.

    Science.gov (United States)

    Dong, Yang; Qi, Ji; He, Honghui; He, Chao; Liu, Shaoxiong; Wu, Jian; Elson, Daniel S; Ma, Hui

    2017-08-01

    Polarization imaging has been recognized as a potentially powerful technique for probing the microstructural information and optical properties of complex biological specimens. Recently, we have reported a Mueller matrix microscope by adding the polarization state generator and analyzer (PSG and PSA) to a commercial transmission-light microscope, and applied it to differentiate human liver and cervical cancerous tissues with fibrosis. In this paper, we apply the Mueller matrix microscope for quantitative detection of human breast ductal carcinoma samples at different stages. The Mueller matrix polar decomposition and transformation parameters of the breast ductal tissues in different regions and at different stages are calculated and analyzed. For more quantitative comparisons, several widely-used image texture feature parameters are also calculated to characterize the difference in the polarimetric images. The experimental results indicate that the Mueller matrix microscope and the polarization parameters can facilitate the quantitative detection of breast ductal carcinoma tissues at different stages.

  9. Carbon Contamination During Ion Irradiation - Accurate Detection and Characterization of its Effect on Microstructure of Ferritic/Martensitic Steels

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Jing; Toloczko, Mychailo B.; Kruska, Karen; Schreiber, Daniel K.; Edwards, Danny J.; Zhu, Zihua; Zhang, Jiandong

    2017-11-17

    Accelerator-based ion beam techniques have been used to study radiation effects in materials for decades. Although carbon contamination induced by ion beam in target materials is a well-known issue, it has not been fully characterized nor quantified for studies in ferritic/martensitic (F/M) steels that are candidate materials for applications such as core structural components in advanced nuclear reactors. It is an especially important issue for this class of material because of the effect of carbon level on precipitate formation. In this paper, the ability to quantify carbon contamination using three common techniques, namely time-of-flight secondary ion mass spectroscopy (ToF-SIMS), atom probe tomography (APT) and transmission electron microscopy (TEM) is compared. Their effectiveness and short-comings in determining carbon contamination will be presented and discussed. The corresponding microstructural changes related to carbon contamination in ion irradiated F/M steels are also presented and briefly discussed.

  10. ZK60 alloy processed by ECAP: Microstructural, physical and mechanical characterization

    Energy Technology Data Exchange (ETDEWEB)

    Dumitru, F.-D., E-mail: dianadumitru1986@yahoo.com [Materials Science and Engineering Faculty, Politehnica University of Bucharest, Splaiul Independentei 313, 060042 Bucharest (Romania); Higuera-Cobos, O.F., E-mail: osfahico@gmail.com [Departamento de Ciencia de los Materiales e Ingeniería Metalúrgica, ETSEIB – Universidad Politécnica de Cataluña, Av. Diagonal 647, 08028 Barcelona (Spain); Facultad de Ingeniería Mecánica, Universidad Tecnológica de Pereira, Vereda La Julita, Pereira (Colombia); Cabrera, J.M., E-mail: jose.maria.cabrera@upc.es [Departamento de Ciencia de los Materiales e Ingeniería Metalúrgica, ETSEIB – Universidad Politécnica de Cataluña, Av. Diagonal 647, 08028 Barcelona (Spain); Fundació CTM Centre Tecnológic, Plaça de la Ciència 2, 08243 Manresa (Spain)

    2014-01-31

    Lately, magnesium alloys have been extensively investigated through severe plastic deformation (SPD) methods in order to extend their application to structural components. In the present work, as-extruded ZK60 magnesium alloy samples were subjected to 4 passes of equal-channel angular pressing (ECAP) at a processing temperature of 250 °C, following route Bc. The microstructural evolution of the deformed grains was analyzed using electron back-scattered diffraction (EBSD). The Orientation Imaging Microscopy (OIM) maps, together with the grain boundary misorientation distribution showed a reduction in the grain size accompanied by a large proportion of high angle grain boundaries. Calorimetric analysis showed a slight increase in the recrystallization temperature of the ECAPed magnesium samples. Mechanical tests showed an improvement in the elongation-to-failure after 4 ECAP passes, which were about 2 times higher than in the as-extruded sample. Also a brittle to ductile transition was observed.

  11. Quantitative data analysis methods for 3D microstructure characterization of Solid Oxide Cells

    DEFF Research Database (Denmark)

    Jørgensen, Peter Stanley

    surfaces and allows constraints on the surface curvature to enforce a smooth surface in the segmentation. A high accuracy method is developed for calculating two phase boundary surface areas and triple phase boundary length of triple phase systems. The calculations are based on sub-voxel accuracy...... the microstructure. The methods are exemplied by the analysis of Ni-YSZ and LSC-CGO electrode samples. Automatic methods for preprocessing the raw 3D image data are developed. The preprocessing steps correct for errors introduced by the image acquisition by the focused ion beam serial sectioning. Alignment...... task of manually delineating structures within each image slice or the quality of manual and automatic segmentation schemes. To solve this, a framework for the automatic segmentation of 3D image data is developed. The technique is based on a level set method and uses numerical approximations to partial...

  12. Microstructural characterization and electron backscatter diffraction analysis across the welded interface of duplex stainless steel

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Zhiqiang; Jing, Hongyang [School of Materials Science and Engineering, Tianjin University, Tianjin 300350 (China); Tianjin Key Laboratory of Advanced Joining Technology, Tianjin 300350 (China); Xu, Lianyong, E-mail: xulianyong@tju.edu.cn [School of Materials Science and Engineering, Tianjin University, Tianjin 300350 (China); Tianjin Key Laboratory of Advanced Joining Technology, Tianjin 300350 (China); Han, Yongdian; Gao, Zhanqi; Zhao, Lei [School of Materials Science and Engineering, Tianjin University, Tianjin 300350 (China); Tianjin Key Laboratory of Advanced Joining Technology, Tianjin 300350 (China); Zhang, Jianli [Welding laboratory, Offshore Oil Engineering (Qing Dao) Company, Qing Dao 266520 (China)

    2017-08-15

    Highlights: • Apparent change in LTHAZ was the intergranular secondary austenite precipitation. • Ferrite in HAZ maintained same distribution as ferrite texture in base metal. • Different austenite in different zones showed different orientation with ferrite. • Ferrite and austenite grains exhibited different boundary characteristics. • Local deformations were generated in grain boundary and within deformed grain. - Abstract: The microstructural evolution, orientation relationships, boundary characteristics, grain type, local deformation, and microhardness across the welded interface of duplex stainless steel (DSS) were investigated. The DSS welded joint consisted of four typical zones: base metal (BM), low-temperature heat-affected zone (LTHAZ), high-temperature heat-affected zone (HTHAZ), and weld metal (WM). The apparent microstructural changes in the HTHAZ and LTHAZ were secondary austenite and Cr{sub 2}N precipitation. A modified cooperative precipitation mechanism of secondary austenite and Cr{sub 2}N at the interface was proposed. Furthermore, the ferrite in both the HTHAZ and LTHAZ maintained the same distribution as the ferrite texture in the BM, while this ferrite texture disappeared completely in the WM. Different austenite grains in the different zones exhibited different orientation relationships with the ferrite matrix. Special grain boundaries were mainly distributed between the austenite grains, while the ferrite grains primarily contained random grain boundaries. Austenite twins constituted the largest proportion of the special boundaries. The special austenite grain boundaries in the BM and LTHAZ were higher in relative frequency than those in the HTHAZ and WM. The ferrite grains in the HTHAZ and WM mainly consisted of substructured grains. In the BM, the recrystallization degree of ferrite was significantly lower than that of austenite grains. The local deformations were mainly generated in the grain boundaries and within the deformed

  13. Characterization of microstructural, mechanical and thermophysical properties of Th-52U alloy

    Energy Technology Data Exchange (ETDEWEB)

    Das, Santanu, E-mail: reachoutsantanu@gmail.com [Integrated Fuel Fabrication Facility, Bhabha Atomic Research Centre, Mumbai (India); Kaity, S. [Radiometallurgy Division, Bhabha Atomic Research Centre, Mumbai (India); Kumar, R. [Uranium Extraction Division, Bhabha Atomic Research Centre, Mumbai (India); Banerjee, J. [Radiometallurgy Division, Bhabha Atomic Research Centre, Mumbai (India); Roy, S.B. [Chemical Engineering Group, Bhabha Atomic Research Centre, Mumbai (India); Chaudhari, G.P.; Daniel, B.S.S. [Indian Institute of Technology Roorkee, Roorkee (India)

    2016-11-15

    Th-52 wt.% U alloy has a microstructure featuring interspersed networks of uranium rich and thorium rich phases. Room temperature hardness of the alloy is more than twice that of unalloyed thorium. The alloy age hardens (550 °C) only slightly (peak hardness/hardness of solution heated and quenched = 1.05). Room temperature thermal conductivity (25.6 W m{sup −1} {sup °}C{sup −1}) is close to that of uranium and most of the binary and ternary metallic alloy fuel materials. Average linear coefficient of thermal expansion (CTE) of Th-52 wt.% U alloy [11.2 × 10{sup −06} °C{sup −1} (27–290 °C) and 16.75 × 10{sup −06} °C{sup −1} (27–600 °C)] are comparable with that of many metallic alloy fuel candidates. Th-52 wt.% U alloy with non-age hardenable microstructure, appreciable thermal conductivity, moderate thermal expansion may find metallic fuel applications in nuclear reactors. - Highlights: • Th-52U alloy consists of continuous, interspersed network of Th-rich and U-rich phases. • This monotectic alloy composition shows negligible age hardening but fast kinetics. • Average linear CTE (27–600 {sup °}C) (16.7 × 10{sup −6} °C{sup -1}) of Th-52U alloy is comparable with that of other metallic fuels. • λ{sub RT} (25.6 W m{sup −1} °C{sup −1}) is comparable with that of most of the binary and ternary alloy fuels.

  14. Characterization and analyses on micro-hardness, residual stress and microstructure in laser cladding coating of 316L stainless steel subjected to massive LSP treatment

    Energy Technology Data Exchange (ETDEWEB)

    Luo, K.Y.; Jing, X.; Sheng, J. [School of Mechanical Engineering, Jiangsu University, Zhenjiang, 212013 (China); Sun, G.F. [School of Mechanical Engineering, Southeast University, Nanjing, 211189 (China); Yan, Z. [School of Mechanical Engineering, Jiangsu University, Zhenjiang, 212013 (China); Lu, J.Z., E-mail: jzlu@ujs.edu.cn [School of Mechanical Engineering, Jiangsu University, Zhenjiang, 212013 (China)

    2016-07-15

    The effects of massive laser shock peening (LSP) treatment on micro-hardness, residual stress and microstructure in four different zones of laser cladding coating was investigated. Furthermore, micro-hardness curves and residual stress distributions with and without massive LSP treatment were presented and compared, and typical microstructure in different zones of both coatings were characterized by transmission electron microscope (TEM) and cross-sectional optical microscope (OM) observations. Results and analyses showed that massive LSP treatment had an important influence on micro-hardness and residual stress of the cladding coating. Special attempt was made to the effects of massive LSP treatment on microstructure in three zones of the cladding coating. In addition, the underlying mechanism of massive LSP treatment on microstructure and mechanical properties of the cladding coating was revealed clearly. - Highlights: • Micro-hardness and residual stress curves of both coatings were presented and compared. • Typical microstructure in different zones of both coatings were characterized and analyzed. • LSP causes increased micro-activities, and induces plastic deformation layer in three zones. • Underlying mechanism of LSP on mechanical properties of cladding coating was revealed.

  15. First Synthesis of a Binuclear [Mn(II)(bipy)-Fe(III)(porphyrin)] Complex: Spectroscopic Characterization and First Evidence of Reversible Formation of Manganese(III) as Manganese Peroxidase.

    Science.gov (United States)

    Policar, Clotilde; Artaud, Isabelle; Mansuy, Daniel

    1996-01-03

    A [(P)Fe(III)-Mn(II)] bimetallic complex, mimicking the active site of manganese peroxidase, has been synthesized. A modified highly fluorinated porphyrin, 5,10,15-tris(pentafluorophenyl)-20-(o-aminophenyl)porphyrin, has been used to introduce, through a short spacer linked to the amino function, a manganese auxiliary ligand, 6-aminomethyl-2,2'-bipyridine. Two successive metalations by FeCl(2) and MnCl(2) afforded the [(P)Fe(III)-Mn(II)] bimetallic complex that has been characterized by elemental analysis and FAB(+) mass spectrometry. X-band EPR spectroscopy and magnetic susceptibility measurements were in agreement with two high spin Fe(III) and Mn(II) centers without magnetic exchange interaction. Moreover, there is no higher intermolecular association through &mgr;-chloro bridging as observed by EPR with a simpler chloromanganese complex, Mn(bipy)(2)Cl(2), at high concentration. Addition of pentafluoroiodosobenzene in methanol at 0 degrees C led to the progressive and complete disappearance of the EPR Mn(II) signals, that were recovered after addition of a phenol. This result is consistent with Mn(III) formation. This production of Mn(III) requires the presence of the iron porphyrin and is proposed to occur through the intermediate formation of a Fe(IV) dimethoxide species which can be related to the oxidation of Mn(II) catalyzed by manganese peroxidase compound II.

  16. Synthesis and characterization of a heptadentate (N4O3 Schiff base ligand and associated La(III, Sm(III and Gd(III complexes, and a theoretical study

    Directory of Open Access Journals (Sweden)

    Sadegh Salehzadeh

    2010-04-01

    Full Text Available A new symmetrical potentially heptadentate (N4O3 Schiff base ligand {N[CH2CH2CH2N=CH(2-OH-5-BrC6H3]3} (H3L6 and associated neutral Gd(III, La(III and Sm(III complexes, were synthesized. The new compounds were characterized by IR spectroscopy, elemental analysis and mass spectrometry in all cases and in the case of ligand also with NMR spectroscopy. The relative capability of H3L6 to encapsulate a lanthanide ion, herein La(III, has been theoretically studied by ab initio restricted Hartree-Fock (RHF and DFT (B3LYP methods. The calculation confirmed that the H3L6 ligand can effectively encapsulate a lanthanide ion and enforce a seven-coordinate geometry.

  17. Modeling and analysis of uncertainty in on-machine form characterization of diamond-machined optical micro-structured surfaces

    Science.gov (United States)

    Zhu, Wu-Le; Zhu, Zhiwei; Ren, Mingjun; Ehmann, Kornel F.; Ju, Bing-Feng

    2016-12-01

    Ultra-precision diamond machining is widely used in the manufacture of optical micro-structured surfaces with sub-micron form accuracy. As optical performance is highly-dependent on surface form accuracy, it is critically important to use reliable form characterization methods for surface quality control. To ascertain the characteristics of real machined surfaces, a reliable on-machine spiral scanning approach with high fidelity is presented in this paper. However, since many uncertainty contributors that lead to significant variations in the characterization results are unavoidable, an error analysis model is developed to identify the associated uncertainties to facilitate the reliable quantification of the demanding specifications of the manufactured surfaces. To accomplish this, both the diamond machining process and the on-machine spiral scanning procedure are investigated. Through the proposed model, via the Monte Carlo method, the estimation of form error parameters of a compound eye lens array is conducted in correlation with form deviations, scanning centering errors, measurement drift and noise, etc. Application experiments, using an on-machine scanning tunneling microscope, verify the proposed model and also confirm its potential superiority over the conventional off-machine raster scanning method for surface characterization and quality control.

  18. Microstructures of Metallurgical Slags

    Directory of Open Access Journals (Sweden)

    Jonczy I.

    2016-03-01

    Full Text Available The article characterizes microstructures of metallurgic slag of varying age remaining from the production of iron and steel and the Zn-Pb ore processing in relation to magmatic rocks and ores. Based on microscopic observations - among others - hypocrystalline, hyaline and felsite (characteristic for magmatic rocks microstructures were observed in the slag. Also microstructures related to ores, including framework and dendritic, colomorphic and corrosive structures were noted. The diversity of the microstructures presented in the article is a result of the differentiation in the formations of individual components of the slags, which depends, inter alia, on the method and the rate of cooling of the alloys.

  19. Synthesis, structural characterization and photoluminescence properties of a novel La(III) complex

    Science.gov (United States)

    Köse, Muhammet; Ceyhan, Gökhan; Atcı, Emine; McKee, Vickie; Tümer, Mehmet

    2015-05-01

    In this study, a novel La(III) complex [La(H2L)2(NO3)3(MeOH)] of a Schiff base ligand was synthesized and characterized by spectroscopic and analytical methods. Single crystals of the complex suitable for X-ray diffraction study were obtained by slow diffusion of diethyl ether into a MeOH solution of the complex which was found to crystallise as [La(H2L)2(NO3)3(MeOH)]ṡ2MeOHṡH2O. The structure was solved in monoclinic crystal system, P21/n space group with unit cell parameters a = 10.5641(11), b = 12.6661(16), c = 16.0022(17) Å, α = 67.364(2), β = 83.794(2)°, γ = 70.541(2)°, V = 1862.9(4) Å3 and Z = 2 with R final value of 0.526. In the complex, the La(III) ion is ten-coordinated by O atoms, five of which come from three nitrate ions, four from the two Schiff base ligands and one from MeOH oxygen atom. The Schiff base ligands in the structure are in a zwitter ion form with the phenolic H transferred to the imine N atom. Thermal properties of the La(III) complex were examined by thermogravimetric analysis and the complex was found to be thermally stable up to 310 °C. The Schiff base ligand and its La(II) complex were screened for their in vitro antimicrobial activity against Bacillus megaterium, Staphylococcus aureus, Bacillus subtilis, Micrococcus luteus (Gram positive bacteria), Klebsiella pneumonia, Escherichia coli, Enterobacter aerogenes, Pseudomonas aeruginosa (Gram negative bacteria), Candida albicans,Yarrowia lipolytica (fungus) and Saccharomyces cerevisiae (yeast). The complex shows more antimicrobial activity than the free ligand.

  20. Precise characterization of self-catalyzed III-V nanowire heterostructures via optical second harmonic generation

    Science.gov (United States)

    Yu, Ying; Wang, Jing; Wei, Yu-Ming; Zhou, Zhang-Kai; Ni, Hai-Qiao; Niu, Zhi-Chuan; Wang, Xue-Hua; Yu, Si-Yuan

    2017-09-01

    We demonstrate the utility of optical second harmonic generation (SHG) polarimetry to perform structural characterization of self-assembled zinc-blende/wurtzite III-V nanowire heterostructures. By analyzing four anisotropic SHG polarimetric patterns, we distinguish between wurtzite (WZ), zinc-blende (ZB) and ZB/WZ mixing III-V semiconducting crystal structures in nanowire systems. By neglecting the surface contributions and treating the bulk crystal within the quasi-static approximation, we can well explain the optical SHG polarimetry from the NWs with diameter from 200-600 nm. We show that the optical in-coupling and out-coupling coefficients arising from depolarization field can determine the polarization of the SHG. We also demonstrate micro-photoluminescence of GaAs quantum dots in related ZB and ZB/WZ mixing sections of core-shell NW structure, in agreement with the SHG polarimetry results. The ability to perform in situ SHG-based crystallographic study of semiconducting single and multi-crystalline nanowire heterostructures will be useful in displaying structure-property relationships of nanodevices.

  1. Antimony(III) complexes with 2-amino-4,6-dimethoxypyrimidines: Synthesis, characterization and biological evaluation.

    Science.gov (United States)

    Tunç, Turgay; Karacan, Mehmet Sayım; Ertabaklar, Hatice; Sarı, Musa; Karacan, Nurcan; Büyükgüngör, Orhan

    2015-12-01

    Novel pyrimidine compound bearing disulfide bridge, 5,5'-disulfanediylbis(2-amino-4,6-dimetoxypyrimidine) (3) was synthesized by reduction of 2-amino-4,6-dimethoxy-5-thiocyanatopyrimidine for the first time, and its structure was confirmed by X-ray crystallographic analysis. Novel binuclear antimony(III) compound of (3), {Sb[5,5'-disulfanediylbis(2-amino-4,6-dimetoxypyrimidine)]Cl3}2 (4) and mononuclear antimony(III) compounds, SbL2Cl3, [L: 2-amino-5-thiol-4,6-dimethoxy pyrimidine (2) and 2-amino-5-(1H-tetrazol-5-ylthio)-4,6-dimethoxypyrimidine (6)] were synthesized and characterized with the help of elemental analysis, molecular conductivity, FT-IR, (1)H-NMR and LC-MS techniques. The geometrical structures optimized by a DFT/B3LYP/LANL2DZ method of the compounds, indicated that monomeric compounds have square pyramidal shape. Both antileishmanial activity against Leishmania tropica promastigote and glutathione reductase inhibitory activity were determined in vitro. The results showed that (3) has the best biological activity. Copyright © 2015 Elsevier B.V. All rights reserved.

  2. Synthesis, characterization and antibacterial studies of ruthenium(III) complexes derived from chitosan schiff base.

    Science.gov (United States)

    Vadivel, T; Dhamodaran, M

    2016-09-01

    Chitosan can be modified chemically by condensation reaction of deacetylated chitosan with aldehyde in homogeneous phase. This condensation is carried by primary amine (NH2) with aldehyde (CHO) to form corresponding schiff base. The chitosan biopolymer schiff base derivatives are synthesized with substituted aldehydes namely 4-hydroxy-3-methoxy benzaldehyde, 2-hydroxy benzaldehyde, and 2-hydroxy-3-methoxy benzaldehyde, becomes a complexing agent or ligand. The Ruthenium(III) complexes were obtained by complexation of Ruthenium with schiff base ligands and this product exhibits as an excellent solubility and more biocompatibility. The novel series of schiff base Ruthenium(III) complexes are characterized by Elemental analysis, FT-IR spectroscopy, and Thermo-gravimetric analysis (TGA). The synthesized complexes have been subjected to antibacterial study. The antibacterial results indicated that the antibacterial activity of the complexes were more effective against Gram positive and Gram negative pathogenic bacteria. These findings are giving suitable support for developing new antibacterial agent and expand our scope for applications. Copyright © 2015 Elsevier B.V. All rights reserved.

  3. Performance Evaluation and Microstructure Characterization of Metakaolin-Based Geopolymer Containing Oil Palm Ash

    Directory of Open Access Journals (Sweden)

    Abideng Hawa

    2013-01-01

    Full Text Available This study reports on the microstructure, compressive strength, and drying shrinkage of metakaolin (MK based geopolymers produced by partially replacing MK by oil palm ash (OPA. The OPA was used as raw material producing different molar ratios of SiO2/Al2O3 and CaO/SiO2. The geopolymer samples were cured at 80°C for 1, 2, or 4 hours and kept at ambient temperature until testing. The compressive strength was measured after 2, 6, and 24 hours and 7 and 28 days. The testing results revealed that the geopolymer with 5% OPA (SiO2 : Al2O3 = 2.88 : 1 gave the highest compressive strength. Scanning electron microscopy (SEM indicated that the 5% OPA sample had a dense-compact matrix and less unreacted raw materials which contributed to the higher compressive strength. In the X-ray diffraction (XRD patterns, the change of the crystalline phase after heat curing for 4 hours was easily detectable compared to the samples subjected to a shorter period of heat curing.

  4. Entrapment of Probiotics in Water Extractable Arabinoxylan Gels: Rheological and Microstructural Characterization

    Directory of Open Access Journals (Sweden)

    Adriana Morales-Ortega

    2014-03-01

    Full Text Available Due to their porous structure, aqueous environment and dietary fiber nature arabinoxylan (AX gels could have potential applications for colon-specific therapeutic molecule delivery. In addition, prebiotic and health related effects of AX have been previously demonstrated. It has been also reported that cross-linked AX can be degraded by bacteria from the intestinal microbiota. However, AX gels have not been abundantly studied as carrier systems and there is no information available concerning their capability to entrap cells. In this regard, probiotic bacteria such as Bifidobacterium longum have been the focus of intense research activity lately. The objective of this research was to investigate the entrapment of probiotic B. longum in AX gels. AX solution at 2% (w/v containing B. longum (1 × 107 CFU/cm formed gels induced by laccase as cross-linking agent. The entrapment of B. longum decreased gel elasticity from 31 to 23 Pa, probably by affecting the physical interactions taking place between WEAX chains. Images of AX gels containing B. longum viewed under a scanning electron microscope show the gel network with the bacterial cells entrapped inside. The microstructure of these gels resembles that of an imperfect honeycomb. The results suggest that AX gels can be potential candidates for the entrapment of probiotics.

  5. Preparation and Microstructural Characterization of Griseofulvin Microemulsions Using Different Experimental Methods: SAXS and DSC.

    Science.gov (United States)

    Moghimipour, Eskandar; Salimi, Anayatollah; Changizi, Sahar

    2017-06-01

    Purpose: The objective of the present study is to formulate and evaluate a new microemulsion (ME) for topical delivery of griseofulvin. Methods: The solubilities of griseofulvin in different combinations of surfactant to co-surfactant (S/Co ratio) were determined. Accordingly, based on their phase diagrams, eight microemulsions were formulated and then evaluated with respect to their particle size, surface tension, viscosity, conductivity, zeta potential and stability. Their release behavior, Scanning Electron Microscopy (SEM), Differential Scanning Calorimetry (DSC), refractory index (RI), pH and Small-angle-X-ray scattering (SAXS) were also assessed. Results: The results indicated that the mean droplet size of the MEs ranged from 30.9 to 84.3 nm. Their zeta potential varied from -4.5 to -20.8. Other determined characteristics were viscosity: 254-381 cps, pH: 5.34-6.57, surface tension: 41.16- 42.83 dyne.cm-1, conductivity: 0.0442 - 0.111 ms.cm-1. The drug release was in the range of 22.4 to 43.69 percent. Also, hexagonal, cubic and lamellar liquid crystals were observed in SAXS experiments. Conclusion: It can be concluded that any alteration in MEs constituents directly affects their microstructure, shape, droplet size and their other physicochemical properties.

  6. Entrapment of probiotics in water extractable arabinoxylan gels: rheological and microstructural characterization.

    Science.gov (United States)

    Morales-Ortega, Adriana; Carvajal-Millan, Elizabeth; Brown-Bojorquez, Francisco; Rascón-Chu, Agustín; Torres-Chavez, Patricia; López-Franco, Yolanda L; Lizardi-Mendoza, Jaime; Martínez-López, Ana L; Campa-Mada, Alma C

    2014-03-24

    Due to their porous structure, aqueous environment and dietary fiber nature arabinoxylan (AX) gels could have potential applications for colon-specific therapeutic molecule delivery. In addition, prebiotic and health related effects of AX have been previously demonstrated. It has been also reported that cross-linked AX can be degraded by bacteria from the intestinal microbiota. However, AX gels have not been abundantly studied as carrier systems and there is no information available concerning their capability to entrap cells. In this regard, probiotic bacteria such as Bifidobacterium longum have been the focus of intense research activity lately. The objective of this research was to investigate the entrapment of probiotic B. longum in AX gels. AX solution at 2% (w/v) containing B. longum (1 × 10⁷ CFU/cm) formed gels induced by laccase as cross-linking agent. The entrapment of B. longum decreased gel elasticity from 31 to 23 Pa, probably by affecting the physical interactions taking place between WEAX chains. Images of AX gels containing B. longum viewed under a scanning electron microscope show the gel network with the bacterial cells entrapped inside. The microstructure of these gels resembles that of an imperfect honeycomb. The results suggest that AX gels can be potential candidates for the entrapment of probiotics.

  7. Creep behavior and in-depth microstructural characterization of dissimilar joints

    Directory of Open Access Journals (Sweden)

    F Kauffmann, T Klein, A Klenk and K Maile

    2013-01-01

    Full Text Available The 700 °C power plants currently under development will utilize Ni-base alloys such as alloy 617 for components to be operated at temperatures >650 °C. Due to economic reasons for components or parts of components which are subjected to temperatures <650 °C, 2% Cr or 9–12% Cr steels is used, depending on the required mechanical properties. This makes the dissimilar joining of Ni-base alloys and Cr steels a necessity in these plants. Experimental investigations show that these joints have to be identified as weak points with regard to damage development under creep and creep-fatigue loading. The present investigation focuses on welds between the alloy 617 and 2% Cr steel. Under creep load the fracture occurs near the fusion line between the 2% Cr steel base metal and alloy 617 weld metal. To explain the reasons for this fracture location, the microstructure of this fusion line was investigated using TEM and FIB techniques after welding and after creep loading. The TEM investigations have shown a small zone in the weld metal near the fusion line exhibiting chromium depletion and clearly reduced amounts of chromium carbides, leading to a weakening of this zone.

  8. Microstructure characterization of onion (A.cepa) peels and thin films for dye sensitized solar cells

    Science.gov (United States)

    Abodunrin, T.; Boyo, A.; Usikalu, M.; Obafemi, L.; Oladapo, O.; Kotsedi, L.; Yenus, Z.; Maaza, M.

    2017-03-01

    A.cepa peels are obtained from mature onion bulbs. Because of the continuous need for energy, alternative avenues for producing energy are gaining importance. The motivation for this work is based on an urgent need to source energy from readily available waste materials like domestic onion peels. Dye sensitized solar cells (DSSCs) fabricated via doctor blade method and high temperature sintering from waste (onion peels) are investigated for their ability to convert solar to electrical energy. The charge carriers were revealed under phytochemical screening. Functional groups of compounds present in A.cepa peel were analyzed with Fourier transform in infrared (FTIR). The influence of different electrolyte sensitizer is observed on the DSSCs under standard air mass conditions of 1.5 AM. The microstructure properties of these A.cepa DSSCs were explored using scanning electron microscope with energy dispersive spectroscopy (SEM/EDS), x-ray diffraction and Fluorecence spectroscopy (XRF). The interfacial boundary between A.cepa dye, TiO2 framework of TiO2 and indium doped tin oxide (ITO) reveals several prominent anatase and rutile peaks. Photoelectric results, revealed dye-sensitized solar cells with a maximum power output of 126 W and incident photon to conversion energy (IPCE) of 0.13%.This work has established that A.cepa peels can be used as a source of micro-energy generation.

  9. Microstructural characterization and influence of manufacturing parameters on technological properties of vitreous ceramic materials

    Energy Technology Data Exchange (ETDEWEB)

    Njoya, D. [Laboratoire de Physico-chimie des Materiaux Mineraux, Departement de Chimie Inorganique, Faculte des Sciences, Universite de Yaounde I, B.P. 812, Yaounde (Cameroon); Laboratoire de Physico-chimie des Materiaux et Environnement, Departement de Chimie, Faculte des Sciences Semlalia, Universite Cadi Ayyad, B.P. 2390, Marrakech (Morocco); Hajjaji, M., E-mail: Hajjaji@ucam.ac.ma [Laboratoire de Physico-chimie des Materiaux et Environnement, Departement de Chimie, Faculte des Sciences Semlalia, Universite Cadi Ayyad, B.P. 2390, Marrakech (Morocco); Bacaoui, A. [Laboratoire de Chimie Organique Appliquee, Departement de Chimie, Faculte des Sciences Semlalia, Universite Cadi Ayyad, B.P. 2390, Marrakech (Morocco); Njopwouo, D. [Laboratoire de Physico-chimie des Materiaux Mineraux, Departement de Chimie Inorganique, Faculte des Sciences, Universite de Yaounde I, B.P. 812, Yaounde (Cameroon)

    2010-03-15

    Microstructure of vitreous ceramic samples manufactured from kaolinitic-clay and feldspars raw materials from Cameroon was investigated in the range 1150-1250 deg. C by X-ray diffraction and scanning electron microscopy and by measuring some technological properties. Moreover, the simultaneous influence of feldspars content, heating temperature and soaking time on water absorption and firing shrinkage was evaluated by adopting the response surface methodology (Doehlert matrix), using the New Efficient Methodology for Research using Optimal Design (NEMROD) software. The results show that a spinel phase, mullite, glassy phase and some amount of hematite were formed. However, the spinel phase and potassic feldspar, as compared to the sodic one, disappeared at moderate firing temperature and soaking time. Apparently, mullite developed from spinel phase, which is formed from the demixion of metakaolin. On the other hand, it is found that the effects of fluxing content and firing temperature on the measured properties were almost similar and more influent than soaking time. Antagonistic and synergetic interactions existed between the considered parameters, and their importance differed for the considered properties. By using this mathematical tool, suitable operating conditions for manufacturing vitreous bodies were determined.

  10. Fractal microstructure characterization of wet microalgal cells disrupted with ultrasonic cavitation for lipid extraction.

    Science.gov (United States)

    Cheng, Jun; Sun, Jing; Huang, Yun; Zhou, Junhu; Cen, Kefa

    2014-10-01

    The effects of ultrasonic treatment on fractal microstructures of wet microalgal cells were investigated for lipid extraction. Fractal dimension of cells with distorted surfaces increased with power and ultrasonication time. Microalgal cells shrank owing to dehydration and cytomembranes were reduced to debris, but cell walls were not fragmented. When ultrasonication power increased from 0 to 500W for 30min, the fractal dimension of cells increased from 1.21 to 1.51, cell sizes decreased from 2.78 to 1.68μm and cell wall thickness decreased from 0.08 to 0.05μm. When ultrasonication time increased from 5 to 30min with a power of 150W, the fractal dimension of cells increased from 1.24 to 1.37, cell sizes decreased from 2.72 to 2.38μm and cell wall thickness first increased to a peak of 0.22μm and then decreased. Long-chain and unsaturated lipids were degraded into short-chain and saturated lipids with ultrasonic cavitation. Copyright © 2014 Elsevier Ltd. All rights reserved.

  11. Microstructure characterization and corrosion testing of MAG pulsed duplex stainless steel welds

    Energy Technology Data Exchange (ETDEWEB)

    Mitelea, Ion; Utu, Ion Dragos; Urlan, Sorin Dumitru; Karancsi, Olimpiu [Politehnica Univ. Timisoara (Romania). Faculty of Mechanical Engineering

    2017-08-01

    Duplex stainless steels are extremely attractive construction materials for their usage in intense aggressive environments. They offer numerous advantages compared to the austenitic stainless steels having an excellent behavior to pitting and cavernous corrosion, and a high resistance to stress cracking corrosion in chlorides media. However, their corrosion properties are largely dependent on the microstructural factors such as: the quantitative ratio of the two phases ferrite/austenite (F/A), the presence of intermetallic compounds and the distribution of the alloying elements between the ferrite and austenite. As a result of the thermal cycles experienced by the base metal without a post-weld heat treatment, the mechanical properties are significantly different in the heat affected zone and the deposited metal compared with the properties of the base metal. The present paper highlights the effect of the post-weld solution treatment in order to restore the balance between austenite and ferrite in the welded joint areas and also to limit undesirable precipitation of secondary phases with implications for increasing the corrosion resistance.

  12. Performance evaluation and microstructure characterization of metakaolin-based geopolymer containing oil palm ash.

    Science.gov (United States)

    Hawa, Abideng; Tonnayopas, Danupon; Prachasaree, Woraphot

    2013-01-01

    This study reports on the microstructure, compressive strength, and drying shrinkage of metakaolin (MK) based geopolymers produced by partially replacing MK by oil palm ash (OPA). The OPA was used as raw material producing different molar ratios of SiO₂/Al₂O₃ and CaO/SiO₂. The geopolymer samples were cured at 80°C for 1, 2, or 4 hours and kept at ambient temperature until testing. The compressive strength was measured after 2, 6, and 24 hours and 7 and 28 days. The testing results revealed that the geopolymer with 5% OPA (SiO₂  : Al₂O₃ = 2.88 : 1) gave the highest compressive strength. Scanning electron microscopy (SEM) indicated that the 5% OPA sample had a dense-compact matrix and less unreacted raw materials which contributed to the higher compressive strength. In the X-ray diffraction (XRD) patterns, the change of the crystalline phase after heat curing for 4 hours was easily detectable compared to the samples subjected to a shorter period of heat curing.

  13. Phase and Micro-Structural Characterization of Sanitary-Ware Fired at Different Temperature

    Directory of Open Access Journals (Sweden)

    ATHER HASSAN

    2017-07-01

    Full Text Available The three main ingredients of sanitary-ware are clay, feldspar and quartz. This ware is being widely used and has therefore, attracted the attention of researchers from time to time. Consequently, it has been extensively investigated. The present study describes the phase and micro-structural analysis of sanitary-ware samples collected from local (Durr Ceramics Peshawar industry. XRD (X-Ray Diffraction of samples fired at 1100oC reveals the presence of ? ? ? ? ?-quartz and primary mullite only. In addition to a-quartz and primary mullite, elongated needles of secondary mullite were also present in samples fired at 1200 and 1300oC. Unlike typical vitreous ceramics bodies, regions containing elongated secondary mullite originating from the clay relict and growing into the feldspar relict were few in number which is consistent with the high clay content in the starting body ingredients of the investigated samples. Another sample investigated for comparison purposes, contained all the phases mentioned above along with some corundum grains which indicated that the composition of sanitary ware varied from manufacturer to manufacturer. EDS (Energy Dispersive Spectroscopy detected high concentration of Fe in some regions in the bulk but the glaze did not contain any Fe.

  14. Synthesis, characterization, crystal structure and electrochemical studies of ionic iron(III) dipicolinato complex

    Science.gov (United States)

    Ghasemi, Fatemeh; Ghasemi, Khaled; Rezvani, Ali Reza; Rosli, Mohd Mustaqim; Razak, Ibrahim Abdul

    2017-09-01

    The new complex (NH4)[Fe(dipic)2] (1) (dipicH2 = 2,6-pyridinedicarboxylic acid), was synthesized and characterized by elemental analysis, FTIR and UV-Vis spectroscopy and single crystal X-ray method. The crystal system is tetragonal with space group I41/a. The FeIII ion and the N atom of the ammonium cation are located on a crystallographic fourfold rotoinversion axis (4 bar). The Nsbnd H⋯O and Csbnd H⋯O intermolecular hydrogen bonding and π⋯π stacking interactions play an important role in the formation of a 3-dimensional anion-cation network and stabilization of the crystal structure. The redox behavior of the complex was also investigated by cyclic voltammetry.

  15. Towards long lasting zirconia-based composites for dental implants. Part I: innovative synthesis, microstructural characterization and in vitro stability.

    Science.gov (United States)

    Palmero, Paola; Fornabaio, Marta; Montanaro, Laura; Reveron, Helen; Esnouf, Claude; Chevalier, Jérôme

    2015-05-01

    In order to fulfill the clinical requirements for strong, tough and stable ceramics used in dental applications, we designed and developed innovative zirconia-based composites, in which equiaxial α-Al2O3 and elongated SrAl12O19 phases are dispersed in a ceria-stabilized zirconia matrix. The composite powders were prepared by an innovative surface coating route, in which commercial zirconia powders were coated by inorganic precursors of the second phases, which crystallize on the zirconia particles surface under proper thermal treatment. Samples containing four different ceria contents (in the range 10.0-11.5 mol%) were prepared by carefully tailoring the amount of the cerium precursor during the elaboration process. Slip cast green bodies were sintered at 1450 °C for 1 h, leading to fully dense materials. Characterization of composites by SEM and TEM analyses showed highly homogeneous microstructures with an even distribution of both equiaxial and elongated-shape grains inside a very fine zirconia matrix. Ce content plays a major role on aging kinetics, and should be carefully controlled: sample with 10 mol% of ceria were transformable, whereas above 10.5 mol% there is negligible or no transformation during autoclave treatment. Thus, in this paper we show the potential of the innovative surface coating route, which allows a perfect tailoring of the microstructural, morphological and compositional features of the composites; moreover, its processing costs and environmental impacts are limited, which is beneficial for further scale-up and real use in the biomedical field. Copyright © 2015 Elsevier Ltd. All rights reserved.

  16. Synthesis and Spectral Characterization of Praseodymium(III Complex with New Amino Acid-Based Azo Dye

    Directory of Open Access Journals (Sweden)

    Man Singh

    2012-01-01

    Full Text Available A new Praseodymium (Pr (III complex has been synthesized and characterized by using a new amino acid-based (leucine azo dye such as N,N-dimethylazoleucine (L1 and 1,10 phenanthroline (L2. Reaction of Pr(III ion with L1 and L2 in 1 : 2 : 1 ratio in alcoholic medium has been carried out with general formula [Pr(L12(L2(H2O2]. Elemental analysis, comparative FT-IR, and 1HNMR spectral studies of Pr(III complex with ligands have been shown in this paper.

  17. Design of an expert system based on neuro-fuzzy inference analyzer for on-line microstructural characterization using magnetic NDT method

    Science.gov (United States)

    Ghanei, S.; Vafaeenezhad, H.; Kashefi, M.; Eivani, A. R.; Mazinani, M.

    2015-04-01

    Tracing microstructural evolution has a significant importance and priority in manufacturing lines of dual-phase steels. In this paper, an artificial intelligence method is presented for on-line microstructural characterization of dual-phase steels. A new method for microstructure characterization based on the theory of magnetic Barkhausen noise nondestructive testing method is introduced using adaptive neuro-fuzzy inference system (ANFIS). In order to predict the accurate martensite volume fraction of dual-phase steels while eliminating the effect and interference of frequency on the magnetic Barkhausen noise outputs, the magnetic responses were fed into the ANFIS structure in terms of position, height and width of the Barkhausen profiles. The results showed that ANFIS approach has the potential to detect and characterize microstructural evolution while the considerable effect of the frequency on magnetic outputs is overlooked. In fact implementing multiple outputs simultaneously enables ANFIS to approach to the accurate results using only height, position and width of the magnetic Barkhausen noise peaks without knowing the value of the used frequency.

  18. Physics, fabrication and characterization of III-V multi-gate FETs for low power electronics

    Science.gov (United States)

    Thathachary, Arun V.

    With transistor technology close to its limits for power constrained scaling and the simultaneous emergence of mobile devices as the dominant driver for new scaling, a pathway to significant reduction in transistor operating voltage to 0.5V or lower is urgently sought. This however implies a fundamental paradigm shift away from mature Silicon technology. III-V compound semiconductors hold great promise in this regard due to their vastly superior electron transport properties making them prime candidates to replace Silicon in the n-channel transistor. Among the plethora of binary and ternary compounds available in the III-V space, InxGa1-xAs alloys have attracted significant interest due to their excellent electron mobility, ideally placed bandgap and mature growth technology. Simultaneously, electrostatic control mandates multigate transistor designs such as the FinFET at extremely scaled nodes. This dissertation describes the experimental realization of III-V FinFETs incorporating InXGa1-XAs heterostructure channels for high performance, low power logic applications. The chapters that follow present experimental demonstrations, simulations and analysis on the following aspects (a) motivation and key figures of merit driving material selection and design; (b) dielectric integration schemes for high-k metal-gate stack (HKMG) realization on InXGa 1-XAs, including surface clean and passivation techniques developed for high quality interfaces; (c) novel techniques for transport (mobility) characterization in nanoscale multi-gate FET architectures with experimental demonstration on In0.7Ga0.3As nanowires; (d) Indium composition and quantum confined channel design for InXGa 1-XAs FinFETs and (e) InAs heterostructure designs for high performance FinFETs. Each chapter also contains detailed benchmarking of results against state of the art demonstrations in Silicon and III-V material systems. The dissertation concludes by assessing the feasibility of InXGa 1-XAs Fin

  19. Synthesis by aerosol assisted chemical vapor deposition and microstructural characterization of PbTiO{sub 3} thin films

    Energy Technology Data Exchange (ETDEWEB)

    Ramos-Cano, J.; Hurtado-Macías, A.; Antúnez-Flores, W.; Fuentes-Cobas, L.; González-Hernández, J.; Amézaga-Madrid, P.; Miki-Yoshida, M., E-mail: mario.miki@cimav.edu.mx

    2013-03-01

    Thin films of PbTiO{sub 3} were deposited onto (001) silicon single-crystal substrates by aerosol assisted chemical vapor deposition method at different temperatures, using organometallic precursors. With the objective of stabilizing and homogenizing the perovskite phase, the films were annealed at 800 °C, in a Pb-rich atmosphere, for 4 and 6 h. The evolution of compositions and microstructure of the films was characterized before and after annealing, by grazing incidence X-ray diffraction, two-dimensional detection of grazing incidence diffraction with synchrotron radiation, scanning electron microscopy and high resolution transmission electron microscopy. X-ray diffraction results showed that the crystalline structure of optimized PbTiO{sub 3} films corresponded to a tetragonal perovskite-type, with lattice parameters a = 0.387(4) nm and c = 0.406(4) nm. In addition, the inverse pole figure of the fiber texture representation, had a Gaussian (1, 1, 0) component and distribution width Ω = 15°. - Highlights: ► We report the synthesis of homogeneous PbTiO{sub 3} thin films on Si substrates. ► They were synthesized by aerosol assisted chemical vapor deposition method. ► Detailed characterization by X-ray diffraction and electron microscopy was performed. ► Crystalline structure of PbTiO{sub 3} films corresponded to a tetragonal perovskite-type. ► The fiber texture representation had a Gaussian (1, 1, 0) component.

  20. Microstructural characterization of Ti-C-N thin films prepared by reactive crossed beam pulsed laser deposition

    Energy Technology Data Exchange (ETDEWEB)

    Escobar-Alarcon, L., E-mail: luis.escobar@inin.gob.mx [Departamento de Fisica, Instituto Nacional de Investigaciones Nucleares, Apdo. Postal 18-1027, Mexico DF 11801 (Mexico); Medina, V.; Camps, Enrique; Romero, S. [Departamento de Fisica, Instituto Nacional de Investigaciones Nucleares, Apdo. Postal 18-1027, Mexico DF 11801 (Mexico); Fernandez, M. [Departamento de Aceleradores, Instituto Nacional de Investigaciones Nucleares, Apdo. Postal 18-1027, Mexico DF 11801 (Mexico); Solis-Casados, D. [Centro Conjunto de Investigacion en Quimica Sustentable, Facultad de Quimica UAEMex, km. 14.5 carr. Toluca-Atlacomulco (Mexico)

    2011-08-15

    In this work, Raman spectroscopy has been used to characterize Ti-C-N thin films in order to obtain information about the microstructure of the deposited materials, and in particular to study the effects due to the carbon incorporation into the TiN lattice. Ti-C-N thin films were prepared using a crossed plasma configuration in which the ablation of two different targets, titanium and carbon, in a reactive atmosphere was performed. With this configuration, the carbon content in the films was varied in an easy way from 5.0 at% to 40.0 at%. Thin film composition was determined from Non-Rutherford Backscattering Spectroscopy (NRBS) measurements. X-ray photoelectron spectroscopy and X-Ray diffraction measurements were also carried out in order to characterize the films in more detail, with this being used to give support to the interpretation of the Raman spectra. The Raman results revealed that at lower carbon concentrations a solid solution Ti(C, N) is formed, whilst at higher carbon concentrations a nanocomposite, consisting of nanocrystalline TiCN and TiC immersed in an amorphous carbon matrix is obtained.

  1. Microstructural, Chemical and Mechanical Characterization of Polymer-Derived Hi-Nicalon Fibers with Surface Coatings

    Science.gov (United States)

    Bansal, Narottam P.; Chen, Yuan L.

    1998-01-01

    Room temperature tensile strengths of as-received Hi-Nicalon fibers and those having BN/SiC, p-BN/SiC, and p-B(Si)N/SiC surface coatings, deposited by chemical vapor deposition, were measured using an average fiber diameter of 13.5 microns. The Weibull statistical parameters were determined for each fiber. The average tensile strength of uncoated Hi-Nicalon on was 3.19 +/- 0.73 GPa with a Weibull modulus of 5.41. Strength of fibers coated with BN/SiC did not change. However, coat with p-BN/SiC and p-B(Si)N/SiC surface layers showed strength loss of approx. 10 and 35 percent, respectively, compared with as-received fibers. The elemental compositions of the fibers and the coatings were analyzed using scanning Auger microprobe and energy dispersive x-ray spectroscopy. The BN coating was contaminated with a large concentration of carbon and some oxygen. In contrast, p-BN, p-B(Si)N, and SiC coatings did not show any contamination. Microstructural analyses of the fibers and the coatings were done by scanning electron microscopy (SEM), transmission electron microscopy (TEM), and selected area electron diffraction. Hi-Nicalon fiber consists of the P-SIC nanocrystals ranging in size from 1 to 30 nm embedded in an amorphous matrix. TEM analysis of the BN coating revealed four distinct layers with turbostatic structure. The p-BN layer was turbostratic and showed considerable preferred orientation. The p-B(Si)N was glassy and the silicon and boron were uniformly distributed. The silicon carbide coating was polycrystalline with a columnar structure along the growth direction. The p-B(Si)N/SiC coatings were more uniform, less defective and of better quality than the BN/SiC or the p-BN/SiC coatings.

  2. Microstructural characterization of a new mechanically alloyed Ni-base ODS superalloy powder

    Energy Technology Data Exchange (ETDEWEB)

    Seyyed Aghamiri, S.M. [Department of Materials Engineering, Tarbiat Modares University, Tehran 14115-143 (Iran, Islamic Republic of); Shahverdi, H.R., E-mail: Shahverdi@modares.ac.ir [Department of Materials Engineering, Tarbiat Modares University, Tehran 14115-143 (Iran, Islamic Republic of); Ukai, S.; Oono, N.; Taya, K.; Miura, S.; Hayashi, S. [Material Science and Engineering, Faculty of Engineering, Hokkaido University, Sapporo 060-8626 (Japan); Okuda, T. [Kobelco Research Institute Ltd., Kobe 651-2271 (Japan)

    2015-02-15

    The microstructure of a new Ni-base oxide dispersion strengthened superalloy powder was studied for high temperature gas turbine applications after the mechanical alloying process. In this study, an atomized powder with a composition similar to the CMSX-10 superalloy was mechanically alloyed with yttria and Hf powders. The mechanically alloyed powder included only the supersaturated solid solution γ phase without γ′ and yttria provided by severe plastic deformation, while after the 3-step aging, the γ′ phase was precipitated due to the partitioning of Al and Ta to the γ′ and Co, Cr, Re, W, and Mo to the γ phase. Mechanical alloying modified the morphology of γ′ to the new coherent γ–γ′ nanoscale lamellar structure to minimize the elastic strain energy of the precipitation, which yielded a low lattice misfit of 0.16% at high temperature. The γ′ lamellae aligned preferentially along the elastically soft [100] direction. Also, the precipitated oxide particles were refined in the γ phase by adding Hf from large incoherent YAlO{sub 3} to fine semi-coherent Y{sub 2}Hf{sub 2}O{sub 7} oxide particles with the average size of 7 nm and low interparticle spacing of 76 nm. - Highlights: • A new Ni-base ODS superalloy powder was produced by mechanical alloying. • The nanoscale γ–γ′ lamellar structure was precipitated after the aging treatment. • Fine semi-coherent Y{sub 2}Hf{sub 2}O{sub 7} oxide particles were precipitated by addition of Hf.

  3. Dielectric properties and microstructural characterization of cubic pyrochlored bismuth magnesium niobates

    KAUST Repository

    Zhang, Yuan

    2013-08-06

    Cubic bismuth pyrochlores in the Bi2O3 Bi 2O3-MgO-Nb2O5 Nb2O 5 system have been investigated as promising dielectric materials due to their high dielectric constant and low dielectric loss. Here, we report on the dielectric properties and microstructures of cubic pyrochlored Bi 1.5 MgNb 1.5 O 7 Bi1.5MgNb1.5O7 (BMN) ceramic samples synthesized via solid-state reactions. The dielectric constant (measured at 1 MHz) was measured to be ∼ 120 ∼120 at room temperature, and the dielectric loss was as low as 0.001. X-ray diffraction patterns demonstrated that the BMN samples had a cubic pyrochlored structure, which was also confirmed by selected area electron diffraction (SAED) patterns. Raman spectrum revealed more than six vibrational models predicted for the ideal pyrochlore structure, indicating additional atomic displacements of the A and O′ O\\' sites from the ideal atomic positions in the BMN samples. Structural modulations of the pyrochlore structure along the [110] and [121] directions were observed in SAED patterns and high-resolution transmission electron microscopy (HR-TEM) images. In addition, HR-TEM images also revealed that the grain boundaries (GBs) in the BMN samples were much clean, and no segregation or impure phase was observed forming at GBs. The high dielectric constants in the BMN samples were ascribed to the long-range ordered pyrochlore structures since the electric dipoles formed at the superstructural direction could be enhanced. The low dielectric loss was attributed to the existence of noncontaminated GBs in the BMN ceramics. © 2013 Springer-Verlag Berlin Heidelberg.

  4. Synthesis, Characterization and Antibacterial Studies of N-(Benzothiazol-2-yl-4-chlorobenzenesulphonamide and Its Neodymium(III and Thallium(III Complexes

    Directory of Open Access Journals (Sweden)

    Lawrence Nnamdi Obasi

    2017-02-01

    Full Text Available N-(Benzothiazol-2-yl-4-chlorobenzenesulphonamide (NBTCS was synthesized by condensation reaction of 4-chlorobenzenesulphonyl chloride and 2-aminobenzothiazole in acetone under reflux. Neodymium(III and thallium(III complexes of the ligand were also synthesized. Both ligand and metal complexes were characterized using UV-Vis, IR, 1H- and 13C-NMR spectroscopies, elemental analysis and molar conductance measurement. IR studies revealed that the ligand is tridentate and coordinates to the metal ions through nitrogen and oxygen atoms of the sulphonamide group and nitrogen atom attached to benzothiazole ring. The neodymium(III complex displays a coordination number of eight while thallium(III complex displays a coordination number of six. The ligand and its complexes were screened in vitro for their antibacterial activities against Escherichia coli strains (E. coli 6 and E. coli 13, Proteus species, Staphylococcus aureus and Pseudomonas aeruginosa using the agar well diffusion technique. The synthesized compounds were found to be more active against the microorganisms screened relative to ciprofloxacin, gentamicin and co-trimoxazole.

  5. Optical and micro-structural characterizations of MBE grown indium gallium nitride polar quantum dots

    KAUST Repository

    Elafandy, Rami T.

    2011-12-01

    Comparison between indium rich (27%) InGaN/GaN quantum dots (QDs) and their underlying wetting layer (WL) is performed by means of optical and structural characterizations. With increasing temperature, micro-photoluminescence (μPL) study reveals the superior ability of QDs to prevent carrier thermalization to nearby traps compared to the two dimensional WL. Thus, explaining the higher internal quantum efficiency of the QD nanostructure compared to the higher dimensional WL. Structural characterization (X-ray diffraction (XRD)) and transmission electron microscopy (TEM)) reveal an increase in the QD indium content over the WL indium content which is due to strain induced drifts. © 2011 IEEE.

  6. Synchrotron X-ray Characterization of Structural Defects in III-Nitride Wide Bandgap Semiconductors

    Science.gov (United States)

    Wu, Shuang

    III-nitrides have long been viewed as promising semiconductor materials for their wide-band gap and high efficiency for emitting light. They have been widely used in electronic and optoelectronic devices, even in the extreme environments such as high frequencies, high voltages and high temperatures. Despite their favorable properties, their performance is strongly affected by factors; such as the growth method employed and consequently the defect types generated and their quantity. In this thesis, the wide bandgap III-nitrides, aluminum nitride (AlN) and gallium nitride (GaN) will be discussed in the aspect of structure, properties and defects characterization. The density of defects, particularly basal plane dislocations and threading edge and screw dislocations, will be measured across multiple wafers and analyzed in order to gain insights into origins of these defects with respect to the growth process employed. Other defects like low angle grain boundaries and prismatic slip bands are also observed and analyzed. In this study, synchrotron white beam and monochromatic X-ray topography are the main techniques employed to characterize samples, with Nomarski optical microscopy used in a complementary manner. For physical vapor transport (PVT) grown AlN wafers, the distribution of basal plane dislocations and threading dislocations imaged and analyzed synchrotron X-ray topography reveals a wide range of densities from as low as 1.7x102cm-2 to greater than 106cm -2, the resolution limit for X-ray topography techniques. For basal plane dislocations (BPDs), the average density is 1.6747x104 cm-2. As for threading dislocations (TDs), both screw and edge, the average dislocation density is about 1.5515x10 4 cm-2 ranging from a low of 3.00x102 cm-2 to a high of 4.477x104cm -2. These differences among the wafers, is clearly attributable to variations in growth conditions. For hydride vapor phase epitaxy (HVPE) grown GaN wafers on ammonothermal GaN substrates, the threading

  7. Microstructural characterization in diffusion bonded TiC–Al2O3/Cr18 ...

    Indian Academy of Sciences (India)

    Unknown

    Key Lab of Liquid Structure and Heredity of Materials, Ministry of Education, Shandong University. (South Campus), Jinan 250061, P.R. China. MS received 10 ... of characterization techniques such as scanning electron microscope (SEM) with energy dispersion spectro- scopy (EDS) and X-ray diffraction (XRD). The results ...

  8. Microstructural characterization in diffusion bonded TiC–Al2O3/Cr18 ...

    Indian Academy of Sciences (India)

    The diffusion bonded TiC–Al2O3/Cr18–Ni8 joint was investigated by a variety of characterization techniques such as scanning electron microscope (SEM) with energy dispersion ... Key Lab of Liquid Structure and Heredity of Materials, Ministry of Education, Shandong University (South Campus), Jinan 250061, P.R. China ...

  9. Microstructural characterization and thermal cycling reliability of solders under isothermal aging and electrical current

    Science.gov (United States)

    Chauhan, Preeti Singh

    Solder joints on printed circuit boards provide electrical and mechanical connections between electronic devices and metallized patterns on boards. These solder joints are often the cause of failure in electronic packages. Solders age under storage and operational life conditions, which can include temperature, mechanical loads, and electrical current. Aging occurring at a constant temperature is called isothermal aging. Isothermal aging leads to coarsening of the bulk microstructure and increased interfacial intermetallic compounds at the solder-pad interface. The coarsening of the solder bulk degrades the creep properties of solders, whereas the voiding and brittleness of interfacial intermetallic compounds leads to mechanical weakness of the solder joint. Industry guidelines on solder interconnect reliability test methods recommend preconditioning the solder assemblies by isothermal aging before conducting reliability tests. The guidelines assume that isothermal aging simulates a "reasonable use period," but do not relate the isothermal aging levels with specific use conditions. Studies on the effect of isothermal aging on the thermal cycling reliability of tin-lead and tin-silver-copper solders are limited in scope, and results have been contradictory. The effect of electrical current on solder joints has been has mostly focused on current densities above 104A/cm2 with high ambient temperature (≥100oC), where electromigration, thermomigration, and Joule heating are the dominant failure mechanisms. The effect of current density below 104A/cm2 on temperature cycling fatigue of solders has not been established. This research provides the relation between isothermal aging and the thermal cycling reliability of select Sn-based solders. The Sn-based solders with 3%, 1%, and 0% silver content that have replaced tin-lead are studied and compared against tin-lead solder. The activation energy and growth exponents of the Arrhenius model for the intermetallic growth in

  10. Manganese-incorporated iron(III) oxide-graphene magnetic nanocomposite: synthesis, characterization, and application for the arsenic(III)-sorption from aqueous solution

    Energy Technology Data Exchange (ETDEWEB)

    Nandi, Debabrata; Gupta, Kaushik; Ghosh, Arup Kumar [Presidency University, Department of Chemistry and Biochemistry (India); De, Amitabha [Saha Institute of Nuclear Physics, Chemical Science Division (India); Banerjee, Sangam [Saha Institute of Nuclear Physics, Surface Physics Division (India); Ghosh, Uday Chand, E-mail: ucghosh@yahoo.co.in [Presidency University, Department of Chemistry and Biochemistry (India)

    2012-12-15

    High specific surface area of graphene (GR) has gained special scientific attention in developing magnetic GR nanocomposite aiming to apply for the remediation of diverse environmental problems like point-of-use water purification and simultaneous separation of contaminants applying low external magnetic field (<1.0 T) from ground water. Fabrication of magnetic manganese-incorporated iron(III) oxide (Mn{sub x}{sup 2+}Fe{sub 2-x}{sup 3+}O{sub 4}{sup 2-}) (IMBO)-GR nanocomposite is reported by exfoliating the GR layers. Latest microscopic, spectroscopic, powder X-ray diffraction, BET surface area, and superconducting quantum interference device characterizations showed that the material is a magnetic nanocomposite with high specific surface area (280 m{sup 2} g{sup -1}) and pore volume (0.3362 cm{sup 3} g{sup -1}). Use of this composite for the immobilization of carcinogenic As(III) from water at 300 K and pH {approx}7.0 showed that the nanocomposite has higher binding efficiency with As(III) than the IMBO owing to its high specific surface area. The composite showed almost complete (>99.9 %) As(III) removal ({<=}10 {mu}g L{sup -1}) from water. External magnetic field of 0.3 T efficiently separated the water dispersed composite (0.01 g/10 mL) at room temperature (300 K). Thus, this composite is a promising material which can be used effectively as a potent As(III) immobilizer from the contaminated groundwater (>10 {mu}g L{sup -1}) to improve drinking water quality.

  11. Synthesis, Characterization, Anticancer, and Antioxidant Studies of Ru(III) Complexes of Monobasic Tridentate Schiff Bases

    Science.gov (United States)

    Ejidike, Ikechukwu P.

    2016-01-01

    Mononuclear Ru(III) complexes of the type [Ru(LL)Cl2(H2O)] (LL = monobasic tridentate Schiff base anion: (1Z)-N′-(2-{(E)-[1-(2,4-dihydroxyphenyl)ethylidene]amino}ethyl)-N-phenylethanimidamide [DAE], 4-[(1E)-N-{2-[(Z)-(4-hydroxy-3-methoxybenzylidene)amino]ethyl}ethanimidoyl]benzene-1,3-diol [HME], 4-[(1E)-N-{2-[(Z)-(3,4-dimethoxybenzylidene)amino]ethyl}ethanimidoyl]benzene-1,3-diol [MBE], and N-(2-{(E)-[1-(2,4-dihydroxyphenyl)ethylidene]amino}ethyl)benzenecarboximidoyl chloride [DEE]) were synthesized and characterized using the microanalytical, conductivity measurements, electronic spectra, and FTIR spectroscopy. IR spectral studies confirmed that the ligands act as tridentate chelate coordinating the metal ion through the azomethine nitrogen and phenolic oxygen atom. An octahedral geometry has been proposed for all Ru(III)-Schiff base complexes. In vitro anticancer studies of the synthesized complexes against renal cancer cells (TK-10), melanoma cancer cells (UACC-62), and breast cancer cells (MCF-7) was investigated using the Sulforhodamine B assay. [Ru(DAE)Cl2(H2O)] showed the highest activity with IC50 valves of 3.57 ± 1.09, 6.44 ± 0.38, and 9.06 ± 1.18 μM against MCF-7, UACC-62, and TK-10, respectively, order of activity being TK-10 [Ru(HME)Cl2(H2O)] > [Ru(DAE)Cl2(H2O)] > [Ru(MBE)Cl2(H2O)]. PMID:27597814

  12. Microstructural characterization of the HRSI thermal protection system for space shuttle

    Science.gov (United States)

    Ransone, P. O.; Rummler, D. R.

    1980-01-01

    Components of the space shuttle high temperature reusable surface insulation (HRSI) system were microscopically characterized, both separately and as a system, to obtain information needed for stress analysis models of the thermal protection system. A tension specimen of the HRSI system was loaded in steps and was microscopically observed at each load condition to demonstrate the tension failure mode associated with strain isolation pad (SIP) behavior. A local failure occurred which should be associated with transfer of load through transverse fibers in the SIP. Stress concentrations attributed to the SIP behavior necessitated strengthening of the HRSI by densification of the RSI at the bondline. An HRSI tile was microscopically characterized after the densification process. The densified surface layer blended into the RSI which caused a gradual change in density. The gradation in density does not appear to represent a sharp discontinuity in elastic modulus between the densified layer and the parent material.

  13. Characterization of Large Grain Nb Ingot Microstructure Using OIM and Laue Methods

    Energy Technology Data Exchange (ETDEWEB)

    D. Kang, D.C. Baars, T.R. Bieler, G. Ciovati, C. Compton, T.L. Grimm, A.A. Kolka

    2011-07-01

    Large grain niobium is being examined for fabricating superconducting radiofrequency cavities as an alternative to using rolled sheet with fine grains. It is desirable to know the grain orientations of a niobium ingot slice before fabrication, as this allows heterogeneous strain and surface roughness effects arising from etching to be anticipated. Characterization of grain orientations has been done using orientation imaging microscopy (OIM), which requires destructive extraction of pieces from an ingot slice. Use of a Laue camera allows nondestructive characterization of grain orientations, a process useful for evaluating slices and deformation during the manufacturing process. Five ingot slices from CBMM, Ningxia, and Heraeus are compared. One set of slices was deformed into a half cell and the deformation processes that cause crystal rotations have been investigated and compared with analytical predictions. The five ingot slices are compared in terms of their grain orientations and grain boundary misorientations, indicating no obvious commonalities, which suggests that grain orientations develop randomly during solidification.

  14. Microstructural Characterization of Ni/YSZ Electrodes in a Solid Oxide Electrolysis Stack Tested for 9000 Hours

    DEFF Research Database (Denmark)

    Trini, Martina; Jørgensen, Peter Stanley; Hauch, Anne

    2017-01-01

    The effects of long-term operation in electrolysis mode on the microstructure of Ni/YSZ electrodes were investigated. The electrode structures were investigated in “as reduced” state and after 9000 h of operation in a 25 cell stack. Microstructural data were obtained by scanning electron microscopy...

  15. Microstructural Characterization and Mechanical Properties of Electron Beam Welded Joint of High Strength Steel Grade S690QL

    Directory of Open Access Journals (Sweden)

    Błacha S.

    2016-06-01

    Full Text Available In the paper the results of metallographic examination and mechanical properties of electron beam welded joint of quenched and tempered steel grade S690QL are presented. Metallographic examination revealed that the concentrated electron beam significantly affect the changes of microstructure in the steel. Parent material as a delivered condition (quenched and tempered had a bainitic-martensitic microstructure at hardness about 290 HV0.5. After welding, the microstructure of heat affected zone is composed mainly of martensite (in the vicinity of the fusion line of hardness 420 HV0.5. It should be noted, however, that the microstructure of steel in the heat affected zone varies with the distance from the fusion line. The observed microstructural changes were in accordance with the CCT-S transformation diagram for the examined steel.

  16. Mechanical and microstructural characterization of new nickel-free low modulus β-type titanium wires during thermomechanical treatments

    Energy Technology Data Exchange (ETDEWEB)

    Guillem-Martí, J. [Biomaterials, Biomechanics and Tissue Engineering Group, Department of Materials Science and Metallurgy, Technical University of Catalonia (UPC), ETSEIB, Av. Diagonal 647, 08028 Barcelona (Spain); Biomedical Research Networking Centre in Bioengineering, Biomaterials and Nanomedicine (CIBER-BBN), Campus Río Ebro, Edificio I+D Bloque 5, 1a planta, C/ Poeta Mariano Esquillor s/n, 50018 Zaragoza (Spain); Centre for Research in NanoEngineering (CRNE) – UPC, C/Pascual i Vila 15, 08028 Barcelona (Spain); Herranz-Díez, C. [Biomaterials, Biomechanics and Tissue Engineering Group, Department of Materials Science and Metallurgy, Technical University of Catalonia (UPC), ETSEIB, Av. Diagonal 647, 08028 Barcelona (Spain); Biomedical Research Networking Centre in Bioengineering, Biomaterials and Nanomedicine (CIBER-BBN), Campus Río Ebro, Edificio I+D Bloque 5, 1a planta, C/ Poeta Mariano Esquillor s/n, 50018 Zaragoza (Spain); Shaffer, J.E. [Fort Wayne Metals Research Products Corporation, 9609 Ardmore Avenue, 46809 Fort Wayne (United States); Gil, F.J. [Biomaterials, Biomechanics and Tissue Engineering Group, Department of Materials Science and Metallurgy, Technical University of Catalonia (UPC), ETSEIB, Av. Diagonal 647, 08028 Barcelona (Spain); Biomedical Research Networking Centre in Bioengineering, Biomaterials and Nanomedicine (CIBER-BBN), Campus Río Ebro, Edificio I+D Bloque 5, 1a planta, C/ Poeta Mariano Esquillor s/n, 50018 Zaragoza (Spain); Centre for Research in NanoEngineering (CRNE) – UPC, C/Pascual i Vila 15, 08028 Barcelona (Spain); and others

    2015-06-11

    NiTi alloy is the only practical shape memory alloy (SMA) in biomedical use because of its excellent mechanical stability and functionality. However, it is estimated that between 4.5% and 28.5% of the population are hypersensitive to nickel metal, with a higher prevalence in females. Therefore, developing nickel-free low modulus β-type titanium alloys showing shape memory or super elastic behavior would have a great interest in the biomaterials field. Homogeneous 127 μm diameter Ti25Hf21Nb wires were produced and compared to straight annealed Ti–50.8 at% Ni (Nitinol) and 90% cold-drawn 316L wires. Microstructural changes taking place during the heat treatment of cold-worked Ti25Hf21Nb wires were investigated. Large plastic deformation during wire drawing and subsequent annealing led to nano-crystallization and amorphization which may contribute to the observed superelasticity. Mechanical properties were characterized using cyclic uniaxial tension and rotary beam fatigue test modes. A modulus of elasticity of less than 60 GPa and axial recoverable strain of greater than 3% were observed with stress hysteresis resembling a reversible stress-induced martensitic transformation at higher temperatures. The new Ti25Hf21Nb alloy is an important candidate for developing Ni-free SMAs in the future.

  17. Comparative investigation of two-dimensional imaging methods and X-ray tomography in the characterization of microstructure

    Energy Technology Data Exchange (ETDEWEB)

    Bacaicoa, Inigo; Luetje, Martin [Kassel Univ. (Germany). Inst. of Materials Engineering, Quality and Reliability; Saelzer, Philipp [Kassel Univ. (Germany). Abt. Materialentwicklung und Verbundwerkstoffe; Umbach, Cristin [Kassel Univ. (Germany). Inst. for Structural Engineering; Brueckner-Foit, Angelika [Kassel Univ. (Germany). Inst. of Materials Engineering; Heim, Hans-Peter [Kassel Univ. (Germany). Plastics Engineering; Middendorf, Bernhard [Kassel Univ. (Germany). Dept. of Building Materials and Construction Chemistry

    2017-11-01

    The microstructural features of three different materials have been quantified by means of 2D image analysis and X-ray micro-computer tomography (CT) and the results were compared to determine the reliability of the 2D analysis in the material characterization. The 3D quantification of shrinkage pores and Fe-rich inclusions of an Al-Si-Cu alloy by X-ray tomography was compared with the statistical analysis of the 2D metallographic pictures and a significant difference in the results was found due to the complex morphology of shrinkage pores and Fe-rich particles. Furthermore, wood particles of a wood-plastic composite were measured by dynamic image analysis and X-ray tomography. Similar results were obtained for the maximum length of the particles, although the results of width differ considerably, which leads to a miscalculation of the particles aspect ratio. Finally, air voids of a foam concrete were investigated by the analysis of the 2D pictures in ImageJ and the results of the 2D circularity were compared with the values of the 3D elongation obtained by micro-computed tomography. The 3D analysis of the air voids in the foam concrete showed a more precise description of the morphology, although the 2D result are in good agreement with the results obtained by X-ray micro-tomography.

  18. Linking Material Properties and Microstructures to Characterize Damage Associated with an Underground Explosion in Granite

    Science.gov (United States)

    Wilson, J. E.; Broome, S.; Sussman, A. J.; Townsend, M.; Schultz-Fellenz, E. S.

    2013-12-01

    The Source Physics Experiment, conducted in granite in Nevada, is a series of explosive tests designed to study the generation and propagation of seismic waves. Extensive seismic monitoring and site rock characterization are being used to improve the predictive capability of models for detecting and characterizing underground explosions. Site rock characterization includes geomechanical and material properties testing, core-scale fracture identification, and optical microscopy studies. Geomechanical and material properties determined via laboratory testing of the site rocks include unconfined compressive strength, Young's modulus, Poisson's ratio, and bulk density. Detailed fracture mapping and characterization of meso- and micro-scale fractures in recovered cores are being conducted and include mineralization changes and the extent of crushed or fractured zone away from the source. We report on the analysis of microfractures in these cores, which provide a detailed and quantitative dataset on the extent and nature of damage in the recovered cores. Microfracture density and character (open, sealed, healed) are recorded in order to differentiate sets of microfractures associated with explosive tests. Densities (mf/mm) of open microfractures correlate with source-related damage, and increase from pre- to post-test samples. Microfracture densities are affected by pre-existing fractures, depending on fracture-zone mineralogy and alteration. These microfracture density data, linked to the bulk material properties, geomechanical properties, and the structural features of the rock at the core-scale, define a damage zone surrounding the source at depth. This link is essential to understanding how the bulk material properties manifest themselves in the rock and how that might affect energy propagation. Work by Los Alamos National Laboratory was sponsored by the National Nuclear Security Administration Award No. DE-AC52-06NA25946/NST10-NCNS-PD00. Work by National Security

  19. Microstructure Related Characterization of a-Si:H Thin Films PECVD Deposited under Varied Hydrogen Dilution

    Directory of Open Access Journals (Sweden)

    Veronika Vavrunkova

    2007-01-01

    Full Text Available We report on the structure and optical properties of hydrogenated silicon thin films deposited by plasma - enhanced chemical vapor deposition (PECVD from silane diluted with hydrogen in a wide dilution range. The samples deposited with dilutions below 30 were detected as amorphous hydrogenated silicon (a-Si:H with crystalline grains of several nanometers in size which represent the medium-range order of a-Si:H. The optical characterization confirmed increasing ordering with the increasing dilution. The optical band gap was observed to be increasing function of the dilution.

  20. Advanced Surface and Microstructural Characterization of Natural Graphite Anodes for Lithium Ion Batteries

    Energy Technology Data Exchange (ETDEWEB)

    Gallego, Nidia C [ORNL; Contescu, Cristian I [ORNL; Meyer III, Harry M [ORNL; Howe, Jane Y [ORNL; Meisner, Roberta Ann [ORNL; Payzant, E Andrew [ORNL; Lance, Michael J [ORNL; Yoon, Steve [A123 Systems, Inc.; Denlinger, Matthew [A123 Systems, Inc.; Wood III, David L [ORNL

    2014-01-01

    Natural graphite powders were subjected to a series of thermal treatments in order to improve the anode irreversible capacity loss (ICL) and capacity retention during long-term cycling of lithium ion batteries. A baseline thermal treatment in inert Ar or N2 atmosphere was compared to cases with a proprietary additive to the furnace gas environment. This additive substantially altered the surface chemistry of the natural graphite powders and resulted in significantly improved long-term cycling performance of the lithium ion batteries over the commercial natural graphite baseline. Different heat-treatment temperatures were investigated ranging from 950-2900 C with the intent of achieving the desired long-term cycling performance with as low of a maximum temperature and thermal budget as possible. A detailed summary of the characterization data is also presented, which includes X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Raman spectroscopy, and temperature-programed desorption mass spectroscopy (TPD-MS). This characterization data was correlated to the observed capacity fade improvements over the course of long-term cycling at high charge-discharge rates in full lithium-ion coin cells. It is believed that the long-term performance improvements are a result of forming a more stable solid electrolyte interface (SEI) layer on the anode graphite surfaces, which is directly related to the surface chemistry modifications imparted by the proprietary gas environment during thermal treatment.

  1. Electrochemical behavior and microstructural characterization of 1026 Ni-B coated steel

    Energy Technology Data Exchange (ETDEWEB)

    Contreras, A. [Instituto Mexicano del Petroleo, Eje Central Lazaro Cardenas Norte 152, Col. San Bartolo Atepehuacan, Mexico D.F. 07730 (Mexico)]. E-mail: acontrer@imp.mx; Leon, C. [Programa de investigacion en Ductos, Materiales y Corrosion, Universidad Michoacana de San Nicolas de Hidalgo, Apdo. Postal 888, Morelia Mich. 58000 (Mexico); Jimenez, O. [Programa de investigacion en Ductos, Materiales y Corrosion, Universidad Michoacana de San Nicolas de Hidalgo, Apdo. Postal 888, Morelia Mich. 58000 (Mexico); Sosa, E. [Instituto Mexicano del Petroleo, Eje Central Lazaro Cardenas Norte 152, Col. San Bartolo Atepehuacan, Mexico D.F. 07730 (Mexico); Perez, R. [Instituto Mexicano del Petroleo, Eje Central Lazaro Cardenas Norte 152, Col. San Bartolo Atepehuacan, Mexico D.F. 07730 (Mexico)

    2006-11-15

    Ni-B coatings have been deposited on the surfaces of commercial steels (SAE-1026). The depositions were carried out using the electroless plating technique employing a nickel chloride solution with borane-dimethylamine as the reducing agent. These specimens were subsequently heat treated at different temperatures (300-500 deg. C) and different periods of time. The obtained coating thickness was in the order of approximately 1.5 {mu}m. X-ray diffraction (XRD) and scanning electron microscopy (SEM) techniques were used to characterize the structure and superficial morphology of the coatings. Phases like Ni, Ni{sub 3}B and Ni{sub 4}B{sub 3} were observed through X-ray diffraction and confirmed by differential scanning calorimeter (DSC) studies. Some of the precipitated phases have been structurally characterized. The corrosion behavior of the coated surfaces was carried out by electrochemical impedance spectroscopy (EIS) using electrolytic sodium chlorine solutions with pH 2 and 7. The EIS results showed an active corrosion mechanism in acid solution while diffusion-reaction phenomena are predominant in neutral solution.

  2. Characterization of Porphyrin-Co(III)-'Nitrene Radical' Species Relevant in Catalytic Nitrene Transfer Reactions.

    Science.gov (United States)

    Goswami, Monalisa; Lyaskovskyy, Volodymyr; Domingos, Sérgio R; Buma, Wybren Jan; Woutersen, Sander; Troeppner, Oliver; Ivanović-Burmazović, Ivana; Lu, Hongjian; Cui, Xin; Zhang, X Peter; Reijerse, Edward J; DeBeer, Serena; van Schooneveld, Matti M; Pfaff, Florian Felix; Ray, Kallol; de Bruin, Bas

    2015-04-29

    To fully characterize the Co(III)-'nitrene radical' species that are proposed as intermediates in nitrene transfer reactions mediated by cobalt(II) porphyrins, different combinations of cobalt(II) complexes of porphyrins and nitrene transfer reagents were combined, and the generated species were studied using EPR, UV-vis, IR, VCD, UHR-ESI-MS, and XANES/XAFS measurements. Reactions of cobalt(II) porphyrins 1(P1) (P1 = meso-tetraphenylporphyrin (TPP)) and 1(P2) (P2 = 3,5-Di(t)Bu-ChenPhyrin) with organic azides 2(Ns) (NsN3), 2(Ts) (TsN3), and 2(Troc) (TrocN3) led to the formation of mono-nitrene species 3(P1)(Ns), 3(P2)(Ts), and 3(P2)(Troc), respectively, which are best described as [Co(III)(por)(NR″(•-))] nitrene radicals (imidyl radicals) resulting from single electron transfer from the cobalt(II) porphyrin to the 'nitrene' moiety (Ns: R″ = -SO2-p-C6H5NO2; Ts: R″ = -SO2C6H6; Troc: R″ = -C(O)OCH2CCl3). Remarkably, the reaction of 1(P1) with N-nosyl iminoiodane (PhI═NNs) 4(Ns) led to the formation of a bis-nitrene species 5(P1)(Ns). This species is best described as a triple-radical complex [(por(•-))Co(III)(NR″(•-))2] containing three ligand-centered unpaired electrons: two nitrene radicals (NR″(•-)) and one oxidized porphyrin radical (por(•-)). Thus, the formation of the second nitrene radical involves another intramolecular one-electron transfer to the "nitrene" moiety, but now from the porphyrin ring instead of the metal center. Interestingly, this bis-nitrene species is observed only on reacting 4(Ns) with 1(P1). Reaction of the more bulky 1(P2) with 4(Ns) results again in formation of mainly mono-nitrene species 3(P2)(Ns) according to EPR and ESI-MS spectroscopic studies. The mono- and bis-nitrene species were initially expected to be five- and six-coordinate species, respectively, but XANES data revealed that both mono- and bis-nitrene species are six-coordinate O(h) species. The nature of the sixth ligand bound to cobalt(III) in the

  3. Microstructural characterization of PH 13-8 Mo maraging steels; Mikrostrukturelle Charakterisierung von PH 13-8 Mo Maraging-Staehlen

    Energy Technology Data Exchange (ETDEWEB)

    Schnitzer, Ronald; Hochfellner, Rainer; Noehrer, Matthias [Christian Doppler Lab. for Early Stages of Precipitation, Leoben (Austria); Schober, Michael; Clemens, Helmut [Dept. Metallkunde und Werkstoffpruefung, Montanuniversitaet Leoben (Austria); Zinner, Silvia [Boehler Edelstahl GmbH und Co. KG, Kapfenberg (Austria); Leitner, Harald [Christian Doppler Lab. for Early Stages of Precipitation, Leoben (Austria); Dept. Metallkunde und Werkstoffpruefung, Montanuniversitaet Leoben (Austria)

    2009-10-15

    Maraging steels are characterized by an excellent combination of high strength coupled with an acceptable level of ductility. Its microstructure consists of a martensitic matrix with intermetallic precipitates and a low amount of austenite, the latter varying according to heat treatment and the composition of the alloy. In this paper methods and processes for comprehensively characterizing the microstructure of maraging steels are set out. Apart from the prior austenite grain size, the martensite and the intermetallic phases these also relate to the reverted austenite formed during heat treatment. In addition to the description of the growth of austenite grains, with the aid of the law of isothermal grain growth, high-resolution methods such as electron back-scattered diffraction (EBSD), transmission electron microscopy (TEM) and atom probe tomography (APT) are employed. (orig.)

  4. Microstructural Characterization of Y{sub 2}O{sub 3} ODS-Fe-Cr Model Alloy s

    Energy Technology Data Exchange (ETDEWEB)

    De Castro, V.; Jenkins, M.L. [Oxford Univ., Dept. of Materials (United Kingdom); Leguey, T.; Mufioz, A.; Pareja, R.; Monge, M.A. [Madrid Univ. Carlos 3, Dept. de Fisica (Spain)

    2007-07-01

    Full text of publication follows: Reduced activation ferritic/martensitic (RAFM) steels with Cr contents ranging between 9-12 wt% are promising candidates for use as structural materials in future fusion reactors. They are likely to be superior to austenitic steels because of their better thermal properties and higher swelling resistance. A major concern of these materials is their maximum service temperature, as this determines the overall efficiency of the reactor. It has been demonstrated that one way to increase this temperature is to homogeneously disperse hard nano-sized oxide particles, such as Y{sub 2}O{sub 3}, into the steel matrix. Oxide dispersion strengthened (ODS) steels produced by mechanical milling and hot isostatic pressing (HIP ) are considered as potential structural materials for fusion reactors. In Europe, efforts have been focused on the ODS-RAFM-9CrW steel EUROFER. These ODS steels show good tensile and creep properties, acceptable ductility, but poor impact properties. Microstructural characterization of real steels, especially of the structures of oxide/steel matrix interfaces which play an important role in the performance of the material, is a difficult task. In the present work we have fabricated and characterised a simpler model ODS system based on a Fe-Cr binary alloy, in the belief that this will help us better to understand complex ODS-RAFM steels. Two Fe-12wt% Cr batches, one containing 0.3 wt% Y{sub 2}O{sub 3} and the other Y{sub 2}O{sub 3} free have been produced by milling plus compaction by HIP. These materials are being characterized by X-ray diffraction, electron microscopy and atom probe field ion microscopy. Results will be compared with those obtained for ODS-EUROFER produced under the same conditions. (authors)

  5. Microstructural and mechanical characterizations of steel tubes joined by transient liquid phase bonding using an amorphous Fe–B–Si interlayer

    Energy Technology Data Exchange (ETDEWEB)

    Di Luozzo, Nicolas, E-mail: nicolasdiluozzo@gmail.com [Laboratorio de Sólidos Amorfos, INTECIN, Facultad de Ingeniería, Universidad de Buenos Aires – CONICET, Paseo Colón 850, C1063ACV Buenos Aires (Argentina); Laboratoire des Matériaux et du Génie Physique (CNRS UMR 5628), Grenoble Institute of Technology, MINATEC, Grenoble Cedex 1 (France); Doisneau, Béatrice; Boudard, Michel [Laboratoire des Matériaux et du Génie Physique (CNRS UMR 5628), Grenoble Institute of Technology, MINATEC, Grenoble Cedex 1 (France); Fontana, Marcelo; Arcondo, Bibiana [Laboratorio de Sólidos Amorfos, INTECIN, Facultad de Ingeniería, Universidad de Buenos Aires – CONICET, Paseo Colón 850, C1063ACV Buenos Aires (Argentina)

    2014-12-05

    Highlights: • We joined steel tubes by means of TLPB process using a Fe–B–Si foil as interlayer. • We characterized both microstructure and mechanical properties of the joint. • The microstructure at the joint consists only of ferrite grains. • Evidences of non-epitaxial solidification were found. • Both tensile and hardness tests show the soundness of the joint. - Abstract: In this work the transient liquid phase bonding process was successfully used to join seamless carbon steel tubes using an amorphous Fe–B–Si foil as interlayer. The tubes were aligned with their butted surfaces in contact with the interlayer and the entire assembly was heated by means of an induction furnace under a reducing atmosphere. The temperature was raised to the process temperature (≈1300 °C) and then held for 7 min. The joining process was performed under a pressure of 5 MPa. The joined tubes microstructures were characterized by direct observations – scanning electron microscopy – and diffraction techniques – electron backscatter diffraction. Chemical analysis was performed by electron probe microanalysis. The joint region (JR) presents only ferrite grains - in contrast with the heat affected zone (HAZ) and the base metal (BM), whose microstructures consist of ferrite and cementite. Si content at the JR was precisely determined by chemical profiling, showing higher concentrations of Si compared with the HAZ and BM. These results are in accordance with the fact that the cementite is unable to form in Si enriched zones. Also, ferrite grains at the JR present high-angle grain boundaries with respect to the grains of the HAZ. Tensile tests show that the joined tubes failed away from the bond, at the HAZ, and reached 96% of the ultimate tensile strength of the BM, in the as-bonded condition. Microindentation hardness profiles across the bonding zone are in agreement with the observed microstructures at the different zones of the bond region.

  6. HRTEM Microstructural Characterization of β-WO3 Thin Films Deposited by Reactive RF Magnetron Sputtering

    Science.gov (United States)

    Faudoa-Arzate, A.; Arteaga-Durán, A.; Saenz-Hernández, R.J.; Botello-Zubiate, M.E.; Realyvazquez-Guevara, P.R.; Matutes-Aquino, J.A.

    2017-01-01

    Though tungsten trioxide (WO3) in bulk, nanosphere, and thin film samples has been extensively studied, few studies have been dedicated to the crystallographic structure of WO3 thin films. In this work, the evolution from amorphous WO3 thin films to crystalline WO3 thin films is discussed. WO3 thin films were fabricated on silicon substrates (Si/SiO2) by RF reactive magnetron sputtering. Once a thin film was deposited, two successive annealing treatments were made: an initial annealing at 400 °C for 6 h was followed by a second annealing at 350 °C for 1 h. Film characterization was carried out by X-ray diffraction (XRD), high-resolution electron transmission microscopy (HRTEM), scanning electron microscopy (SEM), and atomic force microscopy (AFM) techniques. The β-WO3 final phase grew in form of columnar crystals and its growth plane was determined by HRTEM. PMID:28772559

  7. Advanced characterization of MIMAS MOX fuel microstructure to quantify the HBS formation

    Energy Technology Data Exchange (ETDEWEB)

    Bouloré, Antoine, E-mail: antoine.boulore@cea.fr [CEA, DEN, DEC Fuel Research Department, Cadarache, F13108 Saint-Paul-lez-Durance (France); Aufore, Laurence; Federici, Eric [CEA, DEN, DEC Fuel Research Department, Cadarache, F13108 Saint-Paul-lez-Durance (France); Blanpain, Patrick [AREVA NP SAS, 10 rue Juliette Récamier, F-69456 Lyon (France); Blachier, Rémi [EDF, SEPTEN, 12-14 Av. Dutrievoz, F-69628 Villeurbanne (France)

    2015-01-15

    Highlights: • An advanced characterization of MIMAS MOX fuel based only on fresh fuel pellet characterization. • A probabilistic approach to model the High Burnup Structure formation in oxide fuels. • Validation of the method by comparing to experimental data obtained on fuel irradiated in the Halden reactor. - Abstract: Fission gas behaviour in accidental situations is closely related to the location of fission gas before the accident. More precisely, most of the fission gas in intergranular position is released during the accident and HBS zones contribute a lot to this intergranular quantity. So a methodology to characterize the HBS zones a priori from examination of unirradiated pellet has been developed at CEA. Characterization of plutonium distribution in MIMAS MOX fresh fuel pellets can be performed by image analysis on 1 mm{sup 2} X-ray mappings of plutonium acquired using Electron Probe Micro Analysis (EPMA). The specific software developed to describe the fuel using Pu X-ray mapping (ANACONDA) has been improved in order to simulate the fission products (FP) production and recoil during a given irradiation of the fuel, taking into account the evolution of the plutonium due to neutron irradiation. This simulation results from calculations with our fuel performance code ALCYONE combined with image processing. The final result is a mapping of local burn-up, but also the distribution of the relative FP concentration as a function of the local burn-up. A validation of this simulation process has been done by comparing the simulated mapping of neodymium to one measured on the same fuel batch after irradiation. Using previous studies of mechanisms for HBS formation, a probabilistic criterion for HBS formation has been proposed, based on the EPMA measurements of the decrease of the xenon signal as a function of the local burn-up. Combining the simulated FP cartography with this probabilistic HBS formation criterion, it is possible to calculate the surface

  8. Characterization of thermal transport in one-dimensional microstructures using Johnson noise electro-thermal technique

    Science.gov (United States)

    Liu, Jing; Wang, Xinwei

    2015-06-01

    This work reports on the development of a Johnson noise electro-thermal (JET) technique to directly characterize the thermal conductivity of one-dimensional micro-/nanoscale materials. In this technique, the to-be-measured micro-/nanoscale sample is connected between two electrodes and is subjected to steady-state Joule heating. The average temperature rise of the sample is evaluated by simultaneously measuring the Johnson noise over it and its electrical resistance. The system's Johnson noise measurement accuracy is evaluated by measuring the Boltzmann constant ( k B). Our measured k B value (1.375 × 10-23 J/K) agrees very well with the reference value of 1.381 × 10-23 J/K. The temperature measurement accuracy based on Johnson noise is studied against the resistance temperature detector method, and sound agreement (4 %) is obtained. The thermal conductivity of a glass fiber with a diameter of 8.82 μm is measured using the JET technique. The measured value 1.20 W/m K agrees well with the result using a standard technique in our laboratory. The JET technique provides a very compelling way to characterize the thermophysical properties of micro-/nanoscale materials without calibrating the sample's resistance-temperature coefficient, thereby eliminating the effect of resistance drift/change during measurement and calibration. Since JET technique does not require resistance-temperature correlation, it is also applicable to semi-conductive materials which usually have a nonlinear I- V relation.

  9. Dynamical microstructure formation in 3D directional solidification of transparent model alloys: in situ characterization in DECLIC Directional Solidification Insert under diffusion transport in microgravity

    Science.gov (United States)

    Bergeon, N.; Mota, F. L.; Chen, L.; Tourret, D.; Debierre, J. M.; Guérin, R.; Karma, A.; Billia, B.; Trivedi, R.

    2015-06-01

    To clarify and characterize the fundamental physical mechanisms active in the dynamical formation of three-dimensional (3D) arrays of cells and dendrites under diffusive growth conditions, in situ monitoring of series of experiments on transparent model alloy succinonitrile - 0.24 wt% camphor was carried out under low gravity in the DECLIC Directional Solidification Insert on-board the International Space Station. These experiments offered the very unique opportunity to in situ observe and characterize the whole development of the microstructure in extended 3D patterns. The experimental methods will be first briefly described, including in particular the observation modes and the image analysis procedures developed to quantitatively characterize the patterns. Microgravity environment provided the conditions to get quantitative benchmark data: homogeneous patterns corresponding to homogeneous values of control parameters along the whole interface were obtained. The sequence of microstructure formation will be presented as well as the evolution of the primary spacing which is one of the most important pattern characteristic. Time evolution of this primary spacing during the microstructure development will be analysed to identify the mechanisms of spacing selection and adjustment; the importance of the macroscopic interfacial curvature will be pointed out.

  10. Additive Manufacturing of IN100 Superalloy Through Scanning Laser Epitaxy for Turbine Engine Hot-Section Component Repair: Process Development, Modeling, Microstructural Characterization, and Process Control

    Science.gov (United States)

    Acharya, Ranadip; Das, Suman

    2015-09-01

    This article describes additive manufacturing (AM) of IN100, a high gamma-prime nickel-based superalloy, through scanning laser epitaxy (SLE), aimed at the creation of thick deposits onto like-chemistry substrates for enabling repair of turbine engine hot-section components. SLE is a metal powder bed-based laser AM technology developed for nickel-base superalloys with equiaxed, directionally solidified, and single-crystal microstructural morphologies. Here, we combine process modeling, statistical design-of-experiments (DoE), and microstructural characterization to demonstrate fully metallurgically bonded, crack-free and dense deposits exceeding 1000 μm of SLE-processed IN100 powder onto IN100 cast substrates produced in a single pass. A combined thermal-fluid flow-solidification model of the SLE process compliments DoE-based process development. A customized quantitative metallography technique analyzes digital cross-sectional micrographs and extracts various microstructural parameters, enabling process model validation and process parameter optimization. Microindentation measurements show an increase in the hardness by 10 pct in the deposit region compared to the cast substrate due to microstructural refinement. The results illustrate one of the very few successes reported for the crack-free deposition of IN100, a notoriously "non-weldable" hot-section alloy, thus establishing the potential of SLE as an AM method suitable for hot-section component repair and for future new-make components in high gamma-prime containing crack-prone nickel-based superalloys.

  11. Microstructural characterization of an SA508–309L/308L–316L domestic dissimilar metal welded safe-end joint

    Energy Technology Data Exchange (ETDEWEB)

    Ming, Hongliang; Zhang, Zhiming; Wang, Jianqiu, E-mail: wangjianqiu@imr.ac.cn; Han, En-Hou; Ke, Wei

    2014-11-15

    The microstructure of an SA508–309L/308L–316L domestic dissimilar metal welded safe-end joint was characterized in this work by optical microscopy, scanning electron microscopy (with electron back scattering diffraction) and micro-hardness testing. Epitaxial growth and competitive growth are evident in the 308L–316L fusion boundary regions. A martensite layer, carbon-depleted zones, and type-II and type-I boundaries are found in the SA508–309L fusion boundary regions, while only martensite and austenite mixed zones are observed in the SA508–308L fusion boundary regions. The microstructure near the fusion boundary and the microstructure transition in the SA508 heat affected zone are quite complex. Both for SA508–309L/308L and 308L–316L, the highest residual strain is located on the outside of the weldment. The residual strain and the grain boundary character distribution change with increasing distance from the fusion boundary in the heat affected zone of 316L. Micro-hardness measurements also reveal non-uniform mechanical properties across the weldment. - Highlights: • The microstructure of SA508 HAZ, especially near the FB, is very complex. • The outside of the dissimilar metal welded joint has the highest residual. • The micro-hardness distributions along the DMWJ are non-uniform.

  12. Surface Morphology of Fe(III)-Porphyrin Thin Layers as Characterized by Atomic Force Microscopy

    OpenAIRE

    Utari Utari; Kusumandari Kusumandari; Budi Purnama; Mudasir Mudasir; Kamsul Abraha

    2016-01-01

    Surface morphology of Fe(III)–porphyrin thin layers was studied using atomic force microscopy. The thin layer samples used in these experiments were deposited by spin coating methods on indium–tin-oxide substrates at room temperature under atmospheric conditions. Variations of thin layer of Fe(III)-porphyrin were done by modifying the rotational speed and the concentration of the solution. The experimental results demonstrated that the Fe(III)–porphyrin layers were observed as discrete nanomo...

  13. Characterization of dual-phase steel microstructure by combined submicrometer EBSD and EPMA carbon measurements.

    Science.gov (United States)

    Pinard, Philippe T; Schwedt, Alexander; Ramazani, Ali; Prahl, Ulrich; Richter, Silvia

    2013-08-01

    Electron backscatter diffraction (EBSD) and electron probe microanalysis (EPMA) measurements are combined to characterize an industrial produced dual-phase steel containing some bainite fraction. High-resolution carbon mappings acquired on a field emission electron microprobe are utilized to validate and improve the identification of the constituents (ferrite, martensite, and bainite) performed by EBSD using the image quality and kernel average misorientation. The combination eliminates the ambiguity between the identification of bainite and transformation-induced dislocation zones, encountered if only the kernel average misorientation is considered. The detection of carbon in high misorientation regions confirms the presence of bainite. These results are corroborated by secondary electron images after nital etching. Limitations of this combined method due to differences between the spatial resolution of EBSD and EPMA are assessed. Moreover, a quantification procedure adapted to carbon analysis is presented and used to measure the carbon concentration in martensite and bainite on a submicrometer scale. From measurements on reference materials, this method gives an accuracy of 0.02 wt% C and a precision better than 0.05 wt% C despite unavoidable effects of hydrocarbon contamination.

  14. Microstructural characterization of halite inclusion in a glass-bonded ceramic waste form.

    Energy Technology Data Exchange (ETDEWEB)

    Luo, J. S.; Ebert, W. L.

    2000-12-14

    A glass-bonded ceramic waste form is being developed to immobilize radioactively contaminated chloride waste salts generated during the conditioning of spent sodium-bonded nuclear fuel for disposal. The waste salt is first mixed with zeolite A to occlude the salt into cavities in the zeolite structure. The salt-loaded zeolite is then mixed with a borosilicate glass and consolidated by hot isostatic pressing. During this process, the zeolite converts to the mineral sodalite, which retains most of the waste salt, and small amounts of halite are generated. Halite inclusions have been observed within micron- to submicron-sized pores that form within the glass phase in the vicinity of the sodalite/glass interface. These inclusions are important because they may contain small amounts of radionuclide contaminants (eg {sup 135}Cs and {sup 129}I),and may affect the corrosion behavior of the waste form. Optical microscopy, scanning electron microscopy, and transmission electron microscopy were used to characterize the chemical nature and distribution of halite inclusions in the waste form.

  15. FEA and microstructure characterization of a one-piece Y-TZP abutment.

    Science.gov (United States)

    da Silva, Lucas Hian; Ribeiro, Sebastião; Borges, Alexandre Luís Souto; Cesar, Paulo Francisco; Tango, Rubens Nisie

    2014-11-01

    The most important drawback of dental implant/abutment assemblies is the need for a fixing screw. This study aimed to develop an esthetic one-piece Y-TZP abutment to suppress the use of the screw. Material characterization was performed using a bar-shaped specimen obtained by slip-casting to validate the method prior to prototype abutment fabrication by the same process. The mechanical behavior of the prototype abutment was verified and compared with a conventional abutment by finite element analysis (FEA). The abutment was evaluated by micro-CT analysis and its density was measured. FEA showed stress concentration at the first thread pitch during installation and in the cervical region during oblique loading for both abutments. However, stress concentration was observed at the base of the screw head and stem in the conventional abutment. The relative density for the fabricated abutment was 95.68%. Micro-CT analysis revealed the presence of elongated cracks with sharp edges over the surface and porosity in the central region. In the light of these findings, the behavior of a one-piece abutment is expected to be better than that of the conventional model. New studies should be conducted to clarify the performance and longevity of this one-piece Y-TZP abutment. Copyright © 2014 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

  16. Synthesis, characterization and single crystal X-ray analysis of chlorobis(N,N-dimethyldithiocarbamato-S,S′)antimony(III)

    OpenAIRE

    Chauhan, H.P.S.; Jaswant Carpenter

    2015-01-01

    The title compound chlorobis(N,N-dimethyldithiocarbamato-S,S′)antimony(III) has been prepared in distilled acetonitrile and characterized by physicochemical [melting point and molecular weight determination, elemental analysis (C, H, N, S & Sb)], spectral [FT–IR, far IR, NMR (1H & 13C)] studies. The crystal and molecular structure was further confirmed using single crystal X-ray diffraction analysis which features a five-coordinate geometry for antimony(III) within a ClS4 donor set. The disto...

  17. Synthesis and characterization of metal soaps of lanthanides (III); Sintese e caracterizacao de saboes metalicos de lantanidios (III)

    Energy Technology Data Exchange (ETDEWEB)

    Payolla, Filipe Boccato; Ribeiro, Sidney Jose Lima; Massbni, Antonio Carlos [Universidade Estadual Paulista Julio de Mesquita Filho (UNESP), Araraquara, SP (Brazil). Instituto de Quimica; Centro Universitario de Araraquara (UNIARA), Araraquara, SP (Brazil)

    2015-07-01

    The present study describes synthesis and partial characterization of Eu{sup 3+}, Nd{sup 3+}, Dy{sup 3+}, Tb{sup 3+} and Yb{sup 3+} behenate complexes. The compounds were analyzed using IR-Spectroscopy, TG-DTG, DSC, elemental analysis, XRD, luminescence and SEM. The results show the purity of the compounds. The XRD analysis and the SEM images show the high crystallinity of the complexes. TG-DTG and DSC analyses do not show a liquid crystal behavior, as occurs with other lanthanide metallic soaps. The mass loses until 1000° C show that the compounds lose ligand fragments at specific temperatures. XRD of the residues are compatible with the respective lanthanide oxides. The luminescence analysis shows that the Eu{sup 3+}, Nd{sup 3+} and Tb{sup 3+} complexes presents appreciable emission. The Judd-Ofelt parameters obtained are compatible with the values found in the literature. It was not possible to obtain the complexes in a glass-form because it is difficult to prevent the crystallization of the complexes even using liquid nitrogen. The XDR data indicate that one of the complexes axis has 52 Å of length, agreeing with a structure containing behenate-lanthanide ion-behenate. The structures of the complexes were not fully elucidated and more analyses are necessary. The complexes presented a molar ratio of 3:1 (L:M) and were formulated as Bh{sub 3}Eu, Bh{sub 3}Nd, Bh{sub 3}Dy, Bh{sub 3}Tb e Bh{sub 3}Yb (Bh = behenate anion). (author)

  18. Microstructural and electrical characterizations of tungsten-doped La2Mo2O9 prepared by spray pyrolysis

    DEFF Research Database (Denmark)

    Baqué, Laura; Vega-Castillo, Jesús; Georges, Samuel

    2013-01-01

    by applying different sintering programs starting from La2Mo2 − xWxO9 powders (x=0 and 1.3) obtained by SP and SSR processes. The electrical properties of these ionic conductors were analyzed by Electrochemical Impedance Spectroscopy (EIS) and correlated with microstructural observations. No significant...... variation of the electrical properties of these ionic conductors was found as compared to conventional ceramics with remarkable microstructural differences....

  19. Synthesis, Characterization, and Antifungal Studies of Cr(III) Complex of Norfloxacin and Bipiridyl Ligand

    National Research Council Canada - National Science Library

    Debnath, Anamika; Hussain, Firasat; Masram, Dhanraj T

    2014-01-01

    A novel slightly distorted octahedral complex of Cr(III) of norfloxacin (Nor) with the formula [Cr(III)(Nor)(Bipy)Cl2]Cl·2CH3OH has been synthesized hydrothermally in the presence of a N-containing heterocyclic compound 2,2'-bipyridyl...

  20. Superlattice Microstructured Optical Fiber

    Directory of Open Access Journals (Sweden)

    Ming-Leung Vincent Tse

    2014-06-01

    Full Text Available A generic three-stage stack-and-draw method is demonstrated for the fabrication of complex-microstructured optical fibers. We report the fabrication and characterization of a silica superlattice microstructured fiber with more than 800 rhomboidally arranged air-holes. A polarization-maintaining fiber with a birefringence of 8.5 × 10−4 is demonstrated. The birefringent property of the fiber is found to be highly insensitive to external environmental effects, such as pressure.

  1. Thermal and Microstructure Characterization of Zn-Al-Si Alloys and Chemical Reaction with Cu Substrate During Spreading

    Science.gov (United States)

    Berent, Katarzyna; Pstruś, Janusz; Gancarz, Tomasz

    2016-08-01

    The problems associated with the corrosion of aluminum connections, the low mechanical properties of Al/Cu connections, and the introduction of EU directives have forced the potential of new materials to be investigated. Alloys based on eutectic Zn-Al are proposed, because they have a higher melting temperature (381 °C), good corrosion resistance, and high mechanical strength. The Zn-Al-Si cast alloys were characterized using differential scanning calorimetry (DSC) measurements, which were performed to determine the melting temperatures of the alloys. Thermal linear expansion and electrical resistivity measurements were performed at temperature ranges of -50 to 250 °C and 25 to 300 °C, respectively. The addition of Si to eutectic Zn-Al alloys not only limits the growth of phases at the interface of liquid solder and Cu substrate but also raises the mechanical properties of the solder. Spreading test on Cu substrate using eutectic Zn-Al alloys with 0.5, 1.0, 3.0, and 5.0 wt.% of Si was studied using the sessile drop method in the presence of QJ201 flux. Spreading tests were performed with contact times of 1, 8, 15, 30, and 60 min, and at temperatures of 475, 500, 525, and 550 °C. After cleaning the flux residue from solidified samples, the spreadability of Zn-Al-Si on Cu was determined. Selected, solidified solder/substrate couples were cross-sectioned, and the interfacial microstructures were studied using scanning electron microscopy and energy dispersive x-ray spectroscopy. The growth of the intermetallic phase layer was studied at the solder/substrate interface, and the activation energy of growth of Cu5Zn8, CuZn4, and CuZn phases were determined.

  2. Synthesis, characterization and single crystal X-ray analysis of chlorobis(N,N-dimethyldithiocarbamato-S,S′antimony(III

    Directory of Open Access Journals (Sweden)

    H.P.S. Chauhan

    2015-07-01

    Full Text Available The title compound chlorobis(N,N-dimethyldithiocarbamato-S,S′antimony(III has been prepared in distilled acetonitrile and characterized by physicochemical [melting point and molecular weight determination, elemental analysis (C, H, N, S & Sb], spectral [FT–IR, far IR, NMR (1H & 13C] studies. The crystal and molecular structure was further confirmed using single crystal X-ray diffraction analysis which features a five-coordinate geometry for antimony(III within a ClS4 donor set. The distortion in the co-planarity of ClSbS3 evidences the stereochemical influence exerts by the lone pair of electrons on antimony(III. Two centrosymmetrically related molecule held together via C–H···Cl secondary interaction result in molecular aggregation of the compound.

  3. Bone fracture characterization under mixed-mode I+II loading using the single leg bending test.

    Science.gov (United States)

    Pereira, F A M; de Moura, M F S F; Dourado, N; Morais, J J L; Dias, M I R

    2014-11-01

    Fracture under mixed-mode I+II was induced in bovine cortical bone tissue using a developed miniaturized version of the single leg bending test (SLB). Due to the difficulty in crack length monitoring in the course of the test, an equivalent crack method based on specimen compliance and beam theory was adopted as a data reduction scheme. The method was applied to the experimental results in order to obtain the Resistance curves in each loading mode. The determined fracture energy is well described by an energetic power law whose exponent is below one, which means that the linear energetic criterion is not applicable to this material. The proposed procedure was numerically validated by means of a cohesive mixed-mode I+II damage model with bilinear softening. It was concluded that the miniaturized version of the SLB test is adequate for mixed-mode I+II fracture characterization of bone for a constant mode ratio.

  4. Synthesis and characterization of chromium(III) Schiff base complexes: antimicrobial activity and its electrocatalytic sensing ability of catechol.

    Science.gov (United States)

    Kumar, S Praveen; Suresh, R; Giribabu, K; Manigandan, R; Munusamy, S; Muthamizh, S; Narayanan, V

    2015-03-15

    A series of acyclic Schiff base chromium(III) complexes were synthesized with the aid of microwave irradiation method. The complexes were characterized on the basis of elemental analysis, spectral analysis such as UV-Visible, Fourier transform infrared (FT-IR), nuclear magnetic resonance (NMR), electron paramagnetic resonance (EPR) spectroscopies and electrospray ionization (ESI) mass spectrometry. Electrochemical analysis of the complexes indicates the presence of chromium ion in +3 oxidation state. Cr (III) ion is stabilized by the tetradentate Schiff base ligand through its nitrogen and phenolic oxygen. From the spectral studies it is understood that the synthesized chromium(III) complexes exhibits octahedral geometry. Antimicrobial activity of chromium complexes was investigated towards the Gram positive and Gram negative bacteria. In the present work, an attempt was made to fabricate a new kind of modified electrode based on chromium Schiff base complexes for the detection of catechol at nanomolar level. Copyright © 2014 Elsevier B.V. All rights reserved.

  5. Growth and structural characterization of III-V nanowires grown by molecular beam epitaxy

    Energy Technology Data Exchange (ETDEWEB)

    Dheeraj, D.L.

    2010-10-15

    Heterostructured semiconductor nanowires (NWs) have attracted considerable attention in recent years because of their potential in future nano-electronic and nano-photonic device applications. NWs are usually grown by vapor-liquid-solid (VLS) growth mechanism using techniques such as metal-organic vapor phase epitaxy, chemical beam epitaxy and molecular beam epitaxy (MBE). Of all the available techniques, MBE is known to be the technique which yields highest purity materials. In this study, the growth of GaAs NWs, GaAsSb NWs, as well as GaAs/GaAsSb axial and GaAs/AlGaAs radial heterostructured NWs on GaAs(111)B substrates by MBE is demonstrated. The structural and optical properties of the NWs grown are characterized by electron microscopy techniques such as scanning and transmission electron microscopy, and micro-photoluminescence, respectively. Firstly, the optimum growth conditions to obtain rod shaped GaAs NWs on GaAs(111)B substrates by MBE is determined. It has been found that in-addition to the V/III ratio and substrate temperature, buffer growth conditions also play an important role on the orientation of the NWs. The effect of V/III ratio, substrate temperature, and the arsenic species (As{sub 2}/As{sub 4}) on the morphology of GaAs NWs has been determined. Transmission electron microscopy (TEM) characterization of NWs revealed that GaAs in NW form exhibit wurtzite (WZ) crystal phase in contrast to zinc blende (ZB) phase adapted in its bulk form. Since WZ crystal phase is a metastable phase of GaAs, the WZ GaAs NWs often exhibit stacking faults. The stacking faults are known to be a detrimental problem, if not properly controlled. To gain more insight on the growth kinetics of GaAs NWs grown by MBE, several samples such as GaAs NWs grown for different time durations, and GaAs NWs with three GaAsSb inserts, where GaAsSb inserts acts as markers, have been grown. Interestingly, the growth rates of the GaAs segments and GaAsSb inserts were observed to vary

  6. Modeling, Growth and Characterization of III-V and Dilute Nitride Antimonide Materials and Solar Cells

    Science.gov (United States)

    Maros, Aymeric

    III-V multijunction solar cells have demonstrated record efficiencies with the best device currently at 46 % under concentration. Dilute nitride materials such as GaInNAsSb have been identified as a prime choice for the development of high efficiency, monolithic and lattice-matched multijunction solar cells as they can be lattice-matched to both GaAs and Ge substrates. These types of cells have demonstrated efficiencies of 44% for terrestrial concentrators, and with their upright configuration, they are a direct drop-in product for today's space and concentrator solar panels. The work presented in this dissertation has focused on the development of relatively novel dilute nitride antimonide (GaNAsSb) materials and solar cells using plasma-assisted molecular beam epitaxy, along with the modeling and characterization of single- and multijunction solar cells. Nitrogen-free ternary compounds such as GaInAs and GaAsSb were investigated first in order to understand their structural and optical properties prior to introducing nitrogen. The formation of extended defects and the resulting strain relaxation in these lattice-mismatched materials is investigated through extensive structural characterization. Temperature- and power-dependent photoluminescence revealed an inhomogeneous distribution of Sb in GaAsSb films, leading to carrier localization effects at low temperatures. Tuning of the growth parameters was shown to suppress these Sb-induced localized states. The introduction of nitrogen was then considered and the growth process was optimized to obtain high quality GaNAsSb films lattice-matched to GaAs. Near 1-eV single-junction GaNAsSb solar cells were produced. The best devices used a p-n heterojunction configuration and demonstrated a current density of 20.8 mA/cm2, a fill factor of 64 % and an open-circuit voltage of 0.39 V, corresponding to a bandgap-voltage offset of 0.57 V, comparable with the state-of-the-art for this type of solar cells. Post-growth annealing

  7. Microstructural characterization of Ta-Si alloy as cast; Caracterizacao microestrutural de ligas Ta-Si no estado bruto de fusao

    Energy Technology Data Exchange (ETDEWEB)

    Silva, A.A.A.P. da; Coelho, G.C.; Nunes, C.A.; Suzuki, P.A.; Borges, S.P.T., E-mail: antonioaaps@gmail.co [Universidade de Sao Paulo (EEL/USP), Lorena, SP (Brazil). Escola de Engenharia; Faria, M.I.S.T. [Centro Universitario de Volta Redonda (UNIFOA), RJ (Brazil)

    2010-07-01

    Recent experimental studies developed in our group involving systems containing transition metals and silicon differed from the phase diagrams actually accepted. The objective of this study is to experimentally re-evaluate the invariant reactions involving liquid phase of the binary Ta-Si. Samples with different compositions were melted in arc furnace with non-consumable tungsten electrode in the copper crucible cooled water under argon atmosphere and titanium getter, using materials of high purity (minimum purity of 99.5% Ta and 99.999% Si). The samples were melted four times to ensure the microstructural and compositional homogeneity. The microstructures of the samples as cast were characterized by scanning electron microscopy (SEM/EDS) and X-ray diffraction (XRD). The results of this analysis led to a proposal for the phase diagram of Ta-Si slightly different than the diagram currently accepted. (author)

  8. Growth and characterization of III-N ternary thin films by plasma assisted atomic layer epitaxy at low temperatures

    Energy Technology Data Exchange (ETDEWEB)

    Nepal, Neeraj; Anderson, Virginia R.; Hite, Jennifer K.; Eddy, Charles R.

    2015-08-31

    We report the growth and characterization of III-nitride ternary thin films (Al{sub x}Ga{sub 1−x}N, In{sub x}Al{sub 1−x}N and In{sub x}Ga{sub 1−x}N) at ≤ 500 °C by plasma assisted atomic layer epitaxy (PA-ALE) over a wide stoichiometric range including the range where phase separation has been an issue for films grown by molecular beam epitaxy and metal organic chemical vapor deposition. The composition of these ternaries was intentionally varied through alterations in the cycle ratios of the III-nitride binary layers (AlN, GaN, and InN). By this digital alloy growth method, we are able to grow III-nitride ternaries by PA-ALE over nearly the entire stoichiometry range including in the spinodal decomposition region (x = 15–85%). These early efforts suggest great promise of PA-ALE at low temperatures for addressing miscibility gap challenges encountered with conventional growth methods and realizing high performance optoelectronic and electronic devices involving ternary/binary heterojunctions, which are not currently possible. - Highlights: • III-N ternaries grown at ≤ 500 °C by plasma assisted atomic layer epitaxy • Growth of InGaN and AlInN in the spinodal decomposition region (15–85%) • Epitaxial, smooth and uniform III-N film growth at low temperatures.

  9. Synthesis, Characterization, and Antimicrobial and Antispermatogenic Activity of Bismuth(III and Arsenic(III Derivatives of Biologically Potent Nitrogen and Sulfur Donor Ligands

    Directory of Open Access Journals (Sweden)

    Latika Dawara

    2012-01-01

    Full Text Available A series of Bi(III and As(III complexes with two N∩S donor ligands, 1-(4-chloro-2-oxo-2H-chromen-3-yl-methylene-thiosemicarbazide (L1H and N′-[1-(2-oxo-2H-chrome-3yl-ethylidene]-hydrazinecarbodithionic acid benzyl ester (L2H have been synthesized by the reaction of BiCl3 and Ph3As with ligands in 1 : 1 and 1 : 2 molar ratios. All the synthesized compounds were characterized by elemental analyses, melting point determinations, and a combination of electronic, IR, 1H NMR, 13C NMR spectroscopic techniques, and X-ray diffraction for structure elucidation. In order to evaluate the effect of metal ions upon chelation, both the ligands and their complexes have been screened for their antimicrobial activity against the various pathogenic bacterial and fungal strains. The metal complexes have shown to be more antimicrobial against the microbial species as compared to free ligands. Both the ligands and their corresponding metal complexes have been tested for their antifertility activity in male albino rats. The marked reduction in sperm motility and density resulted in infertility. Significant alterations were found in biochemical parameters of reproductive organs in treated animals as compared to control group. It is concluded that all these effects may finally impair the fertility of male rats.

  10. 3D Microstructural Characterization of Uranium Oxide as a Surrogate Nuclear Fuel: Effect of Oxygen Stoichiometry on Grain Boundary Distributions

    Energy Technology Data Exchange (ETDEWEB)

    Rudman, K. [Arizona State Univ., Tempe, AZ (United States); Dickerson, P. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Byler, Darrin David [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Peralta, P. [Arizona State Univ., Tempe, AZ (United States); Lim, H. [Arizona State Univ., Tempe, AZ (United States); McDonald, R. [Arizona State Univ., Tempe, AZ (United States); Dickerson, R. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Mcclellan, Kenneth James [Los Alamos National Lab. (LANL), Los Alamos, NM (United States)

    2017-09-06

    The initial microstructure of an oxide fuel can play a key role in its performance. At low burn-ups, the diffusion of fission products can depend strongly on grain size and grain boundary (GB) characteristics, which in turn depend on processing conditions and oxygen stoichiometry. Serial sectioning techniques using Focused Ion Beam were developed to obtain Electron Backscatter Diffraction (EBSD) data for depleted UO2 pellets that were processed to obtain 3 different oxygen stoichiometries. The EBSD data were used to create 3D microstructure reconstructions and to gather statistical information on the grain and GB crystallography, with emphasis on identifying the character (twist, tilt, mixed) for GBs that meet the Coincident Site Lattice (CSL) criterion as well as GBs with the most common misorientation angles. Data on dihedral angles at triple points were also collected. The results were compared across different samples to understand effects of oxygen content on microstructure evolution.

  11. Synthesis, structural characterization, luminescent properties and theoretical study of three novel lanthanide metal-organic frameworks of Ho(III), Gd(III) and Eu(III) with 2,5-thiophenedicarboxylate anion

    Science.gov (United States)

    Marques, Lippy F.; Correa, Charlane C.; Ribeiro, Sidney J. L.; dos Santos, Molíria V.; Dutra, José Diogo L.; Freire, Ricardo O.; Machado, Flávia C.

    2015-07-01

    In this paper, the synthesis of three new metal-organic frameworks of lanthanides (LnMOFs) {[Ln2(2,5-tdc)3(dmso)2]·H2O}n (Ln=Ho (1); Gd (2); Eu (3); 2,5-tdc=2,5-thiophenedicarboxylate anion; dmso=dimethylsulfoxide), and their complete characterization, including single crystal X-ray diffraction, FTIR spectroscopy and thermogravimetric analysis are reported. In especial, photophysical properties of Eu(III) complex have been studied in detail via both theoretical and experimental approaches. Crystal structure of (1) reveals that each lanthanide ion is seven-coordinated by oxygen atoms in an overall distorted capped trigonal - prismatic geometry. The 2,5-tdc2- ligands connect four Ln(III) centers, adopting (κ1-κ1)-(κ1-κ1)-μ4 coordination mode, generating an 8-connected uninodal 3D network. In addition, theoretical studies for Eu(III) complex were performed using the Sparkle model for lanthanide complexes.

  12. Synthesis, structural characterization, luminescent properties and theoretical study of three novel lanthanide metal-organic frameworks of Ho(III), Gd(III) and Eu(III) with 2,5-thiophenedicarboxylate anion

    Energy Technology Data Exchange (ETDEWEB)

    Marques, Lippy F. [Instituto de Química, Universidade do Estado do Rio de Janeiro, Rio de Janeiro 20550-013 (Brazil); Correa, Charlane C. [Departamento de Química-ICE, Universidade Federal de Juiz de Fora, Juiz de Fora-MG, 36036-330 (Brazil); Ribeiro, Sidney J.L.; Santos, Molíria V. dos [Institute of Chemistry, São Paulo State University − UNESP, CP 355 Araraquara-SP 14801-970 Brazil (Brazil); Dutra, José Diogo L.; Freire, Ricardo O. [Pople Computational Chemistry Laboratory, Departamento de Química, Universidade Federal de Sergipe, São Cristóvão-SE 49100-000 (Brazil); Machado, Flávia C., E-mail: flavia.machado@ufjf.edu.br [Departamento de Química-ICE, Universidade Federal de Juiz de Fora, Juiz de Fora-MG, 36036-330 (Brazil)

    2015-07-15

    In this paper, the synthesis of three new metal-organic frameworks of lanthanides (LnMOFs) ([Ln{sub 2}(2,5-tdc){sub 3}(dmso){sub 2}]·H{sub 2}O){sub n} (Ln=Ho (1); Gd (2); Eu (3); 2,5-tdc=2,5-thiophenedicarboxylate anion; dmso=dimethylsulfoxide), and their complete characterization, including single crystal X-ray diffraction, FTIR spectroscopy and thermogravimetric analysis are reported. In especial, photophysical properties of Eu(III) complex have been studied in detail via both theoretical and experimental approaches. Crystal structure of (1) reveals that each lanthanide ion is seven-coordinated by oxygen atoms in an overall distorted capped trigonal – prismatic geometry. The 2,5-tdc{sup 2−} ligands connect four Ln(III) centers, adopting (κ{sup 1}–κ{sup 1})–(κ{sup 1}–κ{sup 1})–μ{sub 4} coordination mode, generating an 8-connected uninodal 3D network. In addition, theoretical studies for Eu(III) complex were performed using the Sparkle model for lanthanide complexes. - Graphical abstract: Three new metal-organic frameworks of lanthanides (LnMOFs) ([Ln{sub 2}(2,5-tdc){sub 3}(dmso){sub 2}]·H{sub 2}O){sub n} (Ln=Ho (1); Gd (2); Eu (3); 2,5-tdc=2,5-thiophenedicarboxylate anion; dmso=dimethylsulfoxide), were synthesized and their complete characterization, including single crystal X-ray diffraction, FTIR spectroscopy and thermogravimetric analysis are reported. In especial, photophysical properties of Eu(III) complex have been studied in detail via both theoretical and experimental approaches. - Highlights: • Three new LnMOFs were synthesized and fully characterized. • Ho{sup 3+}, Gd{sup 3+} and Eu{sup 3+} complexes photoluminescence properties were investigated. • Theoretical approaches for Eu{sup 3+} complex luminescence has been performed. • An energy level diagram is used to establish the ligand-to-metal energy transfer. • These metal−organic frameworks can act as light conversion molecular devices.

  13. Classification based on mutations of TERT promoter and IDH characterizes subtypes in grade II/III gliomas.

    Science.gov (United States)

    Yang, Pei; Cai, Jinquan; Yan, Wei; Zhang, Wei; Wang, Yinyan; Chen, Baoshi; Li, Guilin; Li, Shouwei; Wu, Chenxing; Yao, Kun; Li, Wenbin; Peng, Xiaoxia; You, Yongping; Chen, Ling; Jiang, Chuanlu; Qiu, Xiaoguang; Jiang, Tao

    2016-08-01

    Grade II and III gliomas have variable clinical behaviors, showing the distinct molecular genetic alterations from glioblastoma (GBM), many of which eventually transform into more aggressive tumors. Since the classifications of grade II/III gliomas based on the genetic alterations have been recently emerging, it is now a trend to include molecular data into the standard diagnostic algorithm of glioma. Here we sequenced TERT promoter mutational status (TERTp-mut) in the DNA of 377 grade II/III gliomas and analyzed the clinical factors, molecular aberrations, and transcriptome profiles. We found that TERTp-mut occurred in 145 of 377 grade II and III gliomas (38.5%), mutually exclusive with a TP53 mutation (TP53-mut; P IDH mutation (IDH-mut) subgroup (P = .018), but it has also been associated with a poor outcome in the IDH wild-type (IDH-wt) subgroup (P = .049). Combining TERTp-mut and IDH-mut allowed the grade II/III malignancies to be reclassified into IDH-mut/TERTp-mut, IDH-mut only, TERTp-mut only, and IDH-wt/TERTp-wt. 1p/19q co-deletion, TP53-muts, Ki-67 expression differences, and p-MET expression differences characterized IDH-mut/TERTp-mut, IDH-mut only, TERTp-mut only, and IDH-wt/TERTp-wt subtypes, respectively. Our results showed that TERTp-mut combined with IDH-mut allowed simple classification of grade II/III gliomas for stratifying patients and clarifying diagnostic accuracy by supplementing standard histopathological criteria. © The Author(s) 2016. Published by Oxford University Press on behalf of the Society for Neuro-Oncology. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com.

  14. Microstructural and mechanical characterization of Nb-based in situ composites from Nb-Si-Ti ternary system

    Energy Technology Data Exchange (ETDEWEB)

    Li, Z. [Department of Mechanics and Mechanical Engineering, CAS Key Laboratory for Mechanical Behavior and Design of Materials, School of Engineering Science, University of Science and Technology of China, Hefei 230026, Anhui (China); Peng, L.M. [Department of Mechanics and Mechanical Engineering, CAS Key Laboratory for Mechanical Behavior and Design of Materials, School of Engineering Science, University of Science and Technology of China, Hefei 230026, Anhui (China)], E-mail: penglm@ustc.edu.cn

    2007-11-15

    This study deals with the Nb-niobium silicide-based composites developed by the hot-pressing of Nb-Si-Ti ternary powder mixtures with a fixed Ti addition (6 at.%) and Si content ranging from hypereutectic (11 at.%) to near-eutectic compositions (18 at.%). The effects of Si content, Ti addition and strain rates on the sample microstructural characterization, flexural strength, fracture toughness, quasi-static compressive deformation and failure processes were investigated. It was revealed that the volume fraction of silicides increased with increasing Si content, and most of the Ti atoms dissolved into the niobium silicides to form (Nb,Ti){sub 5}Si{sub 3} solid solutions instead of binary titanium silicides. The experimental evidence showed that a moderate improvement in the flexural strength, fracture toughness and compressive yield stress of the composites was achieved by the addition of Ti. Higher Si additions produced a much more remarkable enhancement in the compressive yield stress and bulk hardness, whereas both the flexural strength and fracture toughness decreased with increasing Si content owing to the existence of residual porosities in the samples. The composites showed remarkable superiority to the arc-melted Nb-Si alloys and monolithic niobium silicides in fracture toughness (8.3-13.0MPa{radical}(m) vs. 4.5MPa{radical}(m)), where the toughening effect was attributed mainly to crack bridging and crack deflection by the remaining ductile Nb phase. Moreover, quasi-static uniaxial compression tests at strain rates between 10{sup -5} and 10{sup -3} s{sup -1} indicated that the deformation behavior and failure processes were significantly affected by Si content and strain rates. The strain-rate-hardening behavior for all the strain rates was observed in the composite materials and the strain-rate sensitivity decreased with increasing Si content. At a lower strain rate, the composite materials with a hypoeutectic Si composition failed with a pseudoplastic

  15. Synthesize and microstructure characterization of Ni{sub 43}Mn{sub 41}Co{sub 5}Sn{sub 11} Heusler alloy

    Energy Technology Data Exchange (ETDEWEB)

    Elwindari, Nastiti; Manaf, Azwar, E-mail: azwar@ui.ac.id [Physics Department, Faculty of Science, Universitas Indonesia, Depok 16424 (Indonesia)

    2016-06-17

    The ferromagnetic heusler alloys are promising materials in many technical applications due to their multifunctional properties such as shape memory effect, magnetocaloric effect, giant magnetoresistance, etc. In this work, synthesize and characterization of polycrystalline Ni{sub 43}Mn{sub 41}Co{sub 5}Sn{sub 11} (NMCS) alloy are reported. Alloy preparation was conducted by melting the constitute elements under an innert Argon (Ar) atmosphere in a vacuum mini arc-melting furnace. Homogenization of the microstructure of the as-cast ingot was obtained after annealing process at 750°C for 48 hours. It is shown that the dendrites structure has changed to equaixed grains morphology after homogenization. Microstructure characteristics of material by x-ray diffraction revealed that the alloy has a L{sub 21}-type cubic crystal structure as the main phase at room temperature. In order to induce the shape anisotropy, a forging treatment was applied to show the shape orientation of material. Various enhancements of magnetic properties in a longitudinal direction were observed at various degree of anisotropy. The microstructure changes of as-cast NMCS and effects of homogenization treatments as studied by scanning electron microscopy (SEM) and energy dispersive spectrometry (EDS) are discussed in details.

  16. Characterization the microstructure of pulsed Nd:YAG welding method in low frequencies; correlation with tensile and fracture behavior in laser-welded nitinol joints

    Science.gov (United States)

    Shojaei Zoeram, Ali; Rahmani, Aida; Asghar Akbari Mousavi, Seyed Ali

    2017-05-01

    The precise controllability of heat input in pulsed Nd:YAG welding method provided by two additional parameters, frequency and pulse duration, has made this method very promising for welding of alloys sensitive to heat input. The poor weldability of Ti-rich nitinol as a result of the formation of Ti2Ni IMC has deprived us of the unique properties of this alloy. In this study, to intensify solidification rate during welding of Ti-rich nitinol, pulsed Nd:YAG laser beam in low frequency was employed in addition to the employment of a copper substrate. Specific microstructure produced in this condition was characterized and the effects of this microstructure on tensile and fracture behavior of samples welded by two different procedures, full penetration and double-sided method with halved penetration depth for each side were investigated. The investigations revealed although the combination of low frequencies, the use of a high thermal conductor substrate and double-sided method eliminated intergranular fracture and increased tensile strength, the particular microstructure, built in the pulsed welding method in low frequencies, results to the formation of the longitudinal cracks during the first stages of tensile test at weld centerline. This degrades tensile strength of welded samples compared to base metal. The results showed samples welded in double-sided method performed much better than samples welded in full penetration mode.

  17. The Optimization of Process Parameters and Microstructural Characterization of Fiber Laser Welded Dissimilar HSLA and MART Steel Joints

    Directory of Open Access Journals (Sweden)

    Celalettin Yuce

    2016-10-01

    Full Text Available Nowadays, environmental impact, safety and fuel efficiency are fundamental issues for the automotive industry. These objectives are met by using a combination of different types of steels in the auto bodies. Therefore, it is important to have an understanding of how dissimilar materials behave when they are welded. This paper presents the process parameters’ optimization procedure of fiber laser welded dissimilar high strength low alloy (HSLA and martensitic steel (MART steel using a Taguchi approach. The influence of laser power, welding speed and focal position on the mechanical and microstructural properties of the joints was determined. The optimum parameters for the maximum tensile load-minimum heat input were predicted, and the individual significance of parameters on the response was evaluated by ANOVA results. The optimum levels of the process parameters were defined. Furthermore, microstructural examination and microhardness measurements of the selected welds were conducted. The samples of the dissimilar joints showed a remarkable microstructural change from nearly fully martensitic in the weld bead to the unchanged microstructure in the base metals. The heat affected zone (HAZ region of joints was divided into five subzones. The fusion zone resulted in an important hardness increase, but the formation of a soft zone in the HAZ region.

  18. Micro-structured electrode arrays : high-frequency discharges at atmospheric pressure—characterization and new applications

    NARCIS (Netherlands)

    Baars-Hibbe, Lutz; Schrader, Christian; Sichler, Philipp; Cordes, Thorben; Gericke, Karl-Heinz; Büttgenbach, Stephanus; Draeger, Siegfried

    2004-01-01

    Micro-structured electrode (MSE) arrays allow to generate large-area uniform glow discharges over a wide pressure range up to atmospheric pressure. The electrode dimensions in the µm-range realized by means of modern micro-machining and galvanic techniques are small enough to generate sufficiently

  19. Microstructural Characterization of Reinforced Mortar after Corrosion and Cathodic Prevention in the Presence of Core-Shell Micelles

    NARCIS (Netherlands)

    Koleva, D.A.

    2010-01-01

    This work reports on the microstructural properties of reinforced mortar after chloride-induced corrosion and two regimes of cathodic prevention. Additionally, the impact of a very low concentration polymeric nano-aggregates (core-shell micelles from PEO113-b-PS218), admixed in the mortar mixture is

  20. Fabrication and characterization of polycarbonate microstructured polymer optical fibers for high-temperature-resistant fiber Bragg grating strain sensors

    DEFF Research Database (Denmark)

    Fasano, Andrea; Woyessa, Getinet; Stajanca, Pavol

    2016-01-01

    Here we present the fabrication of a solid-core microstructured polymer optical fiber (mPOF) made of polycarbonate (PC), and report the first experimental demonstration of a fiber Bragg grating (FBG) written in a PC optical fiber. The PC used in this work has a glass transition temperature of 145°C...

  1. Characterization of Microstructure and Texture of 13Cr4Ni Martensitic Stainless Steel Weld Before and After Tempering =

    Science.gov (United States)

    Mokhtabad Amrei, Mohsen

    13Cr4Ni martensitic stainless steels are known for their outstanding performances in the hydroelectric industry, where they are mainly used in the construction of turbine components. Considering the size and geometry of turbine runners and blades, multi-pass welding procedures are commonly used in the fabrication and repair of such turbines. The final microstructure and mechanical properties of the weld are sensitive to the welding process parameters and thermal history. In the case of 13Cr4Ni steel, the thermal cycles imposed by the multi-pass welding operation have significant effects on the complex weld microstructure. Additionally, post-weld heat treatments are commonly used to reduce weld heterogeneity and improve the material's mechanical properties by tempering the microstructure and by forming a "room-temperature-stable austenite." In the first phase of this research, the microstructures and crystallographic textures of aswelded single-pass and double-pass welds were studied as a basis to studying the more complex multi-pass weld microstructure. This study found that the maximum hardness is obtained in high temperature heat affected zone inside the base metal. In particular, the results showed that the heat cycle exposed by the second pass increases the hardness of the previous pass because it produces a finer martensite microstructure. In areas of heat affected zone, a tempering effect is reported from 3 up to 6 millimeters far from the fusion line. Finding austenite phase in these areas are matter of interest and it can be indicative of the microstructure complexity of multi-pass welds. In the second phase of research, the microstructure of multi-pass welds was found to be more heterogeneous than that of single- and double-pass welds. Any individual pass in a multi-pass weld consists of several regions formed by adjacent weld passes heat cycle. Results showed that former austenite grains modification occurred in areas close to the subsequent weld passes

  2. Immobilization of Ionophore and Surface Characterization Studies of the Titanium(III Ion in a PVC-Membrane Sensor

    Directory of Open Access Journals (Sweden)

    Majid Rezayi

    2012-06-01

    Full Text Available Novel ionophores comprising various hydroxide and amine structures were immobilized onto poly(vinyl chloride (PVC matrices, and these were examined to determine Ti(III selectivity. To predict the selectivity of Ti(III, a PVC membrane was used to investigate the binding of Ti(III to c-methylcalix[4]resorcinarene (CMCR. The study showed that the chelating ligand, CMCR, was coordinated selectively to Ti(III at eight coordination sites involving the oxygen atoms at the interface of the membrane/solution. The membrane was prepared, based on CMCR as an ionophore, sodium tetrakis(4-fluorophenyl borate (NaTFPB as a lipophilic ionic additive, and dioctylphthalate (DOP as a plasticizer. The immobilization of the ionophore and surface characterization studies revealed that the performance of CMCR-immobilized PVC was equivalent to that of mobile ionophores in supported liquid membranes (SLMs. The strengths of the ion-ionophore (CMCR-Ti(OH(OH252+ interactions and the role of ionophores on membranes were studied via UV-Vis, Fourier transform infrared spectroscopy (FT–IR, scanning electron microscopy (SEM and and X-ray diffraction (XRD.

  3. Microstructural characterization of IF steel after severe plastic deformation via ARB and subsequent heat treatment; Caracterizacao microestrutural de um aco IF apos deformacao plastica severa via ARB e posterior recozimento

    Energy Technology Data Exchange (ETDEWEB)

    Oliveira, F.C.; Abrantes, A.L.A.; Lins, J.F.C., E-mail: cristinafo2@hotmail.co [Universidade Federal Fluminense (PPGEM/UFF), Volta Redonda, RJ (Brazil). Programa de Pos-graduacao em Engenharia Metalurgica

    2010-07-01

    This study aimed to evaluate the microstructural evolution of a titanium stabilized IF steel deformed to warm through the ARB process for 5 consecutive cycles and then annealing at 600 deg C for 1 h. The material was characterized with the aid of the techniques of scanning electron microscopy and electron backscatter diffraction (Electron Backscatter Diffraction - EBSD). An intense process of microstructural refinement was observed in the deformed material and the phenomenon of dynamic recovery was predominant. It can be concluded that the annealing of severely deformed material was not sufficient for a complete recrystallization of the microstructure. (author)

  4. Microstructural and mechanical development and characterization of glass ionomer cements; Desenvolvimento e caracterizacao microestrutural e mecanica de cimentos de ionomero de vidro

    Energy Technology Data Exchange (ETDEWEB)

    Freire, W.P.; Barbosa, R.C.; Castanha, E.M.M.; Barbosa, E. F.; Fook, M.V.L., E-mail: waldeniafreire@hotmail.com [Universidade Federal de Campina Grande (UFCG), PB (Brazil). Departamento de Ciencias e Engenharia de Materiais

    2013-07-01

    Glass Ionomer Cements (GICs) are widely used in dentistry, indicated as a restorative material, cement for orthopedic and dental prostheses. However, there is need for development of new bone cements as alternative or replacement to current polymethylmethacrylate cements. Thus the aim of this research was develop of an experimental GIC and the mechanical and microstructural characterization of this composite; as a control group it was used a commercial GIC called Vidrion R (SS WHITE). These composites were characterized by X-ray diffraction, Infrared Spectroscopy Fourier Transform and Scanning Electron Microscopy. The mechanical properties of the composites were measured by Vickers microhardness testing, flexural strength and compression. These cements were characterized as a semicrystalline; in FTIR spectra observed characteristic bands of these materials and microstructural studies of experimental GIC revealed that there was no proper interaction of the inorganic particles in the polymer matrix, whereas in the control group this interaction was effective resulting in greater homogeneity among its constituent phases. Experimental cement showed a higher value of microhardness in the control group, however, flexural strength of cement experimental cement was lower than the control group, and this behavior can possibly be attributed to inadequate interaction particle / matrix. In tests of compressive strength, experimental GIC showed resistance similar to that shown for control group after variation in the processing conditions of the material. (author)

  5. Synthesis, characterization, luminescent properties and theoretical study of two new coordination polymers containing lanthanide [Ce(III) or Yb(III)] and succinate ions

    Science.gov (United States)

    de Oliveira, Carlos Alberto F.; da Silva, Fausthon Fred; Malvestiti, Ivani; Malta, Valéria Rodrigues dos S.; Dutra, José Diogo L.; da Costa, Nivan B.; Freire, Ricardo O.; Alves, Severino

    2013-06-01

    Two new three-dimensional coordination polymers [Ce2(C4H4O4)3(H2O)2]nṡH2O 1 and [Yb2(C4H4O4)3(H2O)2]nṡH2O 2 have been synthesized under hydrothermal conditions and characterized by single-crystal X-ray, elemental, infrared and thermogravimetric analysis. Both compounds crystallized in the monoclinic system and space group C2/c with cell parameters a = 20.1178(2), b = 7.98150(10), c = 14.03090(10), β = 120.9050(10), cell volume = 1933.07(3) Å3 for 1, and a = 19.7360(3), b = 7.59790(10), c = 13.7564(2), β = 121.3060(10), cell volume = 1762.47(4) for 2. The solid-state structures of the two metal-organic frameworks (MOFs) were subjected to detailed analysis using the semiempirical Sparkle/AM1, Sparkle/PM3 and Sparkle/PM6 quantum models. The theoretical results obtained were in good overall agreement with the experimental data, although the Sparkle/PM3 model presented the highest accuracy. The luminescent spectra of 1 and 2 showed emission bands characteristic of the Ce (III) and Yb (III) at 444 nm and 970 nm, respectively. Thermal analysis revealed that both MOFs lost one molecule of water of hydration and two molecules of coordinated water upon heating. In compound 1, the removal of water occurred in two steps while in 2, water loss occurred in a single step.

  6. Synthesis, characterization and anti-tumour activity of iron(III Schiff base complexes with unsymmetric tetradentate ligands

    Directory of Open Access Journals (Sweden)

    Fahmideh Shabani

    2010-08-01

    Full Text Available The synthesis and characterization of two new iron(III complexes, [Fe(pythsalI]Cl2 and [Fe(pythsalBr]Cl2 with the NSNO-donor tetradentate Schiff base ligands pythsalHX [(5–X-N-(2pyridylethylsulfanylethyl salicylideneimine] (X = I, Br obtained from the inserted condensation of 1-(2-pyridyl-3-thia-5-aminopentane with the respective derivative salicylaldehyde in a 1:1 molar ratio is reported. The iron(III complexes were characterized by several techniques using elemental analysis (C, H, N, FT-IR, electronic spectra and molar conductance measurements. The elemental analysis data suggest the stoichiometry to be 1:2 [M:L] ratio formation. The molar conductance measurements reveal the presence of 1:2 electrolytic nature complexes. Infrared spectral data agreed with the coordination to the central metal ion through deprotonated phenolic oxygen, imine and pyridine type nitrogens and the thioether sulfur atoms. From ligand field spectral data an octahedral geometry is assigned to the iron(III ion in all these complexes. These new compounds have showed anti-tumour activity against two kinds of cancer cells that are K562 (human chronic myeloid leukemia and Jurkat (human T lymphocyte carcinoma.

  7. Identification and Spectroscopic Characterization of Nonheme Iron(III) Hypochlorite Intermediates

    NARCIS (Netherlands)

    Draksharapu, Apparao; Angelone, Davide; Quesne, Matthew G.; Padamati, Sandeep K.; Gomez, Laura; Hage, Ronald; Costas, Miquel; Browne, Wesley R.; de Visser, Sam P.

    2015-01-01

    Fe-III-hypohalite complexes have been implicated in a wide range of important enzyme-catalyzed halogenation reactions including the biosynthesis of natural products and antibiotics and post-translational modification of proteins. The absence of spectroscopic data on such species precludes their

  8. Structural characterization of Am(III) formate complexes. Combining EXAFS spectroscopy with DFT and thermodynamical calculations

    Energy Technology Data Exchange (ETDEWEB)

    Rossberg, Andre [Helmholtz-Zentrum Dresden-Rossendorf e.V., Dresden (Germany). Molecular Structures; Froehlich, D.R. [Heidelberg Univ. (Germany). Physikalisch-Chemisches Inst.

    2017-06-01

    We used iterative transformation factor analysis (ITFA) in order to isolate the EXAFS spectral contributions of the complexing ligand from a Am(III)/formate pH-series. Thermodynamic calculations were used as constraint for ITFA and for density functional theory (DFT) calculations to identify the coordination mode within the formed complexes.

  9. Structural characterization of CFA/III and Longus type IVb pili from enterotoxigenic Escherichia coli.

    Science.gov (United States)

    Kolappan, Subramaniapillai; Roos, Justin; Yuen, Alex S W; Pierce, Owen M; Craig, Lisa

    2012-05-01

    The type IV pili are helical filaments found on many Gram-negative pathogenic bacteria, with multiple diverse roles in pathogenesis, including microcolony formation, adhesion, and twitching motility. Many pathogenic enterotoxigenic Escherichia coli (ETEC) isolates express one of two type IV pili belonging to the type IVb subclass: CFA/III or Longus. Here we show a direct correlation between CFA/III expression and ETEC aggregation, suggesting that these pili, like the Vibrio cholerae toxin-coregulated pili (TCP), mediate microcolony formation. We report a 1.26-Å resolution crystal structure of CofA, the major pilin subunit from CFA/III. CofA is very similar in structure to V. cholerae TcpA but possesses a 10-amino-acid insertion that replaces part of the α2-helix with an irregular loop containing a 3(10)-helix. Homology modeling suggests a very similar structure for the Longus LngA pilin. A model for the CFA/III pilus filament was generated using the TCP electron microscopy reconstruction as a template. The unique 3(10)-helix insert fits perfectly within the gap between CofA globular domains. This insert, together with differences in surface-exposed residues, produces a filament that is smoother and more negatively charged than TCP. To explore the specificity of the type IV pilus assembly apparatus, CofA was expressed heterologously in V. cholerae by replacing the tcpA gene with that of cofA within the tcp operon. Although CofA was synthesized and processed by V. cholerae, no CFA/III filaments were detected, suggesting that the components of the type IVb pilus assembly system are highly specific to their pilin substrates.

  10. Electrochemical and Spectroscopic Characterization of Aluminium(III-para-methyl-meso-tetraphenylporphyrin Complexes Containing Substituted Salicylates as Axial Ligands

    Directory of Open Access Journals (Sweden)

    Gauri D. Bajju

    2013-01-01

    Full Text Available A series of aluminium(III-p-methyl-meso-tetraphenylporphyrin (p-CH3TPP-Al(III containing axially coordinated salicylate anion [p-CH3TPP-Al-X], where X = salicylate (SA, 4-chlorosalicylate (4-CSA, 5-chlorosalicylate (5-CSA, 5-flourosalicylate (5-FSA, 4-aminosalicylate (4-ASA, 5-aminosalicylate (5-ASA, 5-nitrosalicylate (5-NSA, and 5-sulfosalicylate (5-SSA, have been synthesized and characterized by various spectroscopic techniques including ultraviolet-visible (UV-vis, infrared (IR spectroscopy, proton nuclear magnetic resonance (1H NMR spectroscopy, 13C NMR, and elemental analysis. A detailed study of electrochemistry of all the synthesized compounds has been done to compare their oxidation and reduction mechanisms and to explain the effect of axial coordination on their redox properties.

  11. Synthesis and characterization of bismuth(III) and antimony(V) porphyrins: high antileishmanial activity against antimony-resistant parasite.

    Science.gov (United States)

    Gomes, Marcela Luísa; DeFreitas-Silva, Gilson; dos Reis, Priscila Gomes; Melo, Maria Norma; Frézard, Frédéric; Demicheli, Cynthia; Idemori, Ynara Marina

    2015-07-01

    Two bismuth(III) porphyrins-5,10,15,20-tetrakis(phenyl)porphyrinatobismuth(III) nitrate, [Bi(III)(TPP)]NO3, and the unprecedent 5,10,15,20-tetrakis(4-carbomethoxyphenyl)porphyrinatobismuth(III) nitrate, [Bi(III)(T4CMPP)]NO3, and two unprecedented antimony(V) porphyrins dichlorido(5,10,15,20-tetrakis(phenyl)porphyrinato)antimony(V) bromide, [Sb(V)(TPP)Cl2]Br, and dibromido(5,10,15,20-tetrakis(4-carbomethoxyphenyl)porphyrinato)antimony(V) bromide, [Sb(V)(T4CMPP)Br2]Br,-were synthesized by reacting the corresponding porphyrin ligand with Bi(NO3)3·5H2O or SbCl3. All compounds were characterized by UV-vis, (1)H NMR spectroscopy, and mass spectrometry. The new compounds were also characterized by elemental analysis. Because antimony and bismuth compounds have been widely applied in medicine, the activity of these complexes was tested against Sb-sensitive and -resistant Leishmania amazonensis parasites. [Sb(V)(T4CMPP)Br2]Br was more active against the promastigote form of Sb-resistant mutant strain as compared to the sensitive parental strain, with IC50 in the micromolar range. These data contrasted with those obtained using the Sb(III) drug potassium antimony tartrate, which displayed IC50 of 110 μmol L(-1) against the Sb-sensitive parasite and was almost inactive against the Sb-resistant strain. The H2T4CMPP ligand also showed antileishmanial activity against Sb-resistant and -sensitive strains, but with IC50 at least tenfold greater than that of the complex. The Sb(V)-porphyrin complex was also active against intracellular amastigotes and showed a higher selectivity index than the conventional Sb(V) drug glucantime, in both Sb-sensitive and -resistant strains. The greater antileishmanial activity of this complex could be attributed to an increased cellular uptake of Sb. Thus, [Sb(V)(T4CMPP)Br2]Br constitutes a new antileishmanial drug candidate.

  12. Gas tungsten arc welding and friction stir welding of ultrafine grained AISI 304L stainless steel: Microstructural and mechanical behavior characterization

    Energy Technology Data Exchange (ETDEWEB)

    Sabooni, S., E-mail: s.sabooni@ma.iut.ac.ir [Department of Materials Engineering, Isfahan University of Technology, 84156-83111 Isfahan (Iran, Islamic Republic of); Karimzadeh, F.; Enayati, M.H. [Department of Materials Engineering, Isfahan University of Technology, 84156-83111 Isfahan (Iran, Islamic Republic of); Ngan, A.H.W. [Department of Mechanical Engineering, The University of Hong Kong, Pokfulam Road, Hong Kong (China); Jabbari, H. [Department of Materials Engineering, Isfahan University of Technology, 84156-83111 Isfahan (Iran, Islamic Republic of)

    2015-11-15

    In the present study, an ultrafine grained (UFG) AISI 304L stainless steel with the average grain size of 650 nm was successfully welded by both gas tungsten arc welding (GTAW) and friction stir welding (FSW). GTAW was applied without any filler metal. FSW was also performed at a constant rotational speed of 630 rpm and different welding speeds from 20 to 80 mm/min. Microstructural characterization was carried out by High Resolution Scanning Electron Microscopy (HRSEM) with Electron Backscattered Diffraction (EBSD) and Transmission Electron Microscopy (TEM). Nanoindentation, microhardness measurements and tensile tests were also performed to study the mechanical properties of the base metal and weldments. The results showed that the solidification mode in the GTAW welded sample is FA (ferrite–austenite) type with the microstructure consisting of an austenite matrix embedded with lath type and skeletal type ferrite. The nugget zone microstructure in the FSW welded samples consisted of equiaxed dynamically recrystallized austenite grains with some amount of elongated delta ferrite. Sigma phase precipitates were formed in the region ahead the rotating tool during the heating cycle of FSW, which were finally fragmented into nanometric particles and distributed in the weld nugget. Also there is a high possibility that the existing delta ferrite in the microstructure rapidly transforms into sigma phase particles during the short thermal cycle of FSW. These suggest that high strain and deformation during FSW can promote sigma phase formation. The final austenite grain size in the nugget zone was found to decrease with increasing Zener–Hollomon parameter, which was obtained quantitatively by measuring the peak temperature, calculating the strain rate during FSW and exact examination of hot deformation activation energy by considering the actual grain size before the occurrence of dynamic recrystallization. Mechanical properties observations showed that the welding

  13. Real-time in situ characterization of interface dynamics in microstructure formation during 3D-directional solidification of transparent alloys

    Science.gov (United States)

    Bergeon, N.; Trivedi, R.; Billia, B.; Echebarria, B.; Karma, A.; Liu, S.; Weiss, C.

    The properties of structural materials are to a large extent determined by the solid microstructure so that the understanding of the fundamental physics of microstructure formation is critical in the engineering of materials. Also, microstructure selection occurs during the dynamical growth process so that in situ observation of spatio-temporal evolution of the solid-liquid interface shape is necessary. Under terrestrial conditions, convection effects dominates in bulk samples which prevent precise characterization of microstructure selection. As the glass ampoule conducts heat better than transparent materials, e.g. succinonitrile, the sample near the wall is cooler and convection arises. This leads to concave interface and non-uniform morphological instability starting at the center, while the region near the wall remains smooth. Diffusion-controlled experiments in thin samples give microstructures that are neither 2D nor 3D. When the spacing between glass plates is smaller than the spacing, the cell shape near the tip is 3D, and becomes 2D away from the tip. Preliminary rigorous phase-field results show that in 3D tube geometry (reasonable approximation for a hexagonal array), axisymmetric cells only exist over a narrow range of spacing whereas in 2D steady-state shapes span a wide range of spacing. A benchmark experimental study in bulk samples is thus required under low gravity conditions. In the frame of the joint work of DSIP and MISOL3D projects, respectively selected by NASA and CNES, microgravity experiments in a model transparent system are planned on ISS using the Directional Solidification Insert in the DECLIC facility. The critical aspects of hardware design, the key fundamental issues identified through 1g-experiments, the proposed study on ISS, and the results of rigorous theoretical modeling will be presented. The cellular/dendritic interface morphologies will be examined by systematically varying the process parameters, yielding insight into the

  14. Additive Manufacturing of AlSi10Mg Alloy Using Direct Energy Deposition: Microstructure and Hardness Characterization

    Science.gov (United States)

    Javidani, M.; Arreguin-Zavala, J.; Danovitch, J.; Tian, Y.; Brochu, M.

    2017-04-01

    This paper aims to study the manufacturing of the AlSi10Mg alloy with direct energy deposition (DED) process. Following fabrication, the macro- and microstructural evolution of the as-processed specimens was initially investigated using optical microscopy and scanning electron microscopy. Columnar dendritic structure was the dominant solidification feature of the deposit; nevertheless, detailed microstructural analysis revealed cellular morphology near the substrate and equiaxed dendrites at the top end of the deposit. Moreover, the microstructural morphology in the melt pool boundary of the deposit differed from the one in the core of the layers. The remaining porosity of the deposit was evaluated by Archimedes' principle and by image analysis of the polished surface. Crystallographic texture in the deposit was also assessed using electron backscatter diffraction and x-ray diffraction analysis. The dendrites were unidirectionally oriented at an angle of 80° to the substrate. EPMA line scans were performed to evaluate the compositional variation and elemental segregation in different locations. Eventually, microhardness (HV) tests were conducted in order to study the hardness gradient in the as-DED-processed specimen along the deposition direction. The presented results, which exhibited a deposit with an almost defect free structure, indicate that the DED process can suitable for the deposition of Al-Si-based alloys with a highly consolidated structure.

  15. Identification, Characterization, and Developmental Expression Pattern of Type III Interferon Receptor Gene in the Chinese Goose

    Directory of Open Access Journals (Sweden)

    Qin Zhou

    2015-01-01

    Full Text Available Interferons, as the first line of defense against the viral infection, play an important role in innate immune responses. Type III interferon (IFN-λ was a newly identified member of IFN family, which plays IFN-like antiviral activity. Towards a better understanding of the type III interferon system in birds, type III interferon lambda receptor (IFNLR1 was first identified in the Chinese goose. In this paper, we had cloned 1952 bp for goose IFNLR1 (goIFNLR1, including an ORF of 1539 bp, encoding a 512-amino acid protein with a 20 aa predict signal peptide at its N terminal and a 23 aa transmembrane region. The predicted amino acid sequence of goIFNLR1 has 90%, 73%, and 34% identity with duck IFNLR1 (predicted sequence, chicken IFNLR1, and human IFNLR1, respectively. And the age-related tissue distribution of goIFNLR1 was identified by Real Time quantitative PCR (RT-qPCR, we found that the goIFNLR1 has a mainly expression in epithelium-rich tissues similar to other species’, such as small intestinal, lung, liver, and stomach. Moreover, a relatively high expression of goIFNLR1 was also observed in the secondary immune tissues (harderian gland and cecal tonsil. The identification and tissue distribution of goIFNLR1 will facilitate further study of the role of IFN-λ in goose antiviral defense.

  16. Novel Low Spin Mixed Ligand Thiohydrazide Complexes of Iron(III: Synthesis, Spectral Characterization, Molecular Modeling, and Antibacterial Activity

    Directory of Open Access Journals (Sweden)

    Dolan Sengupta

    2014-01-01

    Full Text Available Mixed ligand complexes of Fe(III with aromatic thiohydrazides of general composition [Fe(acac(L2] have been synthesized and characterized (acac-acetylacetonate, L = bidentate uninegative aromatic thiohydrazide ligand, for example, thiobenzhydrazide, 2-hydroxythiobenzhydrazide, furan-2-thiohydrazide, and thiophen-2-thiohydrazide. The magnetic susceptibility data and the EPR spectra of these complexes suggested the formation of rhombically distorted low spin iron center (d5 in octahedral environment, which was also supported by the UV-vis spectral data of the complexes. Biological studies of these complexes also indicated that the iron-thiohydrazido complexes have superior antibacterial properties compared to the corresponding ligands.

  17. The preparation and characterization of uns-cis-(ethylene-diamine-N,N'-di-3-propionato(N-alkylethylenediaminescobalt(III complexes

    Directory of Open Access Journals (Sweden)

    SANJA R. GRGURIC

    2000-03-01

    Full Text Available Three octahedral cobalt(III complexes of the general formula uns-cis-SCo(eddp(R-enCClÿ2H2O, where eddp = the tetradentate ONNO-type ligand ethylenediamine-N,N'-di-3-propionate and R-en = a bidentate NN-type ligand, either N-methyl, N-ethyl or N-isopropylethylenediamine. The complexes were prepared by the reaction of sodium uns-cis-(ethylenediamine-N,N'-di-3-propionato(carbonatocobaltate(IIIdihydrate with the corresponding diamine. They were isolated chromatographically and characterized by elemental analysis, infrared and electronic absorption spectroscopy.

  18. Microstructural characterization of archaeological samples coming from La Venta park, Tabasco, Mexico; Caracterizacion microestructural de muestras arqueologicas procedentes del parque La Venta Tabasco, Mexico

    Energy Technology Data Exchange (ETDEWEB)

    Espinosa P, M.F.; Rodriguez L, V.; Martinez, G. [Instituto Nacional de Investigaciones Nucleares, A.P. 18-1027, 11801 Mexico D.F. (Mexico)

    1997-07-01

    The Olmec culture was the first meso american civilization it presents its main establishment at the Veracruz and Tabasco states in Mexico. Owing to in time and to the weathering factors of the region as warmth, acid rain and that great humidity existing in the environment among others that have been provoked great erosion and damage on the pre hispanic monuments. Through Sem technique it was achieved the microstructural characterization of materials which conform the samples that correspond to those monuments where fundamentally feldspars have been found. It was determined the elemental composition of samples through Emission dispersive X-ray diffraction technique, the crystalline phases existing in samples were determined mainly finding feldspars, so of this way it was corroborated those obtained results through Sem. The materials characterization that are part of these pre hispanic monuments of La Ve nta park is essential for its conservation minimizing so the damage to pre hispanic pieces. (Author)

  19. Catalyst-free III-nitride Nanowires by Plasma-assisted Molecular Beam Epitaxy: Growth, Characterization, and Applications

    Science.gov (United States)

    Carnevale, Santino D.

    In the past twenty years, III-nitride devices have had an enormous impact on semiconductor-based technologies. This impact is seen in both optoelectronic and electronic devices. The aim of this dissertation is to take advantage of III-nitride nanowires grown by plasma-assisted molecular beam epitaxy to form heterostructures that are difficult or impossible to achieve in traditional, thin films. To do this, it is first necessary to establish the growth phase diagrams that correlate the characteristics of GaN nanowires to MBE growth conditions. By using the information in these growth maps we can control growth kinetics and the resulting nanowire structures by making strategic, timely changes to growth conditions. Using this control electronic and optoelectronic III-nitride nanowire devices are created. First, coaxially-oriented AlN/GaN nanowire resonant tunneling diodes are formed on Si substrates. Second, polarization-induced nanowire light emitting diodes (PINLEDs) are fabricated that exhibit electroluminescence at wavelengths from the deep UV into the visible. Because these PINLEDs utilize polarization doping, they can be formed with and without the use of dopants. Device and structural characterization are provided, including a detailed investigation of the mixed material polarity in these nanowires. Finally, the dissertation closes with a discussion of recent work and future ideas for optimizing the PINLED design.

  20. Entrapment of marine microalga, Isochrysis galbana, for biosorption of Cr(III) from aqueous solution: isotherms and spectroscopic characterization

    Science.gov (United States)

    Kadimpati, Kishore Kumar; Mondithoka, Krishna Prasad; Bheemaraju, Sarada; Challa, Venkata Ramachandra Murthy

    2013-03-01

    Microalga, Isochrysis galbana, biomass was entrapped into alginate gel by liquid curing method in the presence of Ca(II) ions. The biosorption of chromium(III) by the entrapped live algal biomass was studied in a batch system. The effect of initial cadmium concentration, pH, temperature and liquid and solid ratio on Cr(III) removal was investigated. The maximum experimental biosorption capacities for entrapped live algal biomass were found to be 335.27 mg Cr(III) g-1 of dry algal biomass. The kinetics of chromium biosorption was slow; approximately 75 % of biosorption took place in 2 h. The percent adsorption increased with increase in pH; pH 5 of the solution was found to favor adsorption very strongly. The equilibrium biosorption data were evaluated by Langmuir and Freundlich isotherm models, and was best described by Langmuir and Freundlich isotherms. The biosorbent was characterized and evaluated, the functional groups -OH, -COOH and C=O were involved in the biosorption process. Since binding capacity was relatively high for immobilized live algal biomass, those algal forms are to be considered as suitable biosorbent for the removal of chromium in wastewater treatment.

  1. Electro-Optical Properties Characterization of Fish Type III Antifreeze Protein

    OpenAIRE

    Salvay, Andrés G.; Santos, Javier; Howard, Eduardo I.

    2007-01-01

    Antifreeze proteins (AFPs) are ice-binding proteins that depress the freezing point of water in a non-colligative manner without a significant modification of the melting point. Found in the blood and tissues of some organisms (such as fish, insects, plants, and soil bacteria), AFPs play an important role in subzero temperature survival. Fish Type III AFP is present in members of the subclass Zoarcoidei. AFPIII are small 7-kDa—or 14-kDa tandem—globular proteins. In the present work, we study ...

  2. Nitroxylcob(III)Alamin: Synthesis And X-Ray Structural Characterization

    Energy Technology Data Exchange (ETDEWEB)

    Hannibal, L.; Smith, C.A.; Jacobsen, D.W.; Brasch, N.E.

    2009-06-01

    The long-elusive crystal structure of nitrosylcobalamin (NOCbl) reveals that the Co-N-O angle is 117.4-121.4{sup o}; hence, NOCbl is best described as nitroxylcob(III)alamin in the solid state (see picture: Co purple, N blue, O red, P orange, C gray, H white). The length of the Co-N bond trans to the NO ligand is typical of those seen when strong {beta}-axial ligands are positioned trans to the 5,6-dimethylbenzimidazole group.

  3. Hierarchical microstructures in CZT

    Energy Technology Data Exchange (ETDEWEB)

    Sundaram, S.K., E-mail: sk.sundaram@pnl.gov [Pacific Northwest National Laboratory, Richland, WA 99352 (United States); Henager, C.H.; Edwards, D.J.; Schemer-Kohrn, A.L.; Bliss, M.; Riley, B.R.; Toloczko, M.B. [Pacific Northwest National Laboratory, Richland, WA 99352 (United States); Lynn, K.G. [School of Mechanical and Materials Engineering, Washington State University, Pullman, WA 99164 (United States)

    2011-10-01

    Advanced characterization tools, such as electron backscatter diffraction and transmitted IR microscopy, are being applied to study critical microstructural features and orientation relations in as-grown CZT crystals to aid in understanding the relation between structure and properties in radiation detectors. Even carefully prepared single crystals of CZT contain regions of slight misorientation, Te-particles, and dislocation networks that must be understood for more accurate models of detector response. This paper describes initial research at PNNL into the hierarchy of microstructures observed in CZT grown via the vertical gradient freeze or vertical Bridgman method at PNNL and WSU.

  4. Hierarchical Microstructures in CZT

    Energy Technology Data Exchange (ETDEWEB)

    Sundaram, S. K.; Henager, Charles H.; Edwards, Danny J.; Schemer-Kohrn, Alan L.; Bliss, Mary; Riley, Brian J.; Toloczko, Mychailo B.; Lynn, Kelvin G.

    2011-10-01

    Advanced characterization tools, such as electron backscatter diffraction and transmitted IR microscopy, are being applied to study critical microstructural features and orientation relations in as-grown CZT crystals to aid in understanding the relation between structure and properties in radiation detectors. Even carefully prepared single crystals of CZT contain regions of slight misorientation, Te-particles, and dislocation networks that must be understood for more accurate models of detector response. This paper describes initial research at PNNL into the hierarchy of microstructures observed in CZT grown via the vertical gradient freeze or vertical Bridgman method at PNNL and WSU.

  5. Metalloprobes: Synthesis, Characterization, and Potency of a Novel Gallium(III) Complex in Human Epidermal Carcinoma Cells

    Science.gov (United States)

    Harpstrite, Scott E.; Prior, Julie; Rath, Nigam P.; Sharma, Vijay

    2009-01-01

    Multidrug resistance (MDR) mediated by overexpression of the MDR1 gene product, P-glycoprotein (Pgp), represents one of the best characterized barriers to chemotherapeutic treatment in cancer and may be a pivotal factor in progression of Alzheimer’s disease (AD). Thus, agents capable of probing Pgp-mediated transport could be beneficial in biomedical imaging. Herein, we synthesized and structurally characterized a gallium(III) complex of the naphthol-Schiff base ligand (5). The crystal structure revealed octahedral geometry for the metallodrug. Cytotoxicity profiles of 5 were evaluated in KB-3-1 (Pgp−) and KB-8-5 (Pgp+) human epidermal carcinoma cell lines. Compared with an LC50 (the half-maximal cytotoxic concentration) value of 1.93 μM in drug-sensitive (Pgp−) cells, the gallium(III) complex 5 demonstrated an LC50 value > 100 μM in drug-resistant (Pgp+) cells, thus indicating that 5 was recognized by the Pgp as its substrate, thereby extruded from the cells and sequestered away from their cytotoxic targets. Radiolabeled analogues of 5 could be beneficial in noninvasive imaging of Pgp-mediated transport in vivo. PMID:17617464

  6. Synthesis and spectroscopic characterization of some lanthanide(III nitrate complexes of ethyl 2-[2-(1-acetyl-2-oxopropylazo]-4,5-dimethyl-3-thiophenecarboxyate

    Directory of Open Access Journals (Sweden)

    CHEMPAKAM JANARDHANAN ATHIRA

    2011-02-01

    Full Text Available Ethyl 2-[2-(1-acetyl-2-oxopropylazo]-4,5-dimethyl-3-thiophenecarboxyate was synthesized by coupling diazotized ethyl 2-amino-4,5-dimethylthiophene-3-carboxylate with acetylacetone. Based on various spectral studies and elemental analysis, an intramolecularly hydrogen-bonded azo-enol structural form was assigned for the ligand. This ligand is versatile in forming a series of lanthanide(III complexes, viz., lanthanum(III, cerium(III, praseodymium(III, neodymium(III, samarium(III and gadolinium(III, which were characterized through various spectral studies, elemental analysis, magnetic susceptibility measurements, molar conductance and thermal analysis. The spectral data revealed that the ligand acted as a neutral tridentate, coordinating to the metal ion through one of the azo nitrogen atoms, the ester carbonyl and the enolic oxygen of the acetylacetone moiety, without deprotonation. Molar conductance values adequately supported their non-electrolytic nature. The ligand and lanthanum(III complex were subjected to X-ray diffraction studies. In addition, the lanthanum(III complex underwent a facile transesterification reaction on refluxing with methanol for a long period. The thermal behaviour of the lanthanum(III complex was also examined

  7. Evaluation of Reaction Rate Theory and Monte Carlo Methods for Application to Radiation-Induced Microstructural Characterization

    Energy Technology Data Exchange (ETDEWEB)

    Stoller, Roger E [ORNL; Golubov, Stanislav I [ORNL; Becquart, C. S. [Universite de Lille; Domain, C. [EDF R& D, Clamart, France

    2007-08-01

    The multiscale modeling scheme encompasses models from the atomistic to the continuum scale. Phenomena at the mesoscale are typically simulated using reaction rate theory, Monte Carlo, or phase field models. These mesoscale models are appropriate for application to problems that involve intermediate length scales, and timescales from those characteristic of diffusion to long-term microstructural evolution (~s to years). Although the rate theory and Monte Carlo models can be used simulate the same phenomena, some of the details are handled quite differently in the two approaches. Models employing the rate theory have been extensively used to describe radiation-induced phenomena such as void swelling and irradiation creep. The primary approximations in such models are time- and spatial averaging of the radiation damage source term, and spatial averaging of the microstructure into an effective medium. Kinetic Monte Carlo models can account for these spatial and temporal correlations; their primary limitation is the computational burden which is related to the size of the simulation cell. A direct comparison of RT and object kinetic MC simulations has been made in the domain of point defect cluster dynamics modeling, which is relevant to the evolution (both nucleation and growth) of radiation-induced defect structures. The primary limitations of the OKMC model are related to computational issues. Even with modern computers, the maximum simulation cell size and the maximum dose (typically much less than 1 dpa) that can be simulated are limited. In contrast, even very detailed RT models can simulate microstructural evolution for doses up 100 dpa or greater in clock times that are relatively short. Within the context of the effective medium, essentially any defect density can be simulated. Overall, the agreement between the two methods is best for irradiation conditions which produce a high density of defects (lower temperature and higher displacement rate), and for

  8. Microstructural characterization, formation mechanism and fracture behavior of the needle δ phase in Fe–Ni–Cr type superalloys with high Nb content

    Energy Technology Data Exchange (ETDEWEB)

    Ning, Yongquan, E-mail: luckyning@nwpu.edu.cn [School of Materials Science & Engineering, Northwestern Polytechnical University, Xi' an 710072 (China); Huang, Shibo [Anshan Iron & Steel Group Corporation Bayuquan Subsidiary Company, Bayuquan 115007 (China); Fu, M.W. [Department of Mechanical Engineering, Hong Kong Polytechnic University, Hung Hom, Kowloon, Hong Kong (China); Dong, Jie [Inspection & Research Institute of Boiler & Pressure Vessel of Jiangxi Province, Nanchang 330029 (China)

    2015-11-15

    Microstructural characterization, formation mechanism and fracture behavior of the needle δ phase in Fe–Ni–Cr type superalloys with high Nb content (GH4169, equivalent to Inconel 718) have been quantitatively investigated in this research. The typical microstructures of δ phases with the stick, mixed and needle shapes obviously present in Inconel 718 after the isothermal upsetting at the temperature of 980–1060 °C with the initial strain rate of 10{sup −3}–10{sup −1} s{sup −1}. It is found that the shape of the δ phase has a great effect on the mechanical properties of the alloy, viz., the stick δ phase behaves good plasticity and the needle δ phase has good strength. In addition, the needle δ phase can be used to control the grain size as it can prevent grain growth. The combined effect of the localized necking and microvoid coalescence leads to the final ductile fracture of the GH4169 components with the needle δ phase. Both dislocation motion and atom diffusion are the root-cause for the needle δ phase to be firstly separated at grain boundary and then at sub-boundary. The formation mechanism of the needle δ phase is the new finding in this research. Furthermore, it is the primary mechanism for controlling the needle δ phase in Fe–Ni–Cr type superalloys with high Nb content. - Highlights: • Shape of the δ phase takes great effect on mechanical property. • Needle δ phase plays a great role to prevent grain growth. • Needle δ phase can enhance the fracture strength. • Microstructure mechanism of the needle δ phase has been investigated. • Fracture behavior of the needle δ phase has been studied.

  9. Electro-optical properties characterization of fish type III antifreeze protein.

    Science.gov (United States)

    Salvay, Andrés G; Santos, Javier; Howard, Eduardo I

    2007-12-01

    Antifreeze proteins (AFPs) are ice-binding proteins that depress the freezing point of water in a non-colligative manner without a significant modification of the melting point. Found in the blood and tissues of some organisms (such as fish, insects, plants, and soil bacteria), AFPs play an important role in subzero temperature survival. Fish Type III AFP is present in members of the subclass Zoarcoidei. AFPIII are small 7-kDa-or 14-kDa tandem-globular proteins. In the present work, we study the behavior of several physical properties, such as the low-frequency dielectric permittivity spectrum, circular dichroism, and electrical conductivity of Fish Type III AFP solutions measured at different concentrations. The combination of the information obtained from these measurements could be explained through the formation of AFP molecular aggregates or, alternatively, by the existence of some other type of interparticle interactions. Thermal stability and electro-optical behavior, when proteins are dissolved in deuterated water, were also investigated.

  10. Ultrasonic spectrum analysis for in vivo characterization of tumor microstructural changes in the evaluation of tumor response to chemotherapy using diagnostic ultrasound.

    Science.gov (United States)

    Lin, Chun-yi; Cao, Long-hui; Wang, Jian-wei; Zheng, Wei; Chen, Yao; Feng, Zi-zhen; Li, An-hua; Zhou, Jian-hua

    2013-06-21

    There is a strong need for early assessment of tumor response to chemotherapy in order to avoid the adverse effects of unnecessary chemotherapy and to allow early transition to second-line therapy. The purpose of this study was to determine the feasibility of ultrasonic spectral analysis for the in vivo characterization of changes in tumor microstructure in the evaluation of tumor response to chemotherapy using diagnostic ultrasound. Experiments were approved by the regional animal care committee. Twenty-four MCF-7 breast cancer bearing nude mice were treated with adriamycin or sterile saline administered by intraperitoneal injection. Ultrasonic radio-frequency (RF) data was collected using a clinically available ultrasound scanner (6-MHz linear transducer). Linear regression parameters (spectral slope and midband-fit) regarding the calibrated power spectra from the RF signals were tested to monitor tumor response to treatment. The section equivalent to the ultrasound imaging plane was stained with hematoxylin and eosin to allow for assessment of the density of tumor cell nuclei. Treatment with adriamycin significantly reduced tumor growth in comparison with the control group (p = 0.003). Significant changes were observed in the ultrasonic parameters of the treated relative to the untreated tumors (p analysis can detect changes in tumor microstructure after chemotherapy, and this will be helpful in the early evaluation tumor response to chemotherapy.

  11. Microstructural characterization of the geopolymer obtained from iron-rich metakaolin; Caracterizacao microestrutural do geopolimero obtido de metacaulim rico em ferro

    Energy Technology Data Exchange (ETDEWEB)

    Vassalo, Erica Antunes de S.; Aguilar, Maria Teresa P.; Gumieri, Adriana Guerra, E-mail: ericaasv@gmail.com [Universidade Federal de Minas Gerais (UFMG), Belo Horizonte, MG (Brazil). Departamento de Engenharia de Materiais e Construcao Civil

    2014-07-01

    Geopolymer is a material derived from precursors rich in SiO{sub 2} and Al{sub 2}O{sub 3}, activated in an alkaline solution by means of a polymerization process. In this process, units of tetrahedral aluminosilicate structures are organized in repetitions that share oxygen. One of the precursors most commonly used to obtain geopolymer is metakaolin. Recent studies have reported iron enhancement in a partial replacement of the aluminium present in metakaolin. This paper presents the microstructural characterization and analysis of a geopolymer obtained by means of the activation of iron-rich metakaolin with sodium hydroxide at 12, 15 and 18 mol, both at room temperature and in an oven at 85±3°C. The geopolymers obtained were classified and analysed using X-ray fluorescence testing (EDX-720), a scanning electron microscope (SEM) and a Fourier transform infrared spectroscopy (FTIR). The results enabled an assessment of their physical-chemical and microstructural characteristics, as well as their reactive potential. (author)

  12. Surface Morphology of Fe(III-Porphyrin Thin Layers as Characterized by Atomic Force Microscopy

    Directory of Open Access Journals (Sweden)

    Utari Utari

    2016-12-01

    Full Text Available Surface morphology of Fe(III–porphyrin thin layers was studied using atomic force microscopy. The thin layer samples used in these experiments were deposited by spin coating methods on indium–tin-oxide substrates at room temperature under atmospheric conditions. Variations of thin layer of Fe(III-porphyrin were done by modifying the rotational speed and the concentration of the solution. The experimental results demonstrated that the Fe(III–porphyrin layers were observed as discrete nanomolecular islands. Both the number of nano-islands and thickness of the layer increased significantly with increasing concentration. A layer thickness of 15 nm was obtained for low concentrations of 0.00153 M and become 25 nm for dense concentrations of 0.153 M. Conversely, the higher number of islands were deposited on the surface of the substrate at a lower rotational speed.

  13. Characterization of type III kerogen from Tyrolean shale (Hahntennjoch, Austria based on its oxidation products

    Directory of Open Access Journals (Sweden)

    D. VITOROVIC

    2008-04-01

    Full Text Available A 29-step alkaline permanganate degradation of type III kerogen from Tyrolean (Hahntennjoch, Austria oil shale was performed. A high yield of oxidation products was obtained (93.7 % relative to the original kerogen: 0.5 % neutrals and bases, 19.5 % ether-soluble acids and 58.9 % of precipitated (PA. A substantial amount of kerogen carbon (14.8 % was oxidized into carbon dioxide. The organic residue remaining after the final oxidation step was 6.9 %. The PA components were further oxidized and the total yields relative to original PA were 1.0 % neutrals and bases and 59.0 % ether-soluble acids, the non-degraded residue being 29.3 %. Detailed quantitative and qualitative analysis of all oxidation products suggested the Tyrolean shale kerogen to be a heterogeneous macromolecular substance consisting of three types of structures differing in composition and susceptibility towards alkaline permanganate: the first, resistant, presumably composed of aromatic structures linked by resorcinol ethereal bonds; the second, combined in nature, the aliphatic part comprising methyl-substituents and short cross-links, both easily oxidized into CO2, water and low molecular weight acids and aromatic structures yielding aromatic di- and tri-carboxylic acids as oxidation products; finally the third, composed of aliphatic cross-links and substituents, alicyclic (and/or heterocyclic and some aromatic structures, bound into units moderately resistant towards oxidation. The overall yields of kerogen and PA oxidation products lead towards a balance between aromatic, alkane mono- and dicarboxylic and alkanepolycarboxylic acids, suggesting a shift of the structure of Tyrolean shale kerogen from typical aromatic reference type III towards a heterogeneous aromatic-aliphatic-alicyclic type structure.

  14. The Evolution of Solid Oxide Fuel Cell Nickel-Yttria Stabilized Zirconia Anodes Studied Using Electrochemical and Three-Dimensional Microstructural Characterizations

    Science.gov (United States)

    Kennouche, David O.

    This thesis focuses on Solid Oxide Fuel Cells (SOFCs). The 21st century will see major changes in the way energy is produced, stored, and used around the world. SOFCs, which provide an efficient, scalable, and low-pollution alternative method for electricity generation, are expected to play an important role. SOFCs can also be operated in electrolysis mode for energy storage, important since health and economic reasons are causing a shift towards intermittent renewable energy resources. However, multiple limitations mainly linked to cost and durability have prevented the expansion of this technology to mass markets. This work focuses on the Nickel - Yttria Stabilized Zirconia (Ni-YSZ) anode that is widely used in SOFCs. Coarsening of Ni in the Ni-YSZ anode has been widely cited as a primary cause of long-term SOFC degradation. While there have been numerous studies of Ni coarsening reported, these have typically only tracked the evolution of Ni particle size, not the entire microstructure, and have typically not been correlated directly with electrochemical performance. In this thesis, the advanced tomography techniques Focused Ion Beam - Scanning Electron Microscopy (FIB-SEM) tomography and Trans- mission X-ray Microscopy (TXM) have been utilized to enable insight into the evolution of Ni-YSZ structure and how it relates to performance degradation. Extensive anode aging studies were done for relatively short times using temperatures higher than in normal SOFC operation in order to accelerate microstructural evolution. In addition the microstructure changes were correlated with changes in anode polarization resistance. While most of the measurements were done by comparing different anodes aged under different conditions, the first example of a "pseudo in situ" measurement where the same anode was 3D imaged repeatedly with intervening aging steps, was also demonstrated. A microstructural evolution model that focuses on the active three-phase boundary density was

  15. Microstructural Characterization of Dislocation Networks During Harper-Dorn Creep of fcc, bcc, and hcp Metals and Alloys

    Energy Technology Data Exchange (ETDEWEB)

    Przystupa, Marek A.

    2007-12-13

    Harper-Dorn (H-D) creep is observed in metals and geological materials exposed to very low stresses at temperatures close to the melting point. It is one of several types of creep processes wherein the steady-state strain rate is proportional to the applied stress, Nabarro-Herring creep and Coble creep being two other important processes. H-D creep can be somewhat insidious because the creep rates are much larger than those expected for Nabarro-Herring or Coble creep. Since the working conditions of structural components of power plants and propulsion systems, as well as the motion of the earth’s mantle all involve very low stresses, an understanding of the factors controlling H-D creep is critical in preventing failures associated with those higher-than-expected creep rates. The purpose of this investigation was to obtain missing microstructural information on the evolution of the dislocation structures during static annealing of materials with fcc, bcc and hcp structure and use obtained results to test predictive capabilities of the dislocation network theory of H-D creep. In our view the evolutionary processes during static annealing and during Harper-Dorn creep are intimately related. The materials used in this study were fcc aluminum, hcp zinc and bcc tin. All characterizations of dislocation structures, densities and dislocation link length distributions were carried out using the etch pit method. To obtain quantitative information on the evolution of the dislocation networks during annealing the pure fcc aluminum samples were pre-deformed by creep at 913 and 620 K and then annealed. The higher deformation temperature was selected to generate starting dislocation networks similar to those forming during Harper-Dorn creep and the lower, to obtain higher dislocation densities suitable for reliable estimates of the parameters of the network growth law. The measured experimental link length distribution were, after scaling, (1) the same for all annealing

  16. Electroencephalographic characterization of seizure activity in the synapsin I/II double knockout mouse

    DEFF Research Database (Denmark)

    Etholm, Lars; Lindén, Henrik; Eken, Torsten

    2011-01-01

    a more gradual development with respect to the emergence of different EEG components and the frequency of these components. No EEG pattern was seen to define a particular seizure behavior. However, myoclonic activity was characterized by more regular patterns of combined sharp waves and spikes. Where...... by cortical activity but rather reflects interplay between cortical activity and activity in other brain regions....

  17. Synthesis, spectroscopic characterization, solid state d.c. electrical conductivity and biological studies of some lanthanide(III chloride complexes with a heterocyclic Schiff base ligand

    Directory of Open Access Journals (Sweden)

    K. Mohanan

    2016-07-01

    Full Text Available Condensation of 2-hydroxy-1-naphthaldehyde with 2-amino-3-carboxyethyl-4,5-dimethylthiophene in 1:1 molar ratio, yielded a potentially tridentate Schiff base viz. 2-[N-(2′-hydroxy-1-naphthylideneamino]-3-carboxyethyl-4,5-dimethylthiophene (HNAT. This ligand formed complexes with lanthanum(III, cerium(III, praseodymium(III, neodymium(III, samarium(III, europium(III and gadolinium(III chloride under well defined conditions. These complexes were characterized through elemental analysis, molar conductance, magnetic moment measurements, IR, UV–Vis, FAB mass and 1H NMR spectral studies. Analytical data showed that all the metal complexes exhibited 1:1 metal–ligand ratio. Molar conductance values adequately confirmed the non-electrolytic nature of the metal complexes. The proton NMR spectral observations supplement the IR spectral assignments. The spectral data revealed that the ligand acted as neutral tridentate, coordinating to the metal ion through azomethine nitrogen, ester carbonyl and naphtholate oxygen without deprotonation. The ligand and its lanthanum(III chloride complex were subjected to XRD studies. The lanthanum(III chloride complex has undergone a facile transesterification reaction. The solid state d.c. electrical conductivity of some selected complexes were measured as a function of temperature, indicating the semiconducting nature of the metal complexes. The antimicrobial activities were examined by disk diffusion method against some pathogenic bacterial and fungal species.

  18. Microstructural Characterization of Clad Interface in Welds of Ni-Cr-Mo High Strength Low Alloy Steel

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Hong-Eun; Kim, Min-Chul; Lee, Ho-Jin; Kim, Keong-Ho [KAERI, Daejeon (Korea, Republic of); Lee, Ki-Hyoung [KAIST, Daejeon (Korea, Republic of); Lee, Chang-Hee [Hanyang Univ., Seoul (Korea, Republic of)

    2011-08-15

    SA508 Gr.4N Ni-Cr-Mo low alloy steel, in which Ni and Cr contents are higher than in commercial SA508 Gr.3 Mn-Mo-Ni low alloy steels, may be a candidate reactor pressure vessel (RPV) material with higher strength and toughness from its tempered martensitic microstructure. The inner surface of the RPV is weld-cladded with stainless steels to prevent corrosion. The goal of this study is to evaluate the microstructural properties of the clad interface between Ni-Cr-Mo low alloy steel and stainless weldment, and the effects of post weld heat treatment (PWHT) on the properties. The properties of the clad interface were compared with those of commercial Mn-Mo-Ni low alloy steel. Multi-layer welding of model alloys with ER308L and ER309L stainless steel by the SAW method was performed, and then PWHT was conducted at 610°C for 30 h. The microstructural changes of the clad interface were analyzed using OM, SEM and TEM, and micro-Vickers hardness tests were performed. Before PWHT, the heat affected zone (HAZ) showed higher hardness than base and weld metals due to formation of martensite after welding in both steels. In addition, the hardness of the HAZ in Ni-Cr-Mo low alloy steel was higher than that in Mn-Mo-Ni low alloy steel due to a comparatively high martensite fraction. The hardness of the HAZ decreased after PWHT in both steels, but the dark region was formed near the fusion line in which the hardness was locally high. In the case of Mn-Mo-Ni low alloy steel, formation of fine Cr-carbides in the weld region near the fusion line by diffusion of C from the base metal resulted in locally high hardness in the dark region. However, the precipitates of the region in the Ni-Cr-Mo low alloy steel were similar to that in the base metal, and the hardness in the region was not greatly different from that in the base metal.

  19. Electrothermal and microstructural characterization of varistors ceramics used in high-voltage surge arresters; Caracterizacao eletrotermica e microestrutural de ceramicas varistoras utilizadas em para-raios de altas tensoes

    Energy Technology Data Exchange (ETDEWEB)

    Barbosa, Flavio Bittencourt; Furtado, Jose G. de Melo [Centro de Pesquisas de Energia Eletrica (CEPEL), Rio de Janeiro, RJ (Brazil); Nobrega, Maria C. de S. [Universidade Federal do Rio de Janeiro (COPPE/UFRJ), RJ (Brazil). Coordenacao dos Programas de Pos-Graduacao de Engenharia

    2008-07-01

    In this work is studied the electrothermal behavior of varistor ceramic blocks used in high voltage surge arresters of transmission and distribution lines, relating this behavior to microstructural characteristics of the studied varistor ceramics. We studied blocks of zinc oxide varistors with nominal voltage of 4.0 kV, by and voltage-capacitance characterization curves, reference voltage test, impulse residual voltage, polarization tests and induced degradation tests. On the other hand, the microstructural characterization was made by scanning electron microscopy and energy-dispersive spectroscopy. The obtained results allow to correlate the behavior of the resistive component of the leakage current with the microstructural characteristics of the studied varistors, specially in pre-breakdown region. (author)

  20. Formation, Characterization, and O-O Bond Activation of a Peroxomanganese(III) Complex Supported by a Cross-Clamped Cyclam Ligand.

    Science.gov (United States)

    Colmer, Hannah E; Howcroft, Anthony W; Jackson, Timothy A

    2016-03-07

    Although there have been reports describing the nucleophilic reactivity of peroxomanganese(III) intermediates, as well as their conversion to high-valent oxo-bridged dimers, it remains a challenge to activate peroxomanganese(III) species for conversion to high-valent, mononuclear manganese complexes. Herein, we report the generation, characterization, and activation of a peroxomanganese(III) adduct supported by the cross-clamped, macrocyclic Me2EBC ligand (4,11-dimethyl-1,4,8,11-tetraazabicyclo[6.6.2]hexadecane). This ligand is known to support high-valent, mononuclear Mn(IV) species with well-defined spectroscopic properties, which provides an opportunity to identify mononuclear Mn(IV) products from O-O bond activation of the corresponding Mn(III)-peroxo adduct. The peroxomanganese(III) intermediate, [Mn(III)(O2)(Me2EBC)](+), was prepared at low-temperature by the addition of KO2 to [Mn(II)(Cl)2(Me2EBC)] in CH2Cl2, and this complex was characterized by electronic absorption, electron paramagnetic resonance (EPR), and Mn K-edge X-ray absorption (XAS) spectroscopies. The electronic structure of the [Mn(III)(O2)(Me2EBC)](+) intermediate was examined by density functional theory (DFT) and time-dependent (TD) DFT calculations. Detailed spectroscopic investigations of the decay products of [Mn(III)(O2)(Me2EBC)](+) revealed the presence of mononuclear Mn(III)-hydroxo species or a mixture of mononuclear Mn(IV) and Mn(III)-hydroxo species. The nature of the observed decay products depended on the amount of KO2 used to generate [Mn(III)(O2)(Me2EBC)](+). The Mn(III)-hydroxo product was characterized by Mn K-edge XAS, and shifts in the pre-edge transition energies and intensities relative to [Mn(III)(O2)(Me2EBC)](+) provide a marker for differences in covalency between peroxo and nonperoxo ligands. To the best of our knowledge, this work represents the first observation of a mononuclear Mn(IV) center upon decay of a nonporphyrinoid Mn(III)-peroxo center.

  1. Microstructural characterization of titanium dental implants by electron microscopy and mechanical tests; Caracterizacao microestrutural de implantes dentarios de titanio por microscopia eletronica e ensaios mecanicos

    Energy Technology Data Exchange (ETDEWEB)

    Helfenstein, B.; Muniz, N.O.; Dedavid, B.A., E-mail: bruhelfenstein@hotmail.co [Pontificia Univ. Catolica do Rio Grande do Sul (FE/PUC/RS), Porto Alegre, RS (Brazil). Fac. de Engenharia; Gehrke, S.A. [Universidade Federal de Santa Maria (FE/UFSM), RS (Brazil). Fac. de Engenharia; Vargas, A.L.M. [Parque Tecnologico da PUCRS (TECNOPUC/GEPSI), Porto Alegre, RS (Brazil). Grupo de Estudos de Propriedades de Superficies e Interfaces

    2010-07-01

    Mini screw types for titanium implants, with differentiated design, were tested for traction and torsion for behavior analysis of the shape relative to the requirements of ASTM F136. All implants showed mechanical tensile strength above by the standard requirement, being that 83.3% of them broke above the doughnut, in support of the prosthesis. Distinct morphologies in ruptured by mechanical tests, were obtained. However, both fracture surfaces showed fragile comportments. Metallographic tests, x-ray diffraction (XRD) and microhardness were used for microstructural characterization of material, before and after heat treatment. The presences of {beta} phase in screw surface after quenching treatment proves that the thermal treatment can contribute for mechanical resistance in surface implants. (author)

  2. Mechanical and microstructural characterization of a HMX-based pressed explosive: Effects of combined high pressure and strain rate

    Science.gov (United States)

    Trumel, H.; Lambert, P.; Biessy, M.

    2012-08-01

    The paper presents a study of the combined effects of strain rate and confining pressure on the behaviour and microstructure evolutions of a HMX-based explosive. Hopkinson bar compression experiments are carried-out on samples confined with a brass sleeve. The latter is instrumented in order to determine the confining pressure on the explosive sample, directly function of the sleeve thickness and yield strength. A sample confined at 75 MPa and deformed at 250s-1 is recovered, cross-sectioned and studied using optical microscopy. Distributed microplasticity and microcracking appear similar to those induced by confined quasi-static experiments, indicating that stress triaxiality is the most important loading parameter. The sample also displays a large shear macrocrack, resulting from the formation of an adiabatic shear band. Shear banding seems to proceed by strong plastic strain gradients, followed by dynamic re-crystallization. Further strong thermal effects are observed, resulting in local reactive melting.

  3. Mechanical and microstructural characterization of a HMX-based pressed explosive: Effects of combined high pressure and strain rate

    Directory of Open Access Journals (Sweden)

    Biessy M.

    2012-08-01

    Full Text Available The paper presents a study of the combined effects of strain rate and confining pressure on the behaviour and microstructure evolutions of a HMX-based explosive. Hopkinson bar compression experiments are carried-out on samples confined with a brass sleeve. The latter is instrumented in order to determine the confining pressure on the explosive sample, directly function of the sleeve thickness and yield strength. A sample confined at 75 MPa and deformed at 250s−1 is recovered, cross-sectioned and studied using optical microscopy. Distributed microplasticity and microcracking appear similar to those induced by confined quasi-static experiments, indicating that stress triaxiality is the most important loading parameter. The sample also displays a large shear macrocrack, resulting from the formation of an adiabatic shear band. Shear banding seems to proceed by strong plastic strain gradients, followed by dynamic re-crystallization. Further strong thermal effects are observed, resulting in local reactive melting.

  4. Microstructural characterization of HIP consolidated NiTi–nano Al{sub 2}O{sub 3} composites

    Energy Technology Data Exchange (ETDEWEB)

    Farvizi, M., E-mail: mmfarvizi@yahoo.com [Ceramic Division, Materials and Energy Research Center, P.O. Box 14155-4777, Tehran (Iran, Islamic Republic of); Ebadzadeh, T. [Ceramic Division, Materials and Energy Research Center, P.O. Box 14155-4777, Tehran (Iran, Islamic Republic of); Vaezi, M.R. [Nanotechnology and Advanced Materials Division, Materials and Energy Research Center, P.O. Box 14155-4777, Tehran (Iran, Islamic Republic of); Yoon, E.Y.; Kim, Y-J. [Korea Institute of Materials Science, Changwon 642-831 (Korea, Republic of); Kim, H.S. [Department of Materials Science and Engineering, Pohang University of Science and Technology, Pohang 790-784 (Korea, Republic of); Simchi, A. [Department of Materials Science and Engineering and Institute for Nanoscience and Nanotechnology, Sharif University of Technology, P.O. Box 11365-9466, Tehran (Iran, Islamic Republic of)

    2014-09-01

    Highlights: • NiTi–6 wt.% nano α-Al{sub 2}O{sub 3} composites have been produced using a HIP method. • Both elemental and prealloyed powders were used for the fabrication of composites. • Generation of mismatch stress and intermetallics affected martensitic transformation. • Nanoparticles partially inhibited thermally induced martensitic transformation. • An interwoven austenite–martensite structure was observed in the composite samples. - Abstract: The microstructure and phase transformational behavior of NiTi-based composites reinforced with 6 wt.% of α-alumina nanoparticles have been investigated. Two kinds of starting materials, elemental Ni–Ti and prealloyed austenitic NiTi, were used to prepare the composites. The samples were consolidated using a hot isostatic pressing method. The X-ray diffraction results showed that while unreinforced NiTi mainly contained B2 phase at room temperature, martensitic B19′ phase appeared in the microstructure after addition of the α-alumina nanoparticles. The differential scanning calorimetry measurements indicated that the martensitic transformation temperatures were elevated in the composite samples, but the transformational enthalpy was reduced in comparison with the NiTi sample. It is believed that the generation of thermal mismatch stress during the sintering and the formation of small contents of NiTi{sub 2}/Ni{sub 3}Ti intermetallics in the composite samples are responsible for this increment of the martensitic transformation temperatures. Also, due to the nanometric size of α-Al{sub 2}O{sub 3}, a larger fraction of the matrix is disturbed by the presence of the nanoparticles, which yields the formation of effective barriers to the thermally induced martensitic transformation in the nanocomposite samples. The high-resolution transmission electron microscopy studies of the samples confirmed the higher defect density and partial microplastic deformation in the composite samples.

  5. Morphological and microstructural characterization of nanostructured pure α-phase W coatings on a wide thickness range

    Energy Technology Data Exchange (ETDEWEB)

    Gordillo, N., E-mail: nuri.gordillo@gmail.com [Instituto de Fusión Nuclear, ETSI de Industriales, Universidad Politécnica de Madrid, C/José Gutierrez Abascal, 2, E-28006 Madrid (Spain); CEI Campus Moncloa, UCM-UPM, Madrid (Spain); Panizo-Laiz, M. [Instituto de Fusión Nuclear, ETSI de Industriales, Universidad Politécnica de Madrid, C/José Gutierrez Abascal, 2, E-28006 Madrid (Spain); Tejado, E. [Department of Materials Science, Research Centre on Safety and Durability of Structures and Materials (CISDEM), UPM-CSIC, C/Profesor Aranguren s/n, E-28040 Madrid (Spain); Centro Nacional de Investigaciones Metalúrgicas, CENIM-CSIC, Madrid (Spain); Fernandez-Martinez, I. [Instituto de Energía Solar (IES), Universidad Politécnica de Madrid, Avenida Complutense s/n, E-28040 Madrid (Spain); Instituto de Microelectrónica de Madrid, IMM-CNM-CSIC, Isaac Newton 8 PTM, Tres Cantos, E-28760 Madrid (Spain); Rivera, A. [Instituto de Fusión Nuclear, ETSI de Industriales, Universidad Politécnica de Madrid, C/José Gutierrez Abascal, 2, E-28006 Madrid (Spain); Pastor, J.Y. [Department of Materials Science, Research Centre on Safety and Durability of Structures and Materials (CISDEM), UPM-CSIC, C/Profesor Aranguren s/n, E-28040 Madrid (Spain); Castro, C. Gómez de [Departamento de Física de Materiales, Facultad de CC. Químicas, Universidad Complutense de Madrid, Ciudad Universitaria s/n, E-28040 Madrid (Spain); and others

    2014-10-15

    Highlights: • Pure α-phase tungsten nanostructures were deposited by DC-magnetron sputtering. • Non-delaminated coatings were achieved at powers ≤50 W. • The coating thicknesses vary from 30 nm up to ∼4.0 μm. • The influence of the substrate on the coating properties was investigated. • We report on the morphological, microstructural and mechanical properties. - Abstract: Nanostructured tungsten (nanoW) coatings have been deposited by DC magnetron sputtering. First, the influence of the sputtering power on the adhesion of the coatings to the substrate was investigated by depositing coatings at powers varying from 30 up to 220 W. Non-delaminated coatings were achieved at powers ≤50 W. Second, the influence of coating thickness on the morphological, microstructural and mechanical properties was investigated for films deposited at 50 W with thicknesses varying from 30 nm up to ∼4.0 μm. SEM images reveal that all the films are highly compact, consisting of nanometer sized columns that grow perpendicular to the substrate. XRD data evidence that films are monophasic, being made of pure α-phase. All coatings show compressive stress and low micro-strain. Nanoindentation tests show that coatings have a hardness higher than that reported for coarse grained W. No significant dependence of the previous properties on coating thickness was observed. Finally, the influence of the substrate on coatings properties was studied, by depositing a W coating at a power of 50 W on a commercial steel substrate: no significant dependence was found.

  6. Development of a fermented ice-cream as influenced by in situ exopolysaccharide production: Rheological, molecular, microstructural and sensory characterization.

    Science.gov (United States)

    Dertli, Enes; Toker, Omer S; Durak, M Zeki; Yilmaz, Mustafa T; Tatlısu, Nevruz Berna; Sagdic, Osman; Cankurt, Hasan

    2016-01-20

    This study aimed to investigate the role of in situ exopolysaccharide (EPS) production by EPS(+)Streptococcus thermophilus strains on physicochemical, rheological, molecular, microstructural and sensory properties of ice cream in order to develop a fermented and consequently functional ice-cream in which no stabilizers would be required in ice-cream production. For this purpose, the effect of EPS producing strains (control, strain 1, strain 2 and mixture) and fermentation conditions (fermentation temperature; 32, 37 and 42 °C and time; 2, 3 and 4h) on pH, S. thermophilus count, EPS amount, consistency coefficient (K), and apparent viscosity (η50) were investigated and optimized using single and multiple response optimization tools of response surface methodology. Optimization analyses indicated that functional ice-cream should be fermented with strain 1 or strain mixture at 40-42 °C for 4h in order to produce the most viscous ice-cream with maximum EPS content. Optimization analysis results also revealed that strain specific conditions appeared to be more effective factor on in situ EPS production amount, K and η50 parameters than did fermentation temperature and time. The rheological analysis of the ice-cream produced by EPS(+) strains revealed its high viscous and pseudoplastic non-Newtonian fluid behavior, which demonstrates potential of S. thermophilus EPS as thickening and gelling agent in dairy industry. FTIR analysis proved that the EPS in ice-cream corresponded to a typical EPS, as revealed by the presence of carboxyl, hydroxyl and amide groups with additional α-glycosidic linkages. SEM studies demonstrated that it had a web-like compact microstructure with pores in ice-cream, revealing its application possibility in dairy products to improve their rheological properties. Copyright © 2015. Published by Elsevier Ltd.

  7. Detailed Microstructural Characterization and Restoration Mechanisms of Duplex and Superduplex Stainless Steel Friction-Stir-Welded Joints

    Science.gov (United States)

    Santos, T. F. A.; Torres, E. A.; Lippold, J. C.; Ramirez, A. J.

    2016-12-01

    Duplex stainless steels are successfully used in a wide variety of applications in areas such as the food industry, petrochemical installations, and sea water desalination plants, where high corrosion resistance and high mechanical strength are required. However, during fusion welding operations, there can be changes to the favorable microstructure of these materials that compromise their performance. Friction stir welding with a non-consumable pin enables welded joints to be obtained in the solid state, which avoids typical problems associated with solidification of the molten pool, such as segregation of alloying elements and the formation of solidification and liquefaction cracks. In the case of superduplex stainless steels, use of the technique can avoid unbalanced proportions of ferrite and austenite, formation of deleterious second phases, or growth of ferritic grains in the heat-affected zone. Consolidated joints with full penetration were obtained for 6-mm-thick plates of UNS S32101 and S32205 duplex stainless steels, and S32750 and S32760 superduplex steels. The welding heat cycles employed avoided the conditions required for formation of deleterious phases, except in the case of the welded joint of the S32760 steel, where SEM images indicated the formation of secondary phases, as corroborated by decreased mechanical performance. Analysis using EBSD and transmission electron microscopy revealed continuous dynamic recrystallization by the formation of cellular arrays of dislocations in the ferrite and discontinuous dynamic recrystallization in the austenite. Microtexture evaluation indicated the presence of fibers typical of shear in the thermomechanically affected zone. These fibers were not obviously present in the stir zone, probably due to the intensity of microstructural reformulation to which this region was subjected.

  8. Some studies on mechanical properties and microstructural characterization of automated TIG welding of thin commercially pure titanium sheets

    Energy Technology Data Exchange (ETDEWEB)

    Karpagaraj, A.; Siva shanmugam, N., E-mail: nsiva@nitt.edu; Sankaranarayanasamy, K.

    2015-07-29

    Gas Tungsten Arc Welding (GTAW) is a commonly used welding process for welding Titanium materials. Welding of titanium and its alloys poses several intricacies to the designer as they are prone to oxidation phenomenon. To overcome this contamination, a relatively new type of shielding arrangement is experimented. The proposed design and arrangement have been employed for joining commercially pure titanium sheets with variations in the GTAW process parameters namely the welding current and travel speed. Bead on plate (BoP) trials were conducted on thin sheets of 2 mm thickness by varying the process parameters. Subsequently, the macro structure images were captured. Based on these results, the process parameters are chosen for carrying out full penetration butt joints on 1.6 mm and 2 mm thick titanium sheets. The influences of these parameters of GTAW on the microstructure, mechanical properties and surface morphology at the fractured locations of the welded joints are examined. The microstructural properties of base metal, heat affected zone and fusion zone are analyzed through optical microscopy. The welded joints showed an ultimate tensile strength of about 383 MPa with 15.7% elongation. The hardness value at fusion zone and base metal are typically observed to be 191 and 153 HV-0.5, respectively. X-ray diffraction study is conducted to examine the chemical composition in the parent metal and fusion zone of the weld. Fractured surface is examined using Scanning Electron Microscopy which revealed dimple kind of rupture present at the fractured surfaces owing to insufficient or excessive heat with slight impurities that prevents the accomplishment of stronger micro-level weld integrity.

  9. Structural and Functional Characterization of the Bacterial Type III Secretion Export Apparatus.

    Directory of Open Access Journals (Sweden)

    Tobias Dietsche

    2016-12-01

    Full Text Available Bacterial type III protein secretion systems inject effector proteins into eukaryotic host cells in order to promote survival and colonization of Gram-negative pathogens and symbionts. Secretion across the bacterial cell envelope and injection into host cells is facilitated by a so-called injectisome. Its small hydrophobic export apparatus components SpaP and SpaR were shown to nucleate assembly of the needle complex and to form the central "cup" substructure of a Salmonella Typhimurium secretion system. However, the in vivo placement of these components in the needle complex and their function during the secretion process remained poorly defined. Here we present evidence that a SpaP pentamer forms a 15 Å wide pore and provide a detailed map of SpaP interactions with the export apparatus components SpaQ, SpaR, and SpaS. We further refine the current view of export apparatus assembly, consolidate transmembrane topology models for SpaP and SpaR, and present intimate interactions of the periplasmic domains of SpaP and SpaR with the inner rod protein PrgJ, indicating how export apparatus and needle filament are connected to create a continuous conduit for substrate translocation.

  10. Structural characterization of a novel Chlamydia pneumoniae type III secretion-associated protein, Cpn0803.

    Directory of Open Access Journals (Sweden)

    Chris B Stone

    Full Text Available Type III secretion (T3S is an essential virulence factor used by gram-negative pathogenic bacteria to deliver effector proteins into the host cell to establish and maintain an intracellular infection. Chlamydia is known to use T3S to facilitate invasion of host cells but many proteins in the system remain uncharacterized. The C. trachomatis protein CT584 has previously been implicated in T3S. Thus, we analyzed the CT584 ortholog in C. pneumoniae (Cpn0803 and found that it associates with known T3S proteins including the needle-filament protein (CdsF, the ATPase (CdsN, and the C-ring protein (CdsQ. Using membrane lipid strips, Cpn0803 interacted with phosphatidic acid and phosphatidylinositol, suggesting that Cpn0803 may associate with host cells. Crystallographic analysis revealed a unique structure of Cpn0803 with a hydrophobic pocket buried within the dimerization interface that may be important for binding small molecules. Also, the binding domains on Cpn0803 for CdsN, CdsQ, and CdsF were identified using Pepscan epitope mapping. Collectively, these data suggest that Cpn0803 plays a role in T3S.

  11. Structural characterization of a novel Chlamydia pneumoniae type III secretion-associated protein, Cpn0803.

    Science.gov (United States)

    Stone, Chris B; Sugiman-Marangos, Seiji; Bulir, David C; Clayden, Rob C; Leighton, Tiffany L; Slootstra, Jerry W; Junop, Murray S; Mahony, James B

    2012-01-01

    Type III secretion (T3S) is an essential virulence factor used by gram-negative pathogenic bacteria to deliver effector proteins into the host cell to establish and maintain an intracellular infection. Chlamydia is known to use T3S to facilitate invasion of host cells but many proteins in the system remain uncharacterized. The C. trachomatis protein CT584 has previously been implicated in T3S. Thus, we analyzed the CT584 ortholog in C. pneumoniae (Cpn0803) and found that it associates with known T3S proteins including the needle-filament protein (CdsF), the ATPase (CdsN), and the C-ring protein (CdsQ). Using membrane lipid strips, Cpn0803 interacted with phosphatidic acid and phosphatidylinositol, suggesting that Cpn0803 may associate with host cells. Crystallographic analysis revealed a unique structure of Cpn0803 with a hydrophobic pocket buried within the dimerization interface that may be important for binding small molecules. Also, the binding domains on Cpn0803 for CdsN, CdsQ, and CdsF were identified using Pepscan epitope mapping. Collectively, these data suggest that Cpn0803 plays a role in T3S.

  12. Chemistry Characterization of Jet Aircraft Engine Particulate by XPS: Results from APEX III

    Science.gov (United States)

    Vander Wal, Randy L.; Bryg, Victoria M.

    2014-01-01

    This paper reports XPS analysis of jet exhaust particulate from a B737, Lear, ERJ, and A300 aircraft during the APEX III NASA led field campaign. Carbon hybridization and bonding chemistry are identified by high-resolution scans about the C1s core-shell region. Significant organic content as gauged by the sp3/sp2 ratio is found across engines and platforms. Polar oxygen functional groups include carboxylic, carbonyl and phenol with combined content of 20 percent or more. By lower resolution survey scans various elements including transition metals are identified along with lighter elements such as S, N, and O in the form of oxides. Burning additives within lubricants are probable sources of Na, Ba, Ca, Zn, P and possibly Sn. Elements present and their percentages varied significantly across all engines, not revealing any trend or identifiable cause for the differences, though the origin is likely the same for the same element when observed. This finding suggests that their presence can be used as a tracer for identifying soots from aircraft engines as well as diagnostic for monitoring engine performance and wear.

  13. Characterization and reactivity of a terminal nickel(III)-oxygen adduct.

    Science.gov (United States)

    Pirovano, Paolo; Farquhar, Erik R; Swart, Marcel; Fitzpatrick, Anthony J; Morgan, Grace G; McDonald, Aidan R

    2015-02-23

    High-valent terminal metal-oxygen adducts are hypothesized to be the potent oxidizing reactants in late transition metal oxidation catalysis. In particular, examples of high-valent terminal nickel-oxygen adducts are scarce, meaning there is a dearth in the understanding of such oxidants. A monoanionic Ni(II)-bicarbonate complex has been found to react in a 1:1 ratio with the one-electron oxidant tris(4-bromophenyl)ammoniumyl hexachloroantimonate, yielding a thermally unstable intermediate in high yield (ca. 95%). Electronic absorption, electronic paramagnetic resonance, and X-ray absorption spectroscopies and density functional theory calculations confirm its description as a low-spin (S = 1/2), square planar Ni(III)-oxygen adduct. This rare example of a high-valent terminal nickel-oxygen complex performs oxidations of organic substrates, including 2,6-di-tert-butylphenol and triphenylphosphine, which are indicative of hydrogen atom abstraction and oxygen atom transfer reactivity, respectively. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  14. Characterization of Nops, nodulation outer proteins, secreted via the type III secretion system of NGR234.

    Science.gov (United States)

    Marie, Corinne; Deakin, William J; Viprey, Virginie; Kopciñska, Joanna; Golinowski, Wladyslaw; Krishnan, Hari B; Perret, Xavier; Broughton, William J

    2003-09-01

    The nitrogen-fixing symbiotic bacterium Rhizobium species NGR234 secretes, via a type III secretion system (TTSS), proteins called Nops (nodulation outer proteins). Abolition of TTSS-dependent protein secretion has either no effect or leads to a change in the number of nodules on selected plants. More dramatically, Nops impair nodule development on Crotalaria juncea roots, resulting in the formation of nonfixing pseudonodules. A double mutation of nopX and nopL, which code for two previously identified secreted proteins, leads to a phenotype on Pachyrhizus tuberosus differing from that of a mutant in which the TTSS is not functional. Use of antibodies and a modification of the purification protocol revealed that NGR234 secretes additional proteins in a TTSS-dependent manner. One of them was identified as NopA, a small 7-kDa protein. Single mutations in nopX and nopL were also generated to assess the involvement of each Nop in protein secretion and nodule formation. Mutation of nopX had little effect on NopL and NopA secretion but greatly affected the interaction of NGR234 with many plant hosts tested. NopL was not necessary for the secretion of any Nops but was required for efficient nodulation of some plant species. NopL may thus act as an effector protein whose recognition is dependent upon the hosts' genetic background.

  15. Microstructural and fabric characterization of brittle-ductile transitional deformation of middle crustal rocks along the Jinzhou detachment fault zone, Northeast China

    Science.gov (United States)

    Zhang, Juyi; Jiang, Hao; Liu, Junlai

    2017-04-01

    Detachment fault zones (DFZs) of metamorphic core complexes generally root into the middle crust. Exhumed DFZs therefore generally demonstrate structural, microstructural and fabric features characteristic of middle to upper crustal deformation. The Jinzhou detachment fault zone from the Liaonan metamorphic core complex is characterized by the occurrence of a sequence of fault rocks due to progressive shearing along the fault zone during exhumation of the lower plate. From the exhumed fabric zonation, cataclastic rocks formed in the upper crust occur near the Jinzhou master detachment fault, and toward the lower plate gradually changed to mylonites, mylonitic gneisses and migmatitic gneisses. Correspondingly, these fault rocks have various structural, microstructural and fabric characteristics that were formed by different deformation and recrystallization mechanisms from middle to upper crustal levels. At the meanwhile, various structural styles for strain localization were formed in the DFZ. As strain localization occurs, rapid changes in deformation mechanisms are attributed to increases in strain rates or involvement of fluid phases during the brittle-ductile shearing. Optical microscopic studies reveal that deformed quartz aggregates in the lower part of the detachment fault zone are characterized by generation of dynamically recrystallized grains via SGR and BLG recrystallization. Quartz rocks from the upper part of the DFZ have quartz porphyroclasts in a matrix of very fine recrystallized grains. The porphyroclasts have mantles of sub-grains and margins grain boundary bulges. Electron backscattered diffraction technique (EBSD) quartz c-axis fabric analysis suggests that quartz grain aggregates from different parts of the DFZ possess distinct fabric complexities. The c-axis fabrics of deformed quartz aggregates from mylonitic rocks in the lower part of the detachment fault zone preserve Y-maxima which are ascribed to intermediate temperature deformation (500

  16. Characterization of the hierarchical microstructure of a Ni-Al-Ti model alloy; Charakterisierung der hierarchischen Mikrostruktur einer Ni-Al-Ti Modell-Legierung

    Energy Technology Data Exchange (ETDEWEB)

    Vogel, Florian

    2014-02-28

    Phase separation of γ{sup '} precipitates determines the microstructure and mechanical properties of nickel-based superalloys. Upon ageing, γ spheres form inside ordered (L1{sub 2}) γ{sup '} precipitates, undergo a morphological change to plates and finally split the γ{sup '} precipitates. To clarify the identity of the insufficiently characterized γ particles and to elucidate their influence on the evolution of the microstructure and the mechanical properties, differently heat treated samples of a Ni-Al-Ti modell alloy were investigated from the micrometer to the atomic scale. The single crystalline cast material was broadly characterized by means of light and scanning electron microscopy, the laue method (back-reflection), differential scanning calorimetry as well as electron probe microanalysis. Dendritic segregations were found, whereas the dendrite cores show an enrichment in nickel and aluminum and in turn the interdendritic regions show an enrichment in titanium. An adequate combination of temperature and time was determined on the basis of quantitative analyses after different homogenization treatments. The evolution of the hierarchical microstructure was investigated on the nanometer scale by means of transmission electron microscopy and on the atomic scale with atom probe tomography. The combined analyses reveal that Ni-rich clusters form within the γ{sup '} precipitates during the early stages of phase separation. These Ni-rich clusters coalesce and thereby form γ spheres which undergo a morphological change to plates accompanied by a chemical evolution. In the beginning the γ spheres are located well within the metastable γ + γ{sup '} two-phase region and later, after the morphological change, achieve the equilibrium composition of the γ phase. Furthermore the involved energies were considered in order to elucidate the driving forces for the phase separation of γ{sup '} precipitates. A correlation between the

  17. Sonochemical synthesis, characterization, antimicrobial activity and textile dyeing behavior of nano-sized cobalt(III) complexes.

    Science.gov (United States)

    Bala, Ritu; Behal, Jagriti; Kaur, Varinder; Jain, Subheet Kumar; Rani, Riveka; Manhas, Rajesh Kumari; Prakash, Vinit

    2017-03-01

    Using ultrasonic irradiations, nano-sized cobalt(III) coordination complexes, [Co(NH3)6]Cl3·2H2O (A), [Co(en)3]Cl3·3H2O (B) (en-ethylenediamine) and [Co(dien)2]Cl3·3.5H2O (C) (dien-diethylenetriamine) were synthesized. These complexes were characterized by spectroscopic studies like IR, UV/Visible and NMR. Morphology of these complexes was determined by SEM and particle size with the help of TEM & Zeta-sizer. The comparative thermal stability along with phase difference between nano structures and their respective bulk complexes has been studied by thermal gravimetric analysis (TGA) and X-ray powder diffraction (XRD) study respectively. The dyeing behavior of nano-sized Co(III) complexes and their respective bulks has also been studied (using both exhaust and pad dyeing methods) on cotton and wool fabrics and results shown rationalized dyeing behavior. All these complexes were further tested for antimicrobial activity (against B. subtilis, E. coli, K. pneumoniae, F. oxysporum and A. alternate) and it was observed that nano sized complexes enhanced the activity further. Copyright © 2016 Elsevier B.V. All rights reserved.

  18. EQCM behavior of copper anodes in alkaline medium and characterization of the electrocatalysis of ethanol oxidation by Cu(III

    Directory of Open Access Journals (Sweden)

    Paixão Thiago R. L. C.

    2006-01-01

    Full Text Available The anodic oxidation of copper electrodes in alkaline solutions was investigated by using voltammetry, chronoamperometry, impedance measurements and the electrochemical quartz crystal microbalance (EQCM. Experiments were carried out in NaOH solutions in the 0.1 to 3.0 mol L-1 concentration range. The formation of soluble and insoluble species such as Cu(OH4(2- and Cu2O during the electrodic dissolution of copper anodes was characterized by analyzing potentiodynamic mass responses and the relationship between mass changes and charge. On the other hand, EQCM data were not effective to confirm the nature of other copper species proposed in literature named as CuO and Cu(OH2 because of viscoelastic changes in the film layer electrodeposited onto the quartz crystal. The participation of a Cu(III soluble species in the electrocatalytic oxidation of ethanol was proved by EQCM measurements, data providing valuable information on the mechanism of the electrode process and formation of a Cu(II insoluble species from the reaction of Cu(III with ethanol.

  19. Microstructural features of Mg-8%Sn alloy and its correlation with mechanical properties

    National Research Council Canada - National Science Library

    Palash Poddar; Ashok Kamaraj; A.P. Murugesan; Sumanta Bagui; K.L. Sahoo

    2017-01-01

    .... Mechanical properties evaluation and corresponding microstructural characterizations were performed to correlate their strength and ductility properties with their microstructural features (i.e...

  20. Synthesis and characterization of meridional isomer of uns-cis-(ethylenediamine-N-N'-di-3-propionato-(S-norleucinatocobalt(III semihydrate

    Directory of Open Access Journals (Sweden)

    SRECKO R. TRIFUNOVIC

    2000-07-01

    Full Text Available The meridional geometrical isomer of uns-cis-(ethylenediamine-N-N'-di-3-propionato(S-norleucinatocobalt(III complex has been prepared by the reaction of sodium uns-cis-(ethylenediamine-N-N'-di-3-propionato(carbonatocobaltate(III with S-norleucine at 75°C. The complex was isolated choromatographically and characterized by elemental analyses, electron absorption and infrared spectroscopy.

  1. Characterization of phosphoproteins from electrophoretic gels by nanoscale Fe(III) affinity chromatography with off-line mass spectrometry analysis

    DEFF Research Database (Denmark)

    Stensballe, A; Andersen, Søren; Jensen, Ole Nørregaard

    2001-01-01

    Detailed characterization of phosphoproteins as well as other post-translationally modified proteins is required to fully understand protein function and regulatory events in cells and organisms. Here we present a mass spectrometry (MS) based experimental strategy for the identification and mapping...... chromatography (Fe(III)-IMAC) columns were employed for enrichment of phosphorylated peptides from crude peptide mixtures prior to off-line analysis by matrix-assisted laser desorption/ionization (MALDI) MS or nanoelectrospray tandem mass spectrometry (MS/MS). An optimized and sensitive procedure for alkaline...... of phosphorylation sites. The advantages and limitations of the experimental strategy was demonstrated by enrichment, identification and sequencing of phosphopeptides from the model proteins ovalbumin and bovine beta-casein isolated by gel electrophoresis. Furthermore, an autophosphorylation site at Ser-3...

  2. Preparation of monolayers of [MnIII 6CrIII]3+ single-molecule magnets on HOPG, mica and silicon surfaces and characterization by means of non-contact AFM

    Directory of Open Access Journals (Sweden)

    Hoeke Veronika

    2011-01-01

    Full Text Available Abstract We report on the characterization of various salts of [MnIII 6CrIII]3+ complexes prepared on substrates such as highly oriented pyrolytic graphite (HOPG, mica, SiO2, and Si3N4. [MnIII 6CrIII]3+ is a single-molecule magnet, i.e., a superparamagnetic molecule, with a blocking temperature around 2 K. The three positive charges of [MnIII 6CrIII]3+ were electrically neutralized by use of various anions such as tetraphenylborate (BPh4 -, lactate (C3H5O3 -, or perchlorate (ClO4 -. The molecule was prepared on the substrates out of solution using the droplet technique. The main subject of investigation was how the anions and substrates influence the emerging surface topology during and after the preparation. Regarding HOPG and SiO2, flat island-like and hemispheric-shaped structures were created. We observed a strong correlation between the electronic properties of the substrate and the analyzed structures, especially in the case of mica where we observed a gradient in the analyzed structures across the surface.

  3. Computer vision in microstructural analysis

    Science.gov (United States)

    Srinivasan, Malur N.; Massarweh, W.; Hough, C. L.

    1992-01-01

    The following is a laboratory experiment designed to be performed by advanced-high school and beginning-college students. It is hoped that this experiment will create an interest in and further understanding of materials science. The objective of this experiment is to demonstrate that the microstructure of engineered materials is affected by the processing conditions in manufacture, and that it is possible to characterize the microstructure using image analysis with a computer. The principle of computer vision will first be introduced followed by the description of the system developed at Texas A&M University. This in turn will be followed by the description of the experiment to obtain differences in microstructure and the characterization of the microstructure using computer vision.

  4. Expression, refolding and spectroscopic characterization of fibronectin type III (FnIII)-homology domains derived from human fibronectin leucine rich transmembrane protein (FLRT)-1,-2, and-3

    DEFF Research Database (Denmark)

    Yang, Lila; Falkesgaard, Maria Hansen; Thulstrup, Peter Waaben

    2017-01-01

    The fibronectin leucine rich transmembrane (FLRT) protein family consists in humans of 3 proteins, FLRT1, -2, and -3. The FLRT proteins contain two extracellular domains separated by an unstructured linker. The most membrane distal part is a leucine rich repeat (LRR) domain responsible for both cis......- and trans-interactions, whereas the membrane proximal part is a fibronectin type III (FnIII) domain responsible for a cis-interaction with members of the fibroblast growth factor receptor 1 (FGFR1) family, which results in FGFR tyrosine kinase activation. Whereas the structures of FLRT LRR domains from...

  5. Synthesis and preliminary structural characterization of some lanthanide(III semicarbazone complex

    Directory of Open Access Journals (Sweden)

    Ram K. Agarwal

    2006-06-01

    Full Text Available Some six and nine coordinated complexes of trivalent lanthanide metal ions with 4[N-(2'-hydroxy-1'-naphthalideneamino]antipyrinesemicarbazone (HNAAPS with the general composition LnX3.n(HNAAPS [X = NO3, n = 1; X = NCS or ClO4, n = 2; Ln = La, Pr, Nd, Sm, Gd, Tb, Dy or Ho] have been isolated. All the complexes have been characterized on the basis of analytical data, molar conductance, magnetic susceptibility, electronic and infrared spectral measurements. The ligand HNAAPS behaves as neutral tridentate (N, N, O ligand. The coordination number of the central metal ion is either six or nine in these complexes. Thermal properties of these complexes were also investigated.

  6. The synthesis, characterization and theoretical study of nano tetrabuthylammonium trichloroiodoaluminate (III

    Directory of Open Access Journals (Sweden)

    shahriar Ghammamy

    2012-10-01

    Full Text Available There is provided a nano aluminate complex that has a quaternary ammonium cation. This nano system has an equal molar ratio of Al to N that has been prepared by reaction of an organic salt R+X- such as [(CH34NBr], and a Lewis acid such as AlCl3, compounds. The synthesized compound was characterized by IR, Mass, X-Ray diffraction measurements. In addition, the structure of synthesized compound was optimized at the theoretical level of the Moller-Plesser perturbations of the second order (MP2, with LanL2DZ basis set and molecular specifications such as band length and angle were extracted using Gaussian 98 program. Theoretical data show good agreement with the experimental result.

  7. Characterizing the microstructural basis of “unidentified bright objects” in neurofibromatosis type 1: A combined in vivo multicomponent T2 relaxation and multi-shell diffusion MRI analysis

    Directory of Open Access Journals (Sweden)

    Thibo Billiet

    2014-01-01

    Conclusion: Our results suggest that demyelination and axonal degeneration are unlikely to be present in UBOs, which appear to be mainly caused by a shift towards a higher T2-value of the intra- and extracellular water pool. This may arise from altered microstructural compartmentalization, and an increase in ‘extracellular-like’, intracellular water, possibly due to intramyelinic edema. These findings confirm the added value of combining dMRI and MET2 to characterize the microstructural basis of T2 hyperintensities in vivo.

  8. Characterization of deliberately nickel-doped silicon wafers and solar cells. [microstructure, electrical properties, and energy conversion efficiency

    Science.gov (United States)

    Salama, A. M.

    1980-01-01

    Microstructural and electrical evaluation tests were performed on nickel-doped p-type silicon wafers before and after solar cell fabrication. The concentration levels of nickel in silicon were 5 x 10 to the 14th power, 4 x 10 to the 15th power, and 8 x 10 to the 15th power atoms/cu cm. It was found that nickel precipitated out during the growth process in all three ingots. Clumps of precipitates, some of which exhibited star shape, were present at different depths. If the clumps are distributed at depths approximately 20 micron apart and if they are larger than 10 micron in diameter, degradation occurs in solar cell electrical properties and cell conversion efficiency. The larger the size of the precipitate clump, the greater the degradation in solar cell efficiency. A large grain boundary around the cell effective area acted as a gettering center for the precipitates and impurities and caused improvement in solar cell efficiency. Details of the evaluation test results are given.

  9. Microstructure and sliding wear characterization of Cu/TiB2 copper matrix composites fabricated via friction stir processing

    Directory of Open Access Journals (Sweden)

    I. Dinaharan

    2017-09-01

    Full Text Available The poor wear performance of copper is improved by reinforcing hard ceramic particles. The present work reports the fabrication of Cu/TiB2 (0, 6, 12, 18 vol.% copper matrix composites (CMCs using friction stir processing (FSP. TiB2 particles were initially packed together into a machined groove and were subjected to FSP under a constant set of process parameters. The microstructure was observed using optical, scanning and transmission electron microscopy. The wear behavior was examined using a pin-on-disc apparatus. The micrographs showed a homogeneous distribution of TiB2 particles without aggregation and segregation. The distribution of TiB2 particles was closely persistent across the stir zone. TiB2 particles were well bonded with the copper matrix without any interfacial reaction. Many TiB2 particles fractured during FSP. The grains in the composite were extensively refined because of dynamic recrystallization and pinning effect of TiB2 particles. The wear behavior under dry sliding condition was presented in detail.

  10. Classification of Induced Magnetic Field Signals for the Microstructural Characterization of Sigma Phase in Duplex Stainless Steels

    Directory of Open Access Journals (Sweden)

    Edgard M. Silva

    2016-07-01

    Full Text Available Duplex stainless steels present excellent mechanical and corrosion resistance properties. However, when heat treated at temperatures above 600 ∘ C, the undesirable tertiary sigma phase is formed. This phase presents high hardness, around 900 HV, and it is rich in chromium, the material toughness being compromised when the amount of this phase is not less than 4%. This work aimed to develop a solution for the detection of this phase in duplex stainless steels through the computational classification of induced magnetic field signals. The proposed solution is based on an Optimum Path Forest classifier, which was revealed to be more robust and effective than Bayes, Artificial Neural Network and Support Vector Machine based classifiers. The induced magnetic field was produced by the interaction between an applied external field and the microstructure. Samples of the 2205 duplex stainless steel were thermal aged in order to obtain different amounts of sigma phases (up to 18% in content. The obtained classification results were compared against the ones obtained by Charpy impact energy test, amount of sigma phase, and analysis of the fracture surface by scanning electron microscopy and X-ray diffraction. The proposed solution achieved a classification accuracy superior to 95% and was revealed to be robust to signal noise, being therefore a valid testing tool to be used in this domain.

  11. Compositional, thermal and microstructural characterization of the Nopal (opuntia ficus indica), for addition in commercial cement mixtures

    Science.gov (United States)

    Hernández Carrillo, C. G.; Gómez-Cuaspud, J. A.; E Martínez Suarez, C.

    2017-12-01

    The Nopal (opuntia ficus indica) from remote times has contributed like food and additive product in prehispanic constructions; although it grows in all the Colombian territory is very little used and its contribution in mixtures of Colombian cement is unknown. In order to evaluate the hydration characteristics of Nopal, several Thermogravimetric Analysis (TGA) were performed to evaluate the optimal temperature of dehydration. Initially, the results show that around 175°C the weight loss is approximately 95%, this mass loss corresponds to the process of physical removal, suggesting that at least a remaining amount of 5% (w/w) has the ability to retain large amounts of water which is stored in the micro-structural deposits of Nopal. The evaluation by means Scanning Electron Microscopy (SEM), confirm that the whole cactus structure enables the water storage at cellular level. The results of infrared spectroscopy (FT-IR) and Energy Dispersive X-ray (EDX) analysis allowed the qualitative and semi-quantitative evaluation of the presence of functional groups and elemental chemical composition of Nopal respectively, mainly related with polysaccharide functional groups, which corresponds to 85% of the total composition. Other functional groups, are related with protein and mineral components. This found characteristics are relevant for the water retention in process that require the decrease of water consumption and the reinforcing of mechanical properties and durability, due to ability of Nopal mucilage to restore its hydration characteristics.

  12. Characterization of optical and microstructural properties of semitransparent TiO{sub 2}/Ti/glass interference decorative coatings

    Energy Technology Data Exchange (ETDEWEB)

    Skowronski, L., E-mail: lukasz.skowronski@utp.edu.pl; Wachowiak, A.A.; Grabowski, A.

    2016-12-01

    Highlights: • The interference color TiO{sub 2}/Ti/glass systems were produced using the GIMS. • The thicknesses of Ti films (12–73 nm) is associated with the transmittance of samples. • The thicknesses of TiO{sub 2} film determine the color of a sample from gold (11 nm) to blue (47 nm). • The samples with thicker titanium film exhibit more saturated colors. • The elaborated method can be used to produce architectural glazing. - Abstract: This paper presents a study of the optical properties and the microstructure of semitransparent interference TiO{sub 2}/Ti/glass systems obtained by gas injection magnetron sputtering (GIMS). The samples are examined by means of spectroscopic ellipsometry, spectrophotometry and atomic force microscopy. The investigation is complemented by colorimetric measurements. Optical constants of titanium and titanium dioxide layers are determined and carefully studied. An influence of the deposition time on the thickness of metallic and dielectric films has been found. The thickness of Ti films ranges from 12 nm to 73 nm, while that of TiO{sub 2} films varies from 11 nm to 43 nm. This thickness directly determines the color of a sample from gold to blue, respectively.

  13. Characterizing ingestive behavior through licking microstructure: Underlying neurobiology and its use in the study of obesity in animal models.

    Science.gov (United States)

    Johnson, Alexander W

    2017-07-03

    Ingestive behavior is controlled by multiple distinct peripheral and central physiological mechanisms that ultimately determine whether a particular food should be accepted or avoided. As rodents consume a fluid they display stereotyped rhythmic tongue movements, and by analyzing the temporal distribution of pauses of licking, it is possible through analyses of licking microstructure to uncover dissociable evaluative and motivational variables that contribute to ingestive behavior. The mean number of licks occurring within each burst of licking (burst and cluster size) reflects the palatability of the consumed solution, whereas the frequency of initiating novel bouts of licking behavior (burst and cluster number) is dependent upon the degree of gastrointestinal inhibition that accrues through continued fluid ingestion. This review describes the analysis of these measures within a context of the behavioral variables that come to influence the acceptance or avoidance of a fluid, and the neurobiological mechanisms that underlie alterations in the temporal distribution of pauses of licks. The application of these studies to models of obesity in animals is also described. Copyright © 2017 ISDN. Published by Elsevier Ltd. All rights reserved.

  14. Microstructural characterization and mechanical properties of dissimilar friction welding of 1060 aluminum to AZ31B magnesium alloy

    Energy Technology Data Exchange (ETDEWEB)

    Liang, Zhida; Qin, Guoliang, E-mail: glqin@sdu.edu.cn; Wang, Liyuan; Meng, Xiangmeng; Li, Fei

    2015-10-01

    Dissimilar welding of aluminum bars and magnesium bars was produced by the friction welding technique. The interfacial microstructure characteristics was evaluated after friction welding of Al–Mg alloy using optical microscopy, scanning electron microscopy, as well as X-ray diffraction analysis. Friction and forge pressure were selected as variable parameters. The friction time was maintained at 10 s for a rotational speed of 2800 rpm. The chemical compositions of the interfaces of the welded joints were determined by using energy dispersive spectroscopy. Experimental results showed that intermetallic compounds (IMCs), consisting of phase β-Al{sub 3}Mg{sub 2} and γ-Al{sub 12}Mg{sub 17}, were generated in the interfaces of the Al and Mg alloys. When the friction and forge pressure increased the thickness of IMCs layer at the interfaces decreased as a result of more mass discarded from the welding interfaces. Heavy thickness of IMCs layer seriously deteriorated the mechanical properties of the joints. Microcracks were generated along the welded interfaces of all the welded samples. Formation of microcracks could be controlled effectively under the higher friction and forge pressure. Mechanical evaluations were conducted by determining microhardness and the tensile tests. It was observed that the tensile strength of the joints depended on the friction and forge pressure and the maximum tensile strength was 138 MPa.

  15. Simultaneous saccharification and fermentation of corncobs with genetically modified Saccharomyces cerevisiae and characterization of their microstructure during hydrolysis.

    Science.gov (United States)

    Song, Hui-Ting; Liu, Shi-Hui; Gao, Yuan; Yang, Yi-Min; Xiao, Wen-Jing; Xia, Wu-Cheng; Liu, Zi-Lu; Li, Rong; Ma, Xiang-Dong; Jiang, Zheng-Bing

    2016-04-01

    Cellulose is an abundant natural polysaccharide that is universally distributed. It can be extracted from corncobs, which are inexpensive, easily accessible, renewable, and environmentally friendly. A common strategy for effectively utilizing cellulose is efficient heterogeneous expression of cellulase genes in Saccharomyces cerevisiae. However, the improvement of cellulose utilization is a relevant issue. Based on our previous findings, we constructed an integrated secretion expression vector, pHBM368-pgk, containing a constitutive promoter sequence. Three genetically modified S. cerevisiae strains containing heterologous β-glucosidase, exoglucanase, and endoglucanase genes were constructed. The results of a 1-L bioreactor fermentation process revealed that the mixed recombinant S. cerevisiae could efficiently carry out simultaneous saccharification and fermentation (SSF) by using corncobs as the sole carbon source. The ethanol concentration reached 6.37 g/L after 96 hours of fermentation, which was about 3 times higher than that produced by genetically modified S. cerevisiae with the inducible promoter sequence. To investigate the microstructure characteristics of hydrolyzed corncobs during the fermentation process, corncob residues were detected by using a scanning electron microscope. This study provides a feasible method to improve the effect of SSF using corncobs as the sole carbon source.

  16. Microstructure-hardness relationship in the fusion zone of TRIP steel welds

    Energy Technology Data Exchange (ETDEWEB)

    Nayak, S.S., E-mail: sashank@uwaterloo.ca [Center for Advanced Materials Joining, Mechanical and Mechatronics Engineering, University of Waterloo, Waterloo, ON N2L 3G1 (Canada); Baltazar Hernandez, V.H. [Center for Advanced Materials Joining, Mechanical and Mechatronics Engineering, University of Waterloo, Waterloo, ON N2L 3G1 (Canada); MPyM-EPMM Academic Unit of Engineering, Autonomous University of Zacatecas, C.P. 98000 Zacatecas (Mexico); Okita, Y. [Center for Advanced Materials Joining, Mechanical and Mechatronics Engineering, University of Waterloo, Waterloo, ON N2L 3G1 (Canada); Joining and Strength Research Department, JFE Steel Corporation, Chiba 260-0835 (Japan); Zhou, Y. [Center for Advanced Materials Joining, Mechanical and Mechatronics Engineering, University of Waterloo, Waterloo, ON N2L 3G1 (Canada)

    2012-08-15

    Highlights: Black-Right-Pointing-Pointer Fusion zone of TRIP steels in resistance spot welding was analyzed. Black-Right-Pointing-Pointer Transmission electron microscopy (TEM) was used for characterizing microstructure. Black-Right-Pointing-Pointer Fusion zone microstructure was found to depend on the chemistry. Black-Right-Pointing-Pointer Hardness values were in accordance with the microstructural constituents in the fusion zone. - Abstract: Fusion zone of three TRIP steels, categorized as AT: C-Mn-Al, AST: C-Mn-Al-Si and ST: C-Mn-Si, in resistance spot welding was characterized with respect to microstructure, phase analysis, and hardness. The fusion zone microstructure was found to depend on chemistry: (i) AT steel contained ferrite phase surrounded by bainite and martensite regions, (ii) AST steel showed a bainite structures along with martensite laths and interlath retained austenite, whereas (iii) ST steel constituted single phase martensite laths with interlath austenite. X-ray diffraction study indicated that retained austenite fraction in the fusion zone increases with increase in Si content in it. The AST fusion zone hardness lies between those of the AT and ST steels; the ST fusion zone hardness was higher than that of AT steel because of the single phase martensite microstructure. Comparison of fusion zone microstructure and hardness to earlier study on laser welding of the TRIP steels with similar chemistries revealed that higher cooling rate in resistance spot welding led to higher fusion zone hardness compared to laser welding; which was attributed either to decrease in softer ferrite phase (AT steel) in the microstructure or refinement of martensite laths (ST steel).

  17. Preparation and Characterization of Cerium (III Doped Captopril Nanoparticles and Study of their Photoluminescence Properties

    Directory of Open Access Journals (Sweden)

    Ghamami Shahriar

    2016-01-01

    Full Text Available In this research Ce3+ doped Captopril nanoparticles (Ce3+ doped CAP-NP were prepared by a cold welding process and have been studied. Captopril may be applied in the treatment of hypertension and some types of congestive heart failure and for preventing kidney failure due to high blood pressure and diabetes. CAP-NP was synthesized by a cold welding process. The cerium nitrate was added at a ratio of 10% and the optical properties have been studied by photoluminescence (PL. The synthesized compounds were characterized by Fourier transform infrared spectroscopy. The size of CAP-NP was calculated by X-ray diffraction (XRD. The size of CAP-NP was in the range of 50 nm. Morphology of surface of synthesized nanoparticles was studied by scanning electron microscopy (SEM. Finally the luminescence properties of undoped and doped CAP-NP were compared. PL spectra from undoped CAP-NP show a strong pack in the range of 546 nm after doped cerium ion into the captopril appeared two bands at 680 and 357 nm, which is ascribed to the well-known 5d–4f emission band of the cerium.

  18. Aminergic systems in pulmonate gastropod molluscs. III. Microspectrofluorometric characterization of the monoamines in the reproductive system.

    Science.gov (United States)

    Hartwig, H G; Brisson, P; Lyncker, I; Collin, J P

    1980-01-01

    Histochemical fluorescence (Falck-Hillarp) and microspectrofluorometric (MSF) methods were used to characterize different types of catecholamine-containing cellular elements located in the reproductive system of fresh-water snails (Bulinus truncatus, Planorbarius corneus) and land snails [Archachatina marginata, Helix (Cryptomphalus) aspersa]. Transverse sections through the genital tract display a common structural pattern of tubular differentiations: (1) an internal epithelium bordering the lumen and containing variable numbers of monoaminergic cells; (2) an enveloping sheath of connective and muscular tissue containing fine nerve fibers in the form of a network that exhibits a variable degree of density. MSF determinations showed that the formaldehyde-induced fluorophores of the intraepithelial aminergic cells belong to the following classes: (1) the DOPA/dopamine group in the duct of the albumen gland of B. truncatus and the carrefour of A. marginata; and (2) the norepinephrine/epinephrine group in the duct of the albumen gland and in the oviduct sac of P. corneus. In the reproductive systems of B. truncatus and P. corneus (duct of the albumen gland, oviduct sac, vagina), A. marginata and H. aspersa (duct of the fertilization pocket, origin of the receptaculum seminis, carrefour), the MSF analysis revealed norepinephrine/epinephrine-containing intramural nerve fibers. On the other hand, the small neurons in the vagina of B. truncatus belong to the DOPA/dopamine group.

  19. Microstructure characterization of Al matrix composite reinforced with Ti-6Al-4V meshes after compression by scanning electron microscope and transmission electron microscope.

    Science.gov (United States)

    Guo, Q; Sun, D L; Han, X L; Cheng, S R; Chen, G Q; Jiang, L T; Wu, G H

    2012-02-01

    Compressive properties of Al matrix composite reinforced with Ti-6Al-4V meshes (TC4(m)/5A06 Al composite) under the strain rates of 10(-3)S(-1) and 1S(-1) at different temperature were measured and microstructure of composites after compression was characterized by scanning electron microscope (SEM) and transmission electron microscope (TEM). Compressive strength decreased with the test temperature increased and the strain-rate sensitivity (R) of composite increased with the increasing temperature. SEM observations showed that grains of Al matrix were elongated severely along 45° direction (angle between axis direction and fracture surface) and TC4 fibres were sheared into several parts in composite compressed under the strain rate of 10(-3)S(-1) at 25°C and 250°C. Besides, amounts of cracks were produced at the interfacial layer between TC4 fibre and Al matrix and in (Fe, Mn)Al(6) phases. With the compressive temperature increasing to 400°C, there was no damage at the interfacial layer between TC4 fibre and Al matrix and in (Fe, Mn)Al(6) phases, while equiaxed recrystal grains with sizes about 10 μm at the original grain boundaries of Al matrix were observed. However, interface separation of TC4 fibres and Al matrix occurred in composite compressed under the strain rate of 1S(-1) at 250°C and 400°C. With the compressive temperature increasing from 25°C to 100°C under the strain rate of 10(-3) S(-1), TEM microstructure in Al matrix exhibited high density dislocations and slipping bands (25°C), polygonized dislocations and dynamic recovery (100°C), equiaxed recrystals with sizes below 500 μm (250°C) and growth of equiaxed recrystals (400°C), respectively. Copyright © 2011 Elsevier Ltd. All rights reserved.

  20. Partial purification and characterization of exopolygalacturonase II and III of Penicillium frequentans Purificação parcial e caracterização das exopoligalacturonases II e III de Penicillium frequentans

    Directory of Open Access Journals (Sweden)

    Renata I. Barense

    2001-12-01

    Full Text Available Previous studies from our laboratory have demonstrated that the fungus Penicillium frequentans produces high levels of polygalacturonase and pectinesterase. Endopolygalacturonase I (Endo-PG I and Exopolygalacturonase I (Exo-PG I were previously purified and characterized. In the present study two extracellular polygalacturonases were separated, partially purified and biochemically characterized. Both were characterized as exopolygalacturonases so they were named exopolygalacturonase II (Exo-PG II and exopolygalacturonase III (Exo-PG III which had a molecular mass of 63 kDa (Exo-PG II and 79 kDa (Exo-PG III. The Km values were 1.6 and 0.059 g/L and the Vmax values were 2571 and 185 U/mg, respectively. The optimum temperature was 50ºC for both enzymes, while the optimum pH was 5.0 for Exo-PG II and 5.8 for Exo-PG III.Estudos prévios realizados em nosso laboratório demonstraram que o fungo Penicillium frequentans produz altos níveis de poligalacturonase e pectinesterase. Endopoligalacturonase I (Endo-PG I e Exopoligalacturonase I (Exo-PG I já foram previamente purificadas e caracterizadas. No presente trabalho foram separadas, purificadas parcialmente e caracterizadas bioquimicamente duas poligalacturonases extracelulares. Ambas foram caracterizadas como exopoligalacturonases e então foram designadas exopoligalacturonase II (Exo-PG II e exopoligalacturonase III (Exo-PG III as quais apresentaram massa molecular de 63 kDa (Exo-PG II e 79 kDa (Exo-PG III. Os valores de Km foram 1,6 e 0,059 g/L e os de Vmáx = 2571 e 185 U/mg, respectivamente. A temperatura ótima de ambas foi 50ºC e enquanto o pH ótimo da Exo-PG II foi 5,0 o da Exo-PG III foi 5,8.

  1. Role of Microstructure on the Performance of UHTCs

    Science.gov (United States)

    Johnson, Sylvia M.; Gasch, Matthew J.; Lawson, John W.; Gusman, Michael I.; Stackpoole, Mairead

    2010-01-01

    We have investigated a number of methods to control microstructure. We have routes to form: a) in situ "composites" b) Very fine microstructures. Arcjet testing and other characterization of monolithic materials. Control oxidation through microstructure and composition. Beginning to incorporate these materials as matrices for composites. Modeling effort to facilitate material design and characterization.

  2. Octafluorodirhenate(III) Revisited: Solid-State Preparation, Characterization, and Multiconfigurational Quantum Chemical Calculations

    Energy Technology Data Exchange (ETDEWEB)

    Mariappan Balasekaran, Samundeeswari; Todorova, Tanya K.; Pham, Chien Thang; Hartmann, Thomas; Abram, Ulrich; Sattelberger, Alfred P.; Poineau, Frederic

    2016-06-06

    A simple method for the high-yield preparation of (NH4)2[Re2F8]· 2H2O has been developed that involves the reaction of (n-Bu4N)2[Re2Cl8] with molten ammonium bifluoride (NH4HF2). Using this method, the new salt [NH4]2[Re2F8]·2H2O was prepared in ~90% yield. The product was characterized in solution by ultraviolet-visible light (UV-vis) and 19F nuclear magnetic resonance (19F NMR) spectroscopies and in the solid-state by elemental analysis, powder X-ray diffraction (XRD), and infrared (IR) spectroscopy. Multiconfigurational CASSCF/CASPT2 quantum chemical calculations were performed to investigate the molecular and electronic structure, as well as the electronic absorption spectrum of the [Re2F8] 2- anion. The metal-metal bonding in the Re2 6+ unit was quantified in terms of effective bond order (EBO) and compared to that of its [Re2Cl8] 2- and [Re2Br8] 2- analogues.

  3. Mononuclear Mn(III) and Mn(IV) bis-terpyridine complexes: electrochemical formation and spectroscopic characterizations.

    Science.gov (United States)

    Romain, Sophie; Baffert, Carole; Duboc, Carole; Leprêtre, Jean-Claude; Deronzier, Alain; Collomb, Marie-Noëlle

    2009-04-06

    The electrochemical behavior of two mononuclear Mn(II) bis-terpyridine complexes, [Mn(II)(L)(2)](2+) (L = terpy (2,2':6',2''-terpyridine) and (t)Bu(3)-terpy (4,4',4''-tritert-butyl-2,2':6',2''-terpyridine)), has been investigated in dry CH(3)CN. Under these conditions, the cyclic voltammograms of these complexes exhibit not only the well-known Mn(II)/Mn(III) oxidation system but also a second metal-based oxidation one, corresponding to the Mn(III)/Mn(IV) redox couple. These oxidative processes are located at E(1/2) = +0.96 and +1.77 V vs Ag/Ag(+) (+1.26 and +2.07 V vs SCE) for the terpy complex and E(1/2) = +0.85 and +1.56 V vs Ag/Ag(+) (+1.15 and +1.86 V vs SCE) for the (t)Bu(3)-terpy derivative. The one-electron oxidized form of these complexes, [Mn(III)(L)(2)](3+), has been quantitatively generated by exhaustive electrolyses at E = 1.30 V, as previously observed in the case of the oxidation of [Mn(II)(tolyl-terpy)(2)](2+) (tolyl-terpy = 4'-(4-Methylphenyl)-2,2':6',2''-terpyridine) (Romain, S.; Duboc, C.; Neese, F.; Riviere, E.; Hanton, L. R.; Blackman, A. G.; Lepretre, J.-C.; Deronzier, A.; Collomb, M.-N. Chem.Eur. J. 2009, 15, 980-988). Further electrolyses at E = 1.65-1.80 V of [Mn(III)(L)(2)](3+) solutions have shown that the [Mn(IV)(L)(2)](4+) species is only stable for L = (t)Bu(3)-terpy because of the strong electron-donating properties of the tert-butyl substituents. These electrogenerated high-valent complexes are rare examples of mononuclear Mn(III) and Mn(IV) complexes stabilized solely by neutral N ligands. They have been fully characterized in solution by UV-visible and electron paramagnetic resonance (EPR) spectroscopies. A detailed investigation of the EPR spectra of the [Mn(II)((t)Bu(3)-terpy)(2)](2+) and [Mn(IV)((t)Bu(3)-terpy)(2)](4+) has allowed the determination of the spin Hamiltonian parameters for both systems (for Mn(II): |D| = 0.059 cm(-1); |E| = 0.014 cm(-1); E/D = 0.259; g(x) = g(y) = g(z) = 2.00 and for Mn(IV): |D| = 1.33(6) cm(-1); |E

  4. Synthesis and micro-structural characterization of graphene/strontium hexaferrite (SrFe{sub 12}O{sub 19}) nanocomposites

    Energy Technology Data Exchange (ETDEWEB)

    Durmus, Zehra, E-mail: zdurmus@bezmialem.edu.tr [Department of Pharmaceutical Biotechnology, Bezmialem Vakif University, 34093, Fatih, Istanbul (Turkey); Kavas, Huseyin [Department of Engineering Physics, Istanbul Medeniyet University, 34700, Kadıköy, Istanbul (Turkey); Durmus, Ali [Department of Chemical Engineering, Istanbul University, 34320, Avcılar, Istanbul (Turkey); Aktaş, Bekir [Department of Physics, Gebze Technical University, 41400, Gebze, Kocaeli (Turkey)

    2015-08-01

    In this study, novel type carbon/ferrite nanocomposites were successfully prepared by decoration of graphene sheets with the magnetic strontium hexaferrite nanoparticles synthesized via the citrate sol–gel combustion method as microwave absorbing material. The microstructural features and physical properties of nanocomposites were characterized by Fourier transform infrared spectroscopy (FTIR), X-Ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and atomic force microscopy (AFM) methods. Magnetic properties of the nanocomposites were determined by a vibrating sample magnetometer (VSM). It was found that the surface of the graphene nanosheets were successfully decorated with the strontium hexaferrite nanoparticles and the resulting layered nanocomposite structures exhibited sufficiently high magnetic saturation values compared to the agglomerated structure of strontium hexaferrite nanoparticles although the nanocomposites include less active magnetic component than the bulk hexaferrite. - Highlights: • Novel type, two-dimensional carbon-ferrite nanocomposites were prepared. • 2D graphene sheets were successfully decorated with the SrFe{sub 12}O{sub 19} nanoparticles. • Morphologies of nanocomposites were characterized with SEM, TEM and AFM methods. • Graphene/SrFe{sub 12}O{sub 19} nanocomposites exhibited sufficiently high M{sub s} values.

  5. Evaluation of five CAD/CAM materials by microstructural characterization and mechanical tests: a comparative in vitro study.

    Science.gov (United States)

    Sonmez, Nesrin; Gultekin, Pinar; Turp, Volkan; Akgungor, Gokhan; Sen, Deniz; Mijiritsky, Eitan

    2018-01-08

    Polymer infiltrated ceramics and nano-ceramic resins are the new restorative materials which have been developed in order to enhance the adverse properties of glass-matrix ceramics and resin composites. The aim of the present in vitro study was to evaluate the characteristics of various CAD/CAM materials through mechanical, microstructural, and SEM analysis. Five test groups (n = 22) were formed by using the indicated CAD/CAM blocks: VITA Enamic (VITA Zahnfabrik), Lava Ultimate (3 M ESPE), IPS e.max CAD (Ivoclar Vivadent), IPS Empress CAD (Ivoclar Vivadent), and VITA Mark II (VITA Zahnfabrik). Two specimens from each test group were used for XRD and EDS analysis. Remaining samples were divided into two subgroups (n = 10). One subgroup specimens were thermocycled (5 °C to 55 °C, 30s, 10,000 cycles) whereas the other were not. All of the specimens were evaluated in terms of flexural strength, Vickers hardness, and fracture toughness. Results were statistically analyzed using two-way ANOVA, one-way ANOVA, Tukey's HSD, and Student's t tests (α = .05). Fractured specimens were evaluated using SEM. The highest Vickers microhardness value was found for VITA Mark II (p CAD was found to have the highest flexural strength (p CAD was also higher than other tested block materials (p CAD groups. It should be realised that simulated aging process seem to affect ceramic-polymer composite materials more significantly than glass ceramics.

  6. Characterization of microstructure and texture across dissimilar super duplex/austenitic stainless steel weldment joint by austenitic filler metal

    Energy Technology Data Exchange (ETDEWEB)

    Eghlimi, Abbas, E-mail: a.eghlimi@ma.iut.ac.ir [Department of Materials Engineering, Isfahan University of Technology, Isfahan 84156-83111 (Iran, Islamic Republic of); Shamanian, Morteza [Department of Materials Engineering, Isfahan University of Technology, Isfahan 84156-83111 (Iran, Islamic Republic of); Eskandarian, Masoomeh [Department of Materials Engineering, Shiraz University, Shiraz 71348-51154 (Iran, Islamic Republic of); Zabolian, Azam [Department of Natural Resources, Isfahan University of Technology, Isfahan 84156-83111 (Iran, Islamic Republic of); Szpunar, Jerzy A. [Department of Mechanical Engineering, University of Saskatchewan, Saskatoon, SK S7N 5A9 (Canada)

    2015-08-15

    The evolution of microstructure and texture across an as-welded dissimilar UNS S32750 super duplex/UNS S30403 austenitic stainless steel joint welded by UNS S30986 (AWS A5.9 ER309LMo) austenitic stainless steel filler metal using gas tungsten arc welding process was evaluated by optical micrography and EBSD techniques. Due to their fabrication through rolling process, both parent metals had texture components resulted from deformation and recrystallization. The weld metal showed the highest amount of residual strain and had large austenite grain colonies of similar orientations with little amounts of skeletal ferrite, both oriented preferentially in the < 001 > direction with cub-on-cube orientation relationship. While the super duplex stainless steel's heat affected zone contained higher ferrite than its parent metal, an excessive grain growth was observed at the austenitic stainless steel's counterpart. At both heat affected zones, austenite underwent some recrystallization and formed twin boundaries which led to an increase in the fraction of high angle boundaries as compared with the respective base metals. These regions showed the least amount of residual strain and highest amount of recrystallized austenite grains. Due to the static recrystallization, the fraction of low degree of fit (Σ) coincident site lattice boundaries, especially Σ3 boundaries, was increased in the austenitic stainless steel heat affected zone, while the formation of subgrains in the ferrite phase increased the content of < 5° low angle boundaries at that of the super duplex stainless steel. - Graphical abstract: Display Omitted - Highlights: • Extensive grain growth in the HAZ of austenitic stainless steel was observed. • Intensification of < 100 > orientated grains was observed adjacent to both fusion lines. • Annealing twins with Σ3 CSL boundaries were formed in the austenite of both HAZ. • Cub-on-cube OR was observed between austenite and ferrite in the weld

  7. Synthesis, characterization and quantitative analysis of porous metal microstructures: Application to microporous copper produced by solid state foaming

    Directory of Open Access Journals (Sweden)

    Mark A. Atwater

    2016-05-01

    Full Text Available Porous metals can be created through a wide variety of processing techniques, and the pore morphology resulting from these processes is equally diverse. The structural and functional properties of metal foams are directly dependent on the size, shape, interconnectedness and volume fraction of pores, so accurately quantifying the pore characteristics is of great importance. Methods for analyzing porous materials are presented here and applied to a copper-based metallic foam generated through solid state foaming via oxide reduction and expansion. This process results in large voids (10s of microns between sintered particles and small pores (10 microns to less than 50 nm within particles. Optical and electron microscopy were used to image the porosity over this wide range, and the pore characteristics were quantified using image segmentation and statistical analysis. Two-dimensional pore analysis was performed using the Chan-Vese method, and two-point correlation and lineal path functions were used to assess three-dimensional reconstructions from FIB tomography. Two-dimensional analysis reveals distinct size and morphological differences in porosity between particles and within them. Three-dimensional analysis adds further information on the high level interconnectedness of the porosity and irregular shape it takes, forming tortuous pathways rather than spherical cells. Mechanical polishing and optical microscopy allow large areas to be created and analyzed quickly, but methods such as focused ion beam (FIB sectioning can provide additional insight about microstructural features. In particular, after FIB milling is used to create a flat surface, that surface can be analyzed for structural and compositional information.

  8. The growth and characterization of group III-nitride transistor devices grown by metalorganic chemical vapor deposition

    Science.gov (United States)

    Wong, Michael Ming

    The InAlGaN, or III-nitride, material system has received much interest from the research community. A direct wide bandgap semiconductor, GaN offers a high breakdown field (>3 x 106 V/cm) due to its large bandgap energy of 3.4 eV, high electron saturation velocity (1.5 x 10 7 cm/s, predicted peak up to 2.7 x 107 cm/s), good thermal conductivity (≥1.7 W/cm K), and reasonable mobility (800 cm 2/V s). In an AlGaN/GaN heterostructure, the formation of a two-dimensional electron gas (2DEG) leads to a higher electron mobility (2000 cm2/V s) and a high sheet density (1--5 x 1013 cm -2). This makes transistors based on the III-nitride material system ideal for high-temperature, high-power, and high-frequency applications. Two such transistors include the heterojunction field-effect transistor (HFET) and bipolar junction transistor (BJT), which includes the heterojunction bipolar transistor (HBT). Both HFETs and HBTs were studied, and the epitaxial heterostructures were grown by the metalorganic chemical vapor deposition (MOCVD) technique. The MOCVD process and system are described, along with the growth details. As material characterization is important for the optimization of growth, several of the techniques used are discussed. An extensive study to improve the performance of AlGaN/GaN HFETs is detailed. Through the use of a delta-doped, binary barrier novel device structure, the highest reported maximum drain current and transconductance is reported: IDSmax = 1.82 A/mm and gm = 331 mS/mm. The device also exhibits excellent RF characteristics. HBTs based on the III-nitride material system face a more difficult challenge associated with p-type material. Development of HBTs is still in the early stages, although there are reports of working devices. The gain is still below its potential, but many of the issues have been identified. Two novel structures are reported for the first time, a GaN/InGaN/GaN pnp HBT and a AlGaN/GaN npn graded-base and collector-up HBT. The

  9. Gold(III) bis-thiosemicarbazonato complexes: synthesis, characterization, radiochemistry and X-ray crystal structure analysis.

    Science.gov (United States)

    Bottenus, Brienne N; Kan, Para; Jenkins, Tyler; Ballard, Beau; Rold, Tammy L; Barnes, Charles; Cutler, Cathy; Hoffman, Timothy J; Green, Mark A; Jurisson, Silvia S

    2010-01-01

    A variety of (bis)thiosemicarbazone-based ligand systems have been investigated as chelating agents for Au(III) complexes with potential radiotherapeutic applications. Ligand systems containing an ethyl, propyl or butyl backbone between the two imine N donors have been synthesized to evaluate chelate ring size effects on the resultant Au(III) complex stability at the macroscopic and radiotracer levels. The Au(III) complexes were synthesized and characterized by NMR, electrospray ionization mass spectra, elemental analysis and X-ray crystallography. The (198)Au complexes were evaluated in vitro at the tracer level for stability in phosphate-buffered saline at pH 7.4 and 37 degrees C. One of these complexes [(198)Au(3,4-HxTSE)] showed high in vitro stability and was further evaluated in vivo in normal mice. [Au(ATSM)]AuCl(4).2CH(3)OH, (ATSM=diacetyl-bis(N(4)-methylthiosemicarbazone)) H(14)C(8)N(6)O(2)S(2)Cl(4)Au(2).2CH(3)OH, crystallized from methanol in the monoclinic space group P21/n with a=14.7293(13) A, b=7.7432(7) A, c=20.4363(18) A, beta=100.140(2) degrees, V=2294.4 (4) A(3), Z=4; [Au(3,4-HxTSE)]Cl.CH(3)CH(2)OH/AuCl(2), (3,4-HxTSE=3,4-hexanedione-bis(N(4)-ethylthiosemicarbazone)) H(26)C(13.6)N(6)O(0.8)S(2)Cl(1.2)Au(1.2), crystallized from ethanol in the monoclinic space group P21/c with a=10.1990(10) A, b=13.8833(14) A, c=15.1752(15) A, beta=99.353(2) degrees , V=2120.2 (4) A(3), Z=4. These studies revealed poor stability of the [(198)Au][Au(3,4-HxTSE)](+) complex; however, crystal structure data suggest potential alterations to the ligand backbone may increase stability. Copyright 2010 Elsevier Inc. All rights reserved.

  10. Stabilization of high-valence ruthenium with silicotungstate ligands: preparation, structural characterization, and redox studies of ruthenium(III)-substituted α-Keggin-type silicotungstates with pyridine ligands, [SiW11O39Ru(III)(Py)]5-.

    Science.gov (United States)

    Sadakane, Masahiro; Moroi, Sachie; Iimuro, Yoshifumi; Izarova, Natalya; Kortz, Ulrich; Hayakawa, Shinjiro; Kato, Kazuo; Ogo, Shuhei; Ide, Yusuke; Ueda, Wataru; Sano, Tsuneji

    2012-06-01

    Ruthenium(III)-substituted α-Keggin-type silicotungstates with pyridine-based ligands, [SiW(11)O(39)Ru(III)(Py)](5-), (Py: pyridine (1), 4-pyridine-carboxylic acid (2), 4,4'-bipyridine (3), 4-pyridine-acetamide (4), and 4-pyridine-methanol (5)) were prepared by reacting [SiW(11)O(39)Ru(III)(H(2)O)](5-) with the pyridine derivatives in water at 80 °C and then isolated as their hydrated cesium salts. These compounds were characterized using cyclic voltammetry (CV), UV/Vis, IR, and (1)H NMR spectroscopy, elemental analysis, titration, and X-ray absorption near-edge structure (XANES) analysis (Ru K-edge and L(3)-edge). Single-crystal X-ray analysis of compounds 2, 3, and 4 revealed that Ru(III) was incorporated in the α-Keggin framework and was coordinated by pyridine derivatives through a Ru-N bond. In the solid state, compounds 2 and 3 formed a dimer through π-π interaction of the pyridine moieties, whereas they existed as monomers in solution. CV indicated that the incorporated Ru(III)-Py was reversibly oxidized into the Ru(IV)-Py derivative and reduced into the Ru(II)-Py derivative. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. Direct genetic characterization of Toxoplasma gondii from clinical samples from Denmark: not only genotypes II and III.

    Science.gov (United States)

    Jokelainen, P; Murat, J-B; Nielsen, H V

    2018-03-01

    Genetic variation within Toxoplasma gondii can have both clinical and epidemiological significance, while the genotypes circulating in many parts of the world, including the Nordic country Denmark, are still unknown. We genetically characterized T. gondii strains that had been detected in human clinical samples in Denmark in 2011-2016. Samples that had tested positive for T. gondii DNA and had a quantification cycle value <33 were included in this study and subjected to direct genetic characterization of T. gondii based on length-polymorphism of 15 microsatellite markers. A total of 23 DNA samples from 22 individual patients were analyzed. The results were consistent with genotype II with 15/15 markers amplified from seven samples from the central nervous system (CNS) including two samples from one patient, four ocular samples, and one unspecified sample; with genotype III with 15/15 markers amplified from two ocular samples; with genotype Africa 1 with 15/15 markers amplified from one amniotic fluid sample and from one CNS-sample; with atypical genotype with 15/15 markers amplified from one CNS-sample and with 11/15 markers amplified from one CNS-sample; and with HG12-like genotype with 9/15 markers amplified from one CNS-sample. Genotype II, which is endemic in Europe, was predominant, but more than a third of the successfully genotyped strains were non-type-II. The possibility that clinical toxoplasmosis is caused by a strain that is not considered endemic to the region is definitely not negligible.

  12. Characterization of the N-terminal domain of BteA: a Bordetella type III secreted cytotoxic effector.

    Directory of Open Access Journals (Sweden)

    Chen Guttman

    Full Text Available BteA, a 69-kDa cytotoxic protein, is a type III secretion system (T3SS effector in the classical Bordetella, the etiological agents of pertussis and related mammalian respiratory diseases. Currently there is limited information regarding the structure of BteA or its subdomains, and no insight as to the identity of its eukaryotic partners(s and their modes of interaction with BteA. The mechanisms that lead to BteA dependent cell death also remain elusive. The N-terminal domain of BteA is multifunctional, acting as a docking platform for its cognate chaperone (BtcA in the bacterium, and targeting the protein to lipid raft microdomains within the eukaryotic host cell. In this study we describe the biochemical and biophysical characteristics of this domain (BteA287 and determine its architecture. We characterize BteA287 as being a soluble and highly stable domain which is rich in alpha helical content. Nuclear magnetic resonance (NMR experiments combined with size exclusion and analytical ultracentrifugation measurements confirm these observations and reveal BteA287 to be monomeric in nature with a tendency to oligomerize at concentrations above 200 µM. Furthermore, diffusion-NMR demonstrated that the first 31 residues of BteA287 are responsible for the apparent aggregation behavior of BteA287. Light scattering analyses and small angle X-ray scattering experiments reveal a prolate ellipsoidal bi-pyramidal dumb-bell shape. Thus, our biophysical characterization is a first step towards structure determination of the BteA N-terminal domain.

  13. Synthesis and Characterization of Chloridobis(dimethylglyoximato4-(2-ferrocenylvinylpyridinecobalt(III: A New Heterobinuclear Cobaloxime

    Directory of Open Access Journals (Sweden)

    Sebastián Pizarro

    2016-01-01

    Full Text Available The synthesis of a new heterobinuclear cobaloxime with 4-(2-ferrocenylvinylpyridine, fcvpy, is reported. The complex [CoCl(dmgH2(fcvpy], where dmgH2 is dimethylglyoxime and dmgH is dimethylglyoximato, has been characterized by 1H-NMR, UV-Vis, cyclic voltammetry, and elemental analysis. The cyclic voltammogram of this complex shows a fc/fc+ reversible wave at +0.58 V versus Ag/AgCl, one irreversible wave, Epc = −0.54 V versus Ag/AgCl, assigned to the reduction of Co(III to Co(II, and two quasireversible processes at −1.02 V and −1.10 V versus Ag/AgCl associated with the reduction of Co(II. The complex showed ferrocene-ligand charge transfer bands at 334 nm and 505 nm. TDDFT/B3LYP/6-31G(d calculations support this assignation.

  14. LaSrMnO{sub 3} thin films on YSZ/YSZ - NiO by the spin coating method: synthesis and microstructural characterization

    Energy Technology Data Exchange (ETDEWEB)

    Garcia, Laurenia Martins Pereira; Souza, Graziele Lopes de [Universidade Federal do Rio Grande do Norte (NUPEG/UFRN), Natal, RN (Brazil). Nucleo de Pesquisa em Petroleo e Gas], Email: lauengmat@hotmail.com; Macedo, Daniel Araujo de; Cela, Beatriz; Paskocimas, Carlos Alberto; Nascimento, Rubens Maribondo do [Universidade Federal do Rio Grande do Norte (PPGCEM/UFRN), Natal, RN (Brazil). Programa de Pos Graduacao em Ciencia e Engenharia de Materiais; Cesario, Moises Romolos [Universidade Federal do Rio Grande do Norte (PPGQ/UFRN), Natal, RN (Brazil). Programa de Pos Graduacao em Quimica

    2010-07-01

    Fuel cells are devices which work by electrochemical mechanism directly converting the chemical energy, by fuel the oxidizing, in electric energy. The Solid Oxide Fuel Cell - SOFC consist an anode, an electrolyte and one cathode made with ceramic materials. The most widely known functional materials used in SOFC are Yttria-stabilized zirconia electrolyte (YSZ), composite anode of YSZ-Ni O and strontium-doped lanthanum manganite cathode (La{sub 1-x}Sr{sub x}MnO{sub 3} - LGSM). In this work the thin films of cathode LSM were deposited by spin coating in a half cell YSZ/YSZ - Ni O. The polymeric resin of 22% strontium-doped lanthanum manganite (LSM 22) was attained by the polymeric precursor method. This resin was directly used for the deposition process. The deposition of 2 or 4 layers occurred by spin coating method with the following conditions: 500 rpm during 15 s and 300 rpm during 40 s. Each layer was thermally treated at 500 deg C for 2 h and heating rate equal to 1 deg C/min. The multi layers were sintered at 1000 deg C for 2 h, heating rate of 3 deg C/min and characterized by X-ray diffraction (XRD) and scanning electronic microscopy (SEM). The LSM 22 thin films presented microstructure with thin particles and thickness of 1 {mu}m. The surface cracks' quantity and size reduction tendency was observed with the increase of the layers deposition number. (author)

  15. Production, microstructural and mechanical characterization of spray formed Al-6 wt.% Fe alloy and pre-mixed Al-6 wt.% Fe/SiC{sub p} composite

    Energy Technology Data Exchange (ETDEWEB)

    Zambon, A.; Badan, B.; Maddalena, A

    2004-07-15

    Different batches of Al-6 wt.% Fe and of pre-composite Al-6 wt.% Fe/SiC powders were produced, via melting of aluminum followed by iron addition in the induction furnace of a gas atomizing unit, eventually adding in situ a suitable amount of SiC particulate. The inclusion of the reinforcing particles in the melt was enhanced by means of stirring under an argon shielding atmosphere. Gas atomization via sonic close-coupled discrete jet nozzles was thereafter performed, and a part of the spray cone was intercepted by a still substrate. The microstructural characterization of both the pre-composite powder and of the spray deposited samples was carried out by microscopy, image analysis and X-ray diffraction. The high viscosity of the matrix allowed to achieve a maximum volumetric fraction of reinforcement of around 10%. By means of X-ray stress analysis the residual stresses in the spray formed specimens were determined, and resulted to be compressive, and higher in the composite material. The elastic properties of the spray formed samples were determined by the flexural resonance test, carried out on prismatic samples cut from the spray formed samples, while their transverse strengths were determined by three points bend test.

  16. Current and future industrial energy service characterizations. Volume III. Energy data on 15 selected states' manufacturing subsector

    Energy Technology Data Exchange (ETDEWEB)

    Krawiec, F.; Thomas, T.; Jackson, F.; Limaye, D.R.; Isser, S.; Karnofsky, K.; Davis, T.D.

    1980-11-01

    An examination is made of the current and future energy demands, and uses, and cost to characterize typical applications and resulting services in the US and industrial sectors of 15 selected states. Volume III presents tables containing data on selected states' manufacturing subsector energy consumption, functional uses, and cost in 1974 and 1976. Alabama, California, Illinois, Indiana, Louisiana, Michigan, Missouri, New Jersey, New York, Ohio, Oregon, Pennsylvania, Texas, West Virginia, and Wisconsin were chosen as having the greatest potential for replacing conventional fuel with solar energy. Basic data on the quantities, cost, and types of fuel and electric energy purchased by industr for heat and power were obtained from the 1974 and 1976 Annual Survey of Manufacturers. The specific indutrial energy servic cracteristics developed for each selected state include. 1974 and 1976 manufacturing subsector fuels and electricity consumption by 2-, 3-, and 4-digit SIC and primary fuel (quantity and relative share); 1974 and 1976 manufacturing subsector fuel consumption by 2-, 3-, and 4-digit SIC and primary fuel (quantity and relative share); 1974 and 1976 manufacturing subsector average cost of purchsed fuels and electricity per million Btu by 2-, 3-, and 4-digit SIC and primary fuel (in 1976 dollars); 1974 and 1976 manufacturing subsector fuels and electric energy intensity by 2-, 3-, and 4-digit SIC and primary fuel (in 1976 dollars); manufacturing subsector average annual growth rates of (1) fuels and electricity consumption, (2) fuels and electric energy intensity, and (3) average cost of purchased fuels and electricity (1974 to 1976). Data are compiled on purchased fuels, distillate fuel oil, residual ful oil, coal, coal, and breeze, and natural gas. (MCW)

  17. Mono- and dinuclear manganese(III) complexes showing efficient catechol oxidase activity: syntheses, characterization and spectroscopic studies.

    Science.gov (United States)

    Banu, Kazi Sabnam; Chattopadhyay, Tanmay; Banerjee, Arpita; Mukherjee, Madhuparna; Bhattacharya, Santanu; Patra, Goutam Kumar; Zangrando, Ennio; Das, Debasis

    2009-10-28

    Four side-off compartmental ligands L1-L4 [L1 = N,N'-ethylenebis(3-formyl-5-methyl-salicylaldimine), L2 = N,N'-1-methylethylenebis(3-formyl-5-methylsalicylaldimine), L3 = N,N'-1,1-dimethylethylenebis(3-formyl-5-methylsalicylaldimine) and L4= N,N'-cyclohexenebis(3-formyl-5-methylsalicylaldimine)] having two binding sites, N2O2 and O4, have been chosen to synthesize mononuclear and dinuclear manganese(III) complexes with the aim to study their catecholase activity using 3,5-di-tert-butylcatechol (3,5-DTBC) as substrate in the presence of molecular oxygen. In all cases only mononuclear manganese complexes (1-4) were obtained, with manganese coordination taking place at the N2O2 binding site only, irrespective of the amount of manganese salt used. All these complexes have been characterized by routine physico-chemical techniques. Complex MnL2Cl.4H2O (2) has further been structurally characterized by X-ray single crystal structure analysis. Four dinuclear manganese complexes, 5-8, were obtained after condensing the two pending formyl groups on each ligand (L1-L4) with aniline followed by reaction with MnCl2 to put the second Mn atom onto another N2O2 site. The catalytic activity of all complexes 1-8 has been investigated following the oxidation of 3,5-di-tert-butylcatechol (3,5-DTBC) to 3,5-di-tert-butylbenzoquinone (3,5-DTBQ) with molecular oxygen in two different solvents, methanol and acetonitrile. The study reveals that the catalytic activity is influenced by the solvent and to a significant extent by the backbone of the diamine and the behavior seems to be related mainly to steric rather than electronic factors. Experimental data suggest that a correlation, the lower the E(1/2) value the higher the catalytic activity, can be drawn between E(1/2) and Vmax of the complexes in a particular solvent. The EPR measurements suggest that the catalytic property of the complexes is related to the metal center(s) participation rather than to a radical mechanism.

  18. An analysis of Mn-Zn ferrite microstructure by impedance spectroscopy, scanning transmission electron microscopy and energy dispersion spectrometry characterizations

    Science.gov (United States)

    Loyau, V.; Wang, G.-Y.; Bue, M. Lo; Mazaleyrat, F.

    2012-03-01

    AC (alternative current) resistivity measurement results on Mn-Zn sintered ferrite were analyzed in the 0.1-500 MHz range. From electrical point of view, the material could be represented by an equivalent circuit of parallel resistance-capacitance cells connected in series corresponding to the contributions from bulk grains in one hand, and grain boundary layers in the other hand. The experimental resistivity curves were fitted with the model. The as obtained parameters give information on dielectric properties and conductivity of both bulk grains and boundary layers. For the studied material, it appears that the resistivity at low frequencies is increased 27 times due to the boundary layers effects. Scanning transmission electron microscopy and energy dispersion spectrometry characterization where performed in order to detect impurities at a grain boundary layer which can explain those wide differences between bulk grains and boundary layers electrical properties. It appears that the two components have close chemical compositions, but some calcium impurities segregate at the boundary which increases dramatically the resistivity of these layers. Furthermore, the bulk grains show relative permittivity around 350 at low frequency which is much smaller than the one measured for the whole material which is in the 50,000-100,000 range. This giant-dielectric behavior can be explained by an internal barrier layer at the grain boundaries. At last, the components of classical eddy current losses including losses due to ohmic effects and (true) dielectric losses on both bulk grain and boundary layers are distinguished.

  19. Characterization of textural, rheological, thermal, microstructural, and water mobility in wheat flour dough and bread affected by trehalose.

    Science.gov (United States)

    Peng, Bo; Li, Youqian; Ding, Shiyong; Yang, Jun

    2017-10-15

    The study aims to elucidate the effects of trehalose on the mechanical, thermal, and rheological properties of wheat flour dough and water distribution in bread. Texture profile analysis, DSC, farinograph, extensograph, and frequency sweep were applied in dough. The results from SEM revealed that the gluten film became less notable with the presence of trehalose. The kinetics of staling process, low-field 1 H NMR, and water-binding capacity were employed to characterize physicochemical properties of bread. Trehalose decreased the staling rate constant k, indicating an inhibitory effect on firming process in bread. Trehalose had the ability to retain water by hindering the interaction among water molecules, gluten and starch, thus relatively increasing the immobility of the part of water represented by T 22 in low-field 1 H NMR tests. Trehalose restricted water mobilization during storage, resulting in a better water-holding capacity. Our findings reveal that trehalose could be an improver in dough and bread-making performance, as well as an antistaling agent in bread. Copyright © 2017 Elsevier Ltd. All rights reserved.

  20. Characterization and Properties of Activated Carbon Prepared from Tamarind Seeds by KOH Activation for Fe(III) Adsorption from Aqueous Solution.

    Science.gov (United States)

    Mopoung, Sumrit; Moonsri, Phansiri; Palas, Wanwimon; Khumpai, Sataporn

    2015-01-01

    This research studies the characterization of activated carbon from tamarind seed with KOH activation. The effects of 0.5 : 1-1.5 : 1 KOH : tamarind seed charcoal ratios and 500-700°C activation temperatures were studied. FTIR, SEM-EDS, XRD, and BET were used to characterize tamarind seed and the activated carbon prepared from them. Proximate analysis, percent yield, iodine number, methylene blue number, and preliminary test of Fe(III) adsorption were also studied. Fe(III) adsorption was carried out by 30 mL column with 5-20 ppm Fe(III) initial concentrations. The percent yield of activated carbon prepared from tamarind seed with KOH activation decreased with increasing activation temperature and impregnation ratios, which were in the range from 54.09 to 82.03 wt%. The surface functional groups of activated carbon are O-H, C=O, C-O, -CO3, C-H, and Si-H. The XRD result showed high crystallinity coming from a potassium compound in the activated carbon. The main elements found in the activated carbon by EDS are C, O, Si, and K. The results of iodine and methylene blue adsorption indicate that the pore size of the activated carbon is mostly in the range of mesopore and macropore. The average BET pore size and BET surface area of activated carbon are 67.9764 Å and 2.7167 m(2)/g, respectively. Finally, the tamarind seed based activated carbon produced with 500°C activation temperature and 1.0 : 1 KOH : tamarind seed charcoal ratio was used for Fe(III) adsorption test. It was shown that Fe(III) was adsorbed in alkaline conditions and adsorption increased with increasing Fe(III) initial concentration from 5 to 20 ppm with capacity adsorption of 0.0069-0.019 mg/g.

  1. Synthesis and characterization of anti-bisFe(III) porphyrins, syn-bisFe(III)-mu-oxo porphyrin, and syn-bisFe(III)-mu-oxo porphyrin cation radical.

    Science.gov (United States)

    Ghosh, Sudip Kumar; Patra, Ranjan; Rath, Sankar Prasad

    2010-04-05

    BisFe(III) porphyrins bridged by a highly flexible ethane linker are reported in which the bisporphyrin platform "opens" and "closes" its binding pockets leading to facile syn-anti conformational switching with very high vertical flexibility in a single molecular framework. With axial ligand X (X: Cl, Br, I, ClO(4)), the anti-forms of the molecule are stabilized. The X-ray structure of anti bis perchloratoFe(III)porphyrin is reported, and the molecule is found to be high-spin in nature. In sharp contrast, all other Fe(III) porphyrins with ClO(4) as axial ligands are in an either intermediate or admixed spin state. The very strong Fe-OClO(3) bond and relatively weaker Fe-N(p) bonds are responsible for the high-spin nature of the molecule. Upon treatment with base, bis Fe(III)-mu-oxo porphyrin is generated in which the Fe-O-Fe unit is remarkably bent (with a 147.9(1) degrees angle) and two porphyrin rings in a molecule are so close that at least six carbon atoms from each of the porphyrin macrocycles are driven to be essentially closer than the van der Waals contact distance. Upon manipulating the acidity/basicity of the solution, the facile syn-anti conformational switching takes place that is also reversible in nature. The complex catalyzes the rapid photoinduced oxygenation of phosphites under mild condition using aerial O(2). Electrochemical data reveals that bis Fe(III)-mu-oxo porphyrin undergoes four one electron oxidations and one electron reduction. However, oxidations become easier in syn Fe(III)-mu-oxo dimer rather than the anti-form of the molecule (with axial ligand X). The presence of two porphyrin macrocycles within a short distance in the syn form makes the porphyrin core highly nonplanar and more electron rich, and that might be responsible for easier oxidations compared to [Fe(OEP)](2)O. Oxidations of the mu-oxo complex are performed using both chemical and electrochemical methods. The addition of 1.00 mol equiv of iodine-silver perchlorate generates

  2. Preparation and characterization of Fe(III)-loaded iminodiacetic acid modified GMA grafted nonwoven fabric adsorbent for anion adsorption

    Science.gov (United States)

    Kavaklı, Pınar Akkaş; Kavaklı, Cengiz; Güven, Olgun

    2014-01-01

    An Fe(III)-loaded chelating fabric with iminodiacetic acid (IDA) functional groups was prepared by radiation induced graft polymerization of an epoxy group containing monomer, glycidyl methacrylate, onto a nonwoven fabric made of polypropylene coated by polyethylene (PE/PP) and subsequent Fe(III) loading. Grafting conditions were optimized, and GMA grafted polymer was modified with iminodiacetic acid in isopropyl alcohol/water at 80 °C. In order to prepare the polymeric ligand exchanger (PLE) for the removal of phosphate, IDA fabrics were loaded with Fe(III) ions. Fe(III) loading capacity of IDA fabric was determined to be 2.83 mmol Fe(III)/g of polymer. For removal of phosphate anion, adsorption experiments were performed in batch mode at different pH (2-9) and phosphate concentrations. It was found that phosphate adsorption by the Fe(III)-loaded IDA fabric is maximum at pH 2.00. The effect of initial concentration of phosphate on the adsorption behaviour of Fe(III)-loaded IDA nonwoven fabric was determined at low phosphate concentrations (0.5-25 ppm) and at high phosphate concentrations (50-1000 ppm).

  3. Microstructural, chemical and textural characterization of ZnO nanorods synthesized by aerosol assisted chemical vapor deposition

    Energy Technology Data Exchange (ETDEWEB)

    Sáenz-Trevizo, A.; Amézaga-Madrid, P.; Fuentes-Cobas, L.; Pizá-Ruiz, P.; Antúnez-Flores, W.; Ornelas-Gutiérrez, C. [Centro de Investigación en Materiales Avanzados, S.C., Chihuahua, Chihuahua 31109 (Mexico); Pérez-García, S.A. [Centro de Investigación en Materiales Avanzados, S.C., Unidad Monterrey, Apodaca, Nuevo León 66600 (Mexico); Miki-Yoshida, M., E-mail: mario.miki@cimav.edu.mx [Centro de Investigación en Materiales Avanzados, S.C., Chihuahua, Chihuahua 31109 (Mexico)

    2014-12-15

    ZnO nanorods were synthesized by aerosol assisted chemical vapor deposition onto TiO{sub 2} covered borosilicate glass substrates. Deposition parameters were optimized and kept constant. Solely the effect of different nozzle velocities on the growth of ZnO nanorods was evaluated in order to develop a dense and uniform structure. The crystalline structure was characterized by conventional X-ray diffraction in grazing incidence and Bragg–Brentano configurations. In addition, two-dimensional grazing incidence synchrotron radiation diffraction was employed to determine the preferred growth direction of the nanorods. Morphology and growth characteristics analyzed by electron microscopy were correlated with diffraction outcomes. Chemical composition was established by X-ray photoelectron spectroscopy. X-ray diffraction results and X-ray photoelectron spectroscopy showed the presence of wurtzite ZnO and anatase TiO{sub 2} phases. Morphological changes noticed when the deposition velocity was lowered to the minimum, indicated the formation of relatively vertically oriented nanorods evenly distributed onto the TiO{sub 2} buffer film. By coupling two-dimensional X-ray diffraction and computational modeling with ANAELU it was proved that a successful texture determination was achieved and confirmed by scanning electron microscopy analysis. Texture analysis led to the conclusion of a preferred growth direction in [001] having a distribution width Ω = 20° ± 2°. - Highlights: • Uniform and pure single-crystal ZnO nanorods were obtained by AACVD technique. • Longitudinal and transversal axis parallel to the [001] and [110] directions, respectively. • Texture was determined by 2D synchrotron diffraction and electron microscopy analysis. • Nanorods have its [001] direction distributed close to the normal of the substrate. • Angular spread about the preferred orientation is 20° ± 2°.

  4. Titanium composite conversion coating formation on CRS In the presence of Mo and Ni ions: Electrochemical and microstructure characterizations

    Energy Technology Data Exchange (ETDEWEB)

    Eivaz Mohammadloo, H.; Sarabi, A.A., E-mail: Sarabi@aut.ac.ir

    2016-11-30

    Highlights: • Eco-friendly protective thin films for covering the CRS substrates were presented. • Comprehensive analyses were performed to evaluate the surface characteristics. • Promising approach for the surface modification of CRS substrate by Ti-based conversion coatings. - Abstract: There have been an increasing interest in finding a replacement for the chromating process due to environmental and health concerns. Hence, in this study Chrome-free chemical conversion coatings were deposited on the surface of cold-rolled steel (CRS) on the basis of Titanium (TiCC), Titanium-Nickel (TiNiCC) and titanium-molybdate (TiMoCC) based conversion coating solutions. The surface characterization was performed by field emission scanning electron microscope (FESEM), X-ray photoelectron spectroscopy (XPS), atomic force microscopy (AFM) and contact angle measuring device. Also, the corrosion behavior was assessed by the means of potentiodynamic polarization and electrochemical impedance spectroscopy (EIS) measurements. FESEM and AFM study show that the TiNiCC is denser and more uniform than that TiCC and TiMoCC since, TiMoCC conversion coating presents network feature, and there were abundant micro-cracks on the surface of the coating. XPS results confirmed the precipitation of Ti and Ni oxide/hydroxide, Mn dioxide/trioxide on the surface of different Ti-based conversion coatings. Electrochemical results revealed that all Ti-based conversion coatings have better anti-corrosion properties than bare CRS. Moreover, TiNiCC treatment inhibited the corrosion of CRS to a significant degree (polarization resistance (R{sub p}) = 5510 Ω cm{sup 2}) in comparison with TiCC (R{sub p} = 2705 Ω cm{sup 2}) and TiMoCC (R{sub p} = 805 Ω cm{sup 2}).

  5. Microstructural processes in irradiated materials

    Science.gov (United States)

    Byun, Thak Sang; Morgan, Dane; Jiao, Zhijie; Almer, Jonathan; Brown, Donald

    2016-04-01

    These proceedings contain the papers presented at two symposia, the Microstructural Processes in Irradiated Materials (MPIM) and Characterization of Nuclear Reactor Materials and Components with Neutron and Synchrotron Radiation, held in the TMS 2015, 144th Annual Meeting & Exhibition at Walt Disney World, Orlando, Florida, USA on March 15-19, 2015.

  6. High-field (high-frequency) EPR spectroscopy and structural characterization of a novel manganese(III) corrole

    OpenAIRE

    Bendix, Jesper; Gray, Harry B.; Golubkov, Galina; Gross, Zeev

    2000-01-01

    The X-ray structure, magnetic susceptibility, and high-field (high-frequency) EPR spectrum of manganese 5,10,15-tris(pentafluorophenyl) corrole unambiguously establish that the complex contains an isolated, slightly rhombic, manganese(III) center.

  7. Synthesis and characterization of Eu(III)-based coordination complexes of modified D-glucosamine and poly(N-isopropylacrylamide)

    Science.gov (United States)

    Cui, Guihua; Zhao, Dehai; Lv, Peng; Gao, Zhengguo; Chen, Shuiying; Qiu, Nannan; Satoh, Toshifumi; Kakuchi, Toyoji; Duan, Qian

    2017-10-01

    A series of novel fluorescent complexes was formed by chelation of the thermosensitive polymers with europium(III) ions. The polymers was synthesized via atom transfer radical polymerization (ATRP), which composed of poly(N-isopropyl acrylamide) (PNIPAM) and 2-amino-2-deoxy-D-glucopyranose(D-glucosamine, GA). The aqueous solutions of the polymers and its Eu(III) complexes exhibited a lower critical solution temperatures (LCSTs), and which were approximately equal to body temperature. The maximum emission intensity of the complexes at 613 nm was enhanced by a factor of approximately 10 relative to that of the corresponding Eu(III) chloride. Cell viability assays suggested that these thermosensitive polymers and Eu(III) complexes showed excellent biocompatibility in vitro.

  8. Synthesis and characterization of novel oxo-bridged, trinuclear mixed-metal complexes of Cr(III and Fe(III

    Directory of Open Access Journals (Sweden)

    HAMAN TAVAKKOLI

    2009-04-01

    Full Text Available Two new heterotrinuclear p-chlorobenzoates, [Fe2CrO(C7H4O2Cl6(py3]NO3 (1 and [Cr2FeO(C7H4O2Cl6(py3]NO3 (2 were prepared as nitrate salts and characterized by elemental analyses (CHN, spectroscopic (infrared, electronic studies and atomic absorption spectroscopy. These complexes are a new type of oxo-bridged mixed-metal complex in which the carboxylate ligand is p-chlorobenzoic acid. Bridging coordination modes for the carboxylates were indicated by the presence of nasym (M2M’O vibrations in the infrared spectra.

  9. Micro-structural characterization of the hydration products of bauxite-calcination-method red mud-coal gangue based cementitious materials.

    Science.gov (United States)

    Liu, Xiaoming; Zhang, Na; Yao, Yuan; Sun, Henghu; Feng, Huan

    2013-11-15

    In this research, the micro-structural characterization of the hydration products of red mud-coal gangue based cementitious materials has been investigated through SEM-EDS, (27)Al MAS NMR and (29)Si MAS NMR techniques, in which the used red mud was derived from the bauxite calcination method. The results show that the red mud-coal gangue based cementitious materials mainly form fibrous C-A-S-H gel, needle-shaped/rod-like AFt in the early hydration period. With increasing of the hydration period, densification of the pastes were promoted resulting in the development of strength. EDS analysis shows that with the Ca/Si of red mud-coal gangue based cementitious materials increases, the average Ca/Si and Ca/(Si+Al) atomic ratio of C-A-S-H gel increases, while the average Al/Si atomic ratio of C-A-S-H gel decreases. MAS NMR analysis reveals that Al in the hydration products of red mud-coal gangue based cementitious materials exists in the forms of Al(IV) and Al(VI), but mainly in the form of Al(VI). Increasing the Ca/Si ratio of raw material promotes the conversion of [AlO4] to [AlO6] and inhibits the combination between [AlO4] and [SiO4] to form C-A-S-H gel. Meanwhile, the polymerization degree of [SiO4] in the hydration products declines. Published by Elsevier B.V.

  10. Synthesis, characterization, and reactivity of a side-on manganese(iii)-peroxo complex bearing a pentadentate aminopyridine ligand.

    Science.gov (United States)

    Du, Junyi; Xu, Daqian; Zhang, Chunxi; Xia, Chungu; Wang, Yong; Sun, Wei

    2016-06-21

    A manganese(ii) complex has been prepared with a proline-derived pentadentate ligand (Pro3Py), and it can be converted to a peroxomanganese(iii) complex in the presence of H2O2 and triethylamine. The resulting peroxomanganese(iii) complex was well characterised by UV-vis, EPR and ESI-MS techniques, and the geometric structure was discussed based on DFT calculations.

  11. Characterization of Monomeric MnII/III/IV–Hydroxo Complexes from X- and Q-Band Dual Mode Electron Paramagnetic Resonance (EPR) Spectroscopy

    Science.gov (United States)

    Gupta, Rupal; Taguchi, Taketo; Borovik, A. S.; Hendrich, Michael P.

    2013-01-01

    Manganese–hydroxo species have been implicated in C–H bond activation performed by metalloenzymes, but the electronic properties of many of these intermediates are not well characterized. The present work presents a detailed characterization of three Mnn–OH complexes (where n = II, III, and IV) of the tris[(N′-tert-butylureaylato)-N-ethylene]aminato ([H3buea]3−) ligand using X- and Q-band dual mode electron paramagnetic resonance (EPR). Quantitative simulations for the [MnIIH3buea(OH)]2− complex demonstrated the ability to characterize similar MnII species commonly present in the resting states of manganese-containing enzymes. The spin states of the MnIII and MnIV complexes determined from EPR spectroscopy are S = 2 and 3/2, respectively, as expected for the C3 symmetry imposed by the [H3buea]3− ligand. Simulations of the spectra indicated the constant presence of two MnIV species in solutions of [MnIVH3buea(OH)] complex. The simulations of perpendicular- and parallel-mode EPR spectra allow determination of zero-field splitting and hyperfine parameters for all complexes. For the MnIII and MnIV complexes, density functional theory calculations are used to determine the isotropic Mn hyperfine values, to compare the excited electronic state energies, and to give theoretical estimates of the zero-field energy. PMID:24156406

  12. Characterization of monomeric Mn(II/III/IV)-hydroxo complexes from X- and Q-band dual mode electron paramagnetic resonance (EPR) spectroscopy.

    Science.gov (United States)

    Gupta, Rupal; Taguchi, Taketo; Borovik, A S; Hendrich, Michael P

    2013-11-04

    Manganese-hydroxo species have been implicated in C-H bond activation performed by metalloenzymes, but the electronic properties of many of these intermediates are not well characterized. The present work presents a detailed characterization of three Mn(n)-OH complexes (where n = II, III, and IV) of the tris[(N'-tert-butylureaylato)-N-ethylene]aminato ([H3buea](3-)) ligand using X- and Q-band dual mode electron paramagnetic resonance (EPR). Quantitative simulations for the [Mn(II)H3buea(OH)](2-) complex demonstrated the ability to characterize similar Mn(II) species commonly present in the resting states of manganese-containing enzymes. The spin states of the Mn(III) and Mn(IV) complexes determined from EPR spectroscopy are S = 2 and 3/2, respectively, as expected for the C3 symmetry imposed by the [H3buea](3-) ligand. Simulations of the spectra indicated the constant presence of two Mn(IV) species in solutions of [Mn(IV)H3buea(OH)] complex. The simulations of perpendicular- and parallel-mode EPR spectra allow determination of zero-field splitting and hyperfine parameters for all complexes. For the Mn(III) and Mn(IV) complexes, density functional theory calculations are used to determine the isotropic Mn hyperfine values, to compare the excited electronic state energies, and to give theoretical estimates of the zero-field energy.

  13. Characterization of Monomeric MnII/III/IV–Hydroxo Complexes from X- and Q-Band Dual Mode Electron Paramagnetic Resonance (EPR) Spectroscopy

    OpenAIRE

    Gupta, Rupal; Taguchi, Taketo; Borovik, A. S.; Hendrich, Michael P.

    2013-01-01

    Manganese–hydroxo species have been implicated in C–H bond activation performed by metalloenzymes, but the electronic properties of many of these intermediates are not well characterized. The present work presents a detailed characterization of three Mnn–OH complexes (where n = II, III, and IV) of the tris[(N′-tert-butylureaylato)-N-ethylene]aminato ([H3buea]3−) ligand using X- and Q-band dual mode electron paramagnetic resonance (EPR). Quantitative simulations for the [MnIIH3buea(OH)]2− comp...

  14. Application of Advanced Reservoir Characterization, Simulation, and Production Optimization Strategies to Maximize Recovery in Slope and Basin Clastic Reservoirs, West Texas (Delaware Basin), Class III

    Energy Technology Data Exchange (ETDEWEB)

    Dutton, Shirley P.; Flanders, William A.

    2001-11-04

    The objective of this Class III project was demonstrate that reservoir characterization and enhanced oil recovery (EOR) by CO2 flood can increase production from slope and basin clastic reservoirs in sandstones of the Delaware Mountain Group in the Delaware Basin of West Texas and New Mexico. Phase 1 of the project, reservoir characterization, focused on Geraldine Ford and East Ford fields, which are Delaware Mountain Group fields that produce from the upper Bell Canyon Formation (Ramsey sandstone). The demonstration phase of the project was a CO2 flood conducted in East Ford field, which is operated by Orla Petco, Inc., as the East Ford unit.

  15. Complexes of 4-chlorophenoxyacetates of Nd(III), Gd(III) and Ho(III)

    OpenAIRE

    Ferenc, W.; Bernat, M.; Sarzyński, J.; Głuchowska, H.

    2010-01-01

    The complexes of 4-chlorophenoxyacetates of Nd(III), Gd(III) and Ho(III) have been synthesized as polycrystalline hydrated solids, and characterized by elemental analysis, spectroscopy, magnetic studies and also by X-ray diffraction and thermogravimetric measurements. The analysed complexes have the following colours: violet for Nd(III), white for Gd(III) and cream for Ho(III) compounds. The carboxylate groups bind as bidentate chelating (Ho) or bridging ligands (Nd, Gd). On heating to 1173K ...

  16. Spectroscopic, structural characterizations and antioxidant capacity of the chromium (III) niacinamide compound as a diabetes mellitus drug model

    Science.gov (United States)

    Refat, Moamen S.; El-Megharbel, Samy M.; Hussien, M. A.; Hamza, Reham Z.; Al-Omar, Mohamed A.; Naglah, Ahmed M.; Afifi, Walid M.; Kobeasy, Mohamed I.

    2017-02-01

    New binuclear chromium (III) niacinamide compound with chemical formula [Cr2(Nic)(Cl)6(H2O)4]·H2O was obtained upon the reaction of chromium (III) chloride with niacinamide (Nic) in methanol solvent at 60 °C. The proposed structure was discussed with the help of microanalytical analyses, conductivity, spectroscopic (FT-IR and UV-vis.), magnetic calculations, thermogravimetric analyses (TG/TGA), and morphological studies (X-ray of solid powder and scan electron microscopy. The infrared spectrum of free niacinamide in comparison with its chromium (III) compound indicated that the chelation mode occurs via both nitrogen atoms of pyridine ring and primary -NH2 group. The efficiency of chromium (III) niacinamide compound in decreasing of glucose level of blood and HbA1c in case of diabetic rats was checked. The ameliorating gluconeogenic enzymes, lipid profile and antioxidant defense capacities are considered as an indicator of the efficiency of new chromium (III) compound as antidiabetic drug model.

  17. Spectroscopic, structural characterizations and antioxidant capacity of the chromium (III) niacinamide compound as a diabetes mellitus drug model.

    Science.gov (United States)

    Refat, Moamen S; El-Megharbel, Samy M; Hussien, M A; Hamza, Reham Z; Al-Omar, Mohamed A; Naglah, Ahmed M; Afifi, Walid M; Kobeasy, Mohamed I

    2017-02-15

    New binuclear chromium (III) niacinamide compound with chemical formula [Cr 2 (Nic)(Cl) 6 (H 2 O) 4 ]·H 2 O was obtained upon the reaction of chromium (III) chloride with niacinamide (Nic) in methanol solvent at 60°C. The proposed structure was discussed with the help of microanalytical analyses, conductivity, spectroscopic (FT-IR and UV-vis.), magnetic calculations, thermogravimetric analyses (TG/TGA), and morphological studies (X-ray of solid powder and scan electron microscopy. The infrared spectrum of free niacinamide in comparison with its chromium (III) compound indicated that the chelation mode occurs via both nitrogen atoms of pyridine ring and primary -NH 2 group. The efficiency of chromium (III) niacinamide compound in decreasing of glucose level of blood and HbA1c in case of diabetic rats was checked. The ameliorating gluconeogenic enzymes, lipid profile and antioxidant defense capacities are considered as an indicator of the efficiency of new chromium (III) compound as antidiabetic drug model. Copyright © 2016 Elsevier B.V. All rights reserved.

  18. Advances in X-ray Mapping for Characterization of Microstructures: Silicon Drift Detectors, Microcalorimeters, X-ray Spectrum Imaging, and Data Mining

    Science.gov (United States)

    Newbury, D. E.

    2006-05-01

    X-ray mapping, performed with the electron probe microanalyzer (EPMA) or scanning electron microscope/energy dispersive x-ray spectrometer (SEM/EDS), is one of the most popular modes of studying chemically heterogeneous microstructures [1]. Despite the maturity of the technique, now in its 50th anniversary year [2], recent remarkable advances in instrumentation and software will provide microanalysts with an even more effective and efficient microstructural characterization tool: (1) Increased x-ray mapping speed: The silicon drift detector (SDD) [3] is a new form of the familiar silicon EDS that uses the same detection physics but with a radically different design that outperforms the classic Si-EDS in nearly every way [4]: (1) the SDD operates requires only Peltier cooling to -20 oC to - 50 oC; (2) for a given detector active area, the SDD has superior resolution; (3) the SDD achieves the same resolution but with a peaking time that is 5 to 8 times faster; and (4) maximum output count rate (OCR) ranges from about 14 kHz at optimum resolution (134 eV at MnKa for a 50 mm2 area) to 500 kHz (217 eV). This OCR performance enables rapid x-ray mapping collection in the x-ray spectrum image (XSI) mode, in which a complete EDS spectrum (2048 10eV-channels) is captured at each pixel (e.g., 10 ms dwell with 1.3 ms overhead per pixel, or 185 seconds for a 128x128 pixel map). XSI collection captures all possible spectral information within the limits imposed by the spectrometer and the primary beam dose. (2) EDS with WDS resolution: The microcalorimeter EDS measures the temperature rise when a single x-ray photon is absorbed in a metal target [5]. Demonstrated resolution is 4.5 eV at Mn Ka for a broad energy range (0.2 - 10 keV) spectrometer and 2 eV (AlKa) for a low photon energy range (0.2 - 2.0 keV) version. The low energy spectrometer is sensitive to peak shape and position changes associated with chemical bonding, opening the possibility of EDS chemical-state mapping. (3

  19. Characterization of nineteen antimony(III) complexes as potent inhibitors of photosystem II, carbonic anhydrase, and glutathione reductase.

    Science.gov (United States)

    Karacan, Mehmet Sayım; Rodionova, Margarita V; Tunç, Turgay; Venedik, Kübra Begüm; Mamaş, Serhat; Shitov, Alexandr V; Zharmukhamedov, Sergei K; Klimov, Vyacheslav V; Karacan, Nurcan; Allakhverdiev, Suleyman I

    2016-12-01

    Nineteen antimony(III) complexes were obtained and examined as possible herbicides. Six of these were synthesized for the first time, and their structures were identified using elemental analyses, (1)H-NMR, (13)C-NMR, FTIR, LCMS, magnetic susceptibility, and conductivity measurement techniques. For the nineteen examined antimony(III) complexes their most-stable forms were determined by DFT/B3LYP/LanL2DZ calculation method. These compounds were examined for effects on photosynthetic electron transfer and carbonic anhydrase activity of photosystem II, and glutathione reductase from chloroplast as well were investigated. Our results indicated that all antimony(III) complexes inhibited glutathione reductase activity of chloroplast. A number of these also exhibited good inhibitory efficiency of the photosynthetic and carbonic anhydrase activity of Photosystem II.

  20. Rational development and characterization of humanized anti–EGFR variant III chimeric antigen receptor T cells for glioblastoma

    Science.gov (United States)

    Johnson, Laura A.; Scholler, John; Ohkuri, Takayuki; Kosaka, Akemi; Patel, Prachi R.; McGettigan, Shannon E.; Nace, Arben K.; Dentchev, Tzvete; Thekkat, Pramod; Loew, Andreas; Boesteanu, Alina C.; Cogdill, Alexandria P.; Chen, Taylor; Fraietta, Joseph A.; Kloss, Christopher C.; Posey, Avery D.; Engels, Boris; Singh, Reshma; Ezell, Tucker; Idamakanti, Neeraja; Ramones, Melissa H.; Li, Na; Zhou, Li; Plesa, Gabriela; Seykora, John T.; Okada, Hideho; June, Carl H.; Brogdon, Jennifer L.; Maus, Marcela V.

    2015-01-01

    Chimeric antigen receptors (CARs) are synthetic molecules designed to redirect T cells to specific antigens. CAR-modified T cells can mediate long-term durable remissions in B cell malignancies, but expanding this platform to solid tumors requires the discovery of surface targets with limited expression in normal tissues. The variant III mutation of the epidermal growth factor receptor (EGFRvIII) results from an in-frame deletion of a portion of the extracellular domain, creating a neoepitope. We chose a vector backbone encoding a second-generation CAR based on efficacy of a murine scFv–based CAR in a xenograft model of glioblastoma. Next, we generated a panel of humanized scFvs and tested their specificity and function as soluble proteins and in the form of CAR-transduced T cells; a low-affinity scFv was selected on the basis of its specificity for EGFRvIII over wild-type EGFR. The lead candidate scFv was tested in vitro for its ability to direct CAR-transduced T cells to specifically lyse, proliferate, and secrete cytokines in response to antigen-bearing targets. We further evaluated the specificity of the lead CAR candidate in vitro against EGFR-expressing keratinocytes and in vivo in a model of mice grafted with normal human skin. EGFRvIII-directed CAR T cells were also able to control tumor growth in xenogeneic subcutaneous and orthotopic models of human EGFRvIII+ glioblastoma. On the basis of these results, we have designed a phase 1 clinical study of CAR T cells transduced with humanized scFv directed to EGFRvIII in patients with either residual or recurrent glioblastoma (NCT02209376). PMID:25696001

  1. Rational development and characterization of humanized anti-EGFR variant III chimeric antigen receptor T cells for glioblastoma.

    Science.gov (United States)

    Johnson, Laura A; Scholler, John; Ohkuri, Takayuki; Kosaka, Akemi; Patel, Prachi R; McGettigan, Shannon E; Nace, Arben K; Dentchev, Tzvete; Thekkat, Pramod; Loew, Andreas; Boesteanu, Alina C; Cogdill, Alexandria P; Chen, Taylor; Fraietta, Joseph A; Kloss, Christopher C; Posey, Avery D; Engels, Boris; Singh, Reshma; Ezell, Tucker; Idamakanti, Neeraja; Ramones, Melissa H; Li, Na; Zhou, Li; Plesa, Gabriela; Seykora, John T; Okada, Hideho; June, Carl H; Brogdon, Jennifer L; Maus, Marcela V

    2015-02-18

    Chimeric antigen receptors (CARs) are synthetic molecules designed to redirect T cells to specific antigens. CAR-modified T cells can mediate long-term durable remissions in B cell malignancies, but expanding this platform to solid tumors requires the discovery of surface targets with limited expression in normal tissues. The variant III mutation of the epidermal growth factor receptor (EGFRvIII) results from an in-frame deletion of a portion of the extracellular domain, creating a neoepitope. We chose a vector backbone encoding a second-generation CAR based on efficacy of a murine scFv-based CAR in a xenograft model of glioblastoma. Next, we generated a panel of humanized scFvs and tested their specificity and function as soluble proteins and in the form of CAR-transduced T cells; a low-affinity scFv was selected on the basis of its specificity for EGFRvIII over wild-type EGFR. The lead candidate scFv was tested in vitro for its ability to direct CAR-transduced T cells to specifically lyse, proliferate, and secrete cytokines in response to antigen-bearing targets. We further evaluated the specificity of the lead CAR candidate in vitro against EGFR-expressing keratinocytes and in vivo in a model of mice grafted with normal human skin. EGFRvIII-directed CAR T cells were also able to control tumor growth in xenogeneic subcutaneous and orthotopic models of human EGFRvIII(+) glioblastoma. On the basis of these results, we have designed a phase 1 clinical study of CAR T cells transduced with humanized scFv directed to EGFRvIII in patients with either residual or recurrent glioblastoma (NCT02209376). Copyright © 2015, American Association for the Advancement of Science.

  2. Surface characterization of III-V MOCVD films from heterocyclic single-source precursors; Oberflaechencharakterisierung von III-V MOCVD-Filmen aus heterozyklischen Single Source Precursoren

    Energy Technology Data Exchange (ETDEWEB)

    Seemayer, Andreas

    2009-07-13

    In the present thesis the sublimation and evaporation properties of heterocyclic gallium and antimony containing single-source precursors as well as the chemical composition and morphology of the films fabricated from this were studied. The single-source precursors available by a new synthesis route were characterized concerning their evaporation properties and the obtained films studied surface-physically. By this way the process parameters were optimized and the applicability of the single-source precursors in HV-MOCVD processes studied. By evaporation experiments in the UHV it could be shown that thereby lighter ligands like ethyl- and methyl-groups lead to a lower contamination of the reaction space with carbon containing molecules. Furthermore it was expected that the 6-rings synthetized with short ligands exhibit a high stability. This however could not be confirmed. By unwanted parasitary reactions in the gaseous phase respectively dissociative sublimation in the gaseous phase a deposition of GaSb with these precursors was not possible. The 4-ring stabilized with tertiary-butyl and ethyl-groups caused in the evaporation the largest contamination of the gaseous phase, becauselonger-chain hydrocarbons exhibil only a bad pump cross section. By parasitary reactions originating elementary antimony is detectable in the gaseous phase. The films were studied concerning their chemical composition and their transport- respectively storage-conditioned surface contamination. Furthermore it has become clear that not only a purely synthetized precursor substance but also the reactor design is deciding for a successful deposition and a high film quality. First by successive optimization of the evaporation geometry it was possible to reduce the roughness of the produced GaSb films down to about 10 nm-30 nm.

  3. Spectroscopic characterization of the competitive binding of Eu(III), Ca(II), and Cu(II) to a sedimentary originated humic acid

    Energy Technology Data Exchange (ETDEWEB)

    Marang, L.; Reiller, P.E. [CEA Saclay, Nucl Energy Div, DPC SECR, Lab Speciat Radionucleides and Mol, 91 - Gif sur Yvette (France); Marang, L.; Benedetti, M.F. [Univ Paris 07, Lab Geochim Eaux, IPGP UMR CNRS 7154, F-75205 Paris 13 (France); Eidner, S.; Kumke, M.U. [Univ Potsdam, Inst Chem, D-14476 Potsdam (Germany)

    2009-06-15

    The competition between REE, alkaline earth and d-transition metals for organic matter binding sites is still an open field of research; particularly, the mechanisms governing these phenomena need to be characterized in more detail. In this study, we examine spectroscopically the mechanisms of competitive binding of Eu(III)/Cu(II) and Eu(III)/Ca(II) pair to Gorleben humic acid (HA), as previously proposed in the framework of the NICA-Donnan model. The evolution of time-resolved laser induced luminescence spectra of humic-complexed Eu(Ill) showed two strikingly different environments for a comparable bound proportion for Cu(II) and Ca(II). Cu(II) seems to compete more effectively with Eu(III) inducing its release into the Donnan phase, and into the bulk solution as free Eu{sup 3+}. This is evidenced both by the shapes of the spectra and by the decrease in the luminescence decay times. In contrast with that, Ca(II) induces a modification of the HA structure, which enhances the luminescence of humic-bound Eu(III), and causes a minor modification of the chemical environment of the complexed rare earth ion. (authors)

  4. Characterization of the Edge Crack Torsion (ECT) Test for Mode III Fracture Toughness Measurement of Laminated Composites

    Science.gov (United States)

    Ratcliffe, James G.

    2004-01-01

    The edge crack torsion (ECT) test is designed to initiate mode III delamination growth in composite laminates. The test has undergone several design changes during its development. The objective of this paper was to determine the suitability of the current ECT test design a mode III fracture test. To this end, ECT tests were conducted on specimens manufactured from IM7/8552 and S2/8552 tape laminates. Three-dimensional finite element analyses were performed. The analysis results were used to calculate the distribution of mode I, mode II, and mode III strain energy release rate along the delamination front. The results indicated that mode IIIdominated delamination growth would be initiated from the specimen center. However, in specimens of both material types, the measured values of GIIIc exhibited significant dependence on delamination length. Load-displacement response of the specimens exhibited significant deviation from linearity before specimen failure. X-radiographs of a sample of specimens revealed that damage was initiated in the specimens prior to failure. Further inspection of the failure surfaces is required to identify the damage and determine that mode III delamination is initiated in the specimens.

  5. Structural and catalytic characterization of a heterovalent Mn(II)Mn(III) complex that mimics purple acid phosphatases.

    Science.gov (United States)

    Smith, Sarah J; Riley, Mark J; Noble, Christopher J; Hanson, Graeme R; Stranger, Robert; Jayaratne, Vidura; Cavigliasso, Germán; Schenk, Gerhard; Gahan, Lawrence R

    2009-11-02

    The binuclear heterovalent manganese model complex [Mn(II)Mn(III)(L1)(OAc)(2)] ClO(4) x H(2)O (H(2)L1 = 2-(((3-((bis(pyridin-2-ylmethyl)amino)methyl)-2-hydroxy-5-methylbenzyl)(pyridin-2-ylmethyl)amino)-methyl)phenol) has been prepared and studied structurally, spectroscopically, and computationally. The magnetic and electronic properties of the complex have been related to its structure. The complex is weakly antiferromagnetically coupled (J approximately -5 cm(-1), H = -2J S(1) x S(2)) and the electron paramagnetic resonance (EPR) and magnetic circular dichroism (MCD) spectra identify the Jahn-Teller distortion of the Mn(III) center as predominantly a tetragonal compression, with a significant rhombic component. Electronic structure calculations using density functional theory have confirmed the conclusions derived from the experimental investigations. In contrast to isostructural M(II)Fe(III) complexes (M = Fe, Mn, Zn, Ni), the Mn(II)Mn(III) system is bifunctional possessing both catalase and hydrolase activities, and only one catalytically relevant pK(a) (= 8.2) is detected. Mechanistic implications are discussed.

  6. Characterization of HMPA-Coordinated Titanium(III) Species in Solutions of Zinc-Reduced Titanocene Dihalides

    DEFF Research Database (Denmark)

    Larsen, Jens; Juel Enemærke, Rasmus; Daasbjerg, Kim

    2006-01-01

    of mainly Cp2Ti(hmpa)+, Cp2Ti(hmpa)2+, and Cp2TiX(hmpa) with an increase in the amount of ionic constituents as X is changed from Cl to Br and I. The oxidation potentials of all HMPA-coordinated TiIII species are more negative than those of the uncoordinated analogues, but nevertheless an inverse...

  7. Transmission electron microscopy study of microstructural properties and dislocation characterization in the GaN film grown on the cone-shaped patterned Al2O3 substrate.

    Science.gov (United States)

    Park, Jung Sik; Yang, Jun-Mo; Park, Kyung Jin; Park, Yun Chang; Yoo, Jung Ho; Jeong, Chil Seong; Park, Jucheol; He, Yinsheng; Shin, Keesam

    2014-02-01

    Growing a GaN film on a patterned Al2O3 substrate is one of the methods of reducing threading dislocations (TDs), which can significantly deteriorate the performance of GaN-based LEDs. In this study, the microstructural details of the GaN film grown on a cone-shaped patterned Al2O3 substrate were investigated using high-resolution transmission electron microscopy and weak-beam dark-field techniques. Various defects such as misfit dislocations (MDs), recrystallized GaN (R-GaN) islands and nano-voids were observed on the patterned Al2O3 surfaces, i.e. the flat surface (FS), the inclined surface (IS) and the top surface (TS), respectively. Especially, the crystallographic orientation of R-GaN between the GaN film and the inclined Al2O3 substrate was identified as $[\\overline 1 2\\overline 1 0]_{{\\rm GaN}} \\hbox{//}[\\overline 1 101]_{{\\rm R - GaN} \\,{\\rm on}\\,{\\rm IS}} \\hbox{//}[\\overline 1 100]_{ {{\\rm Al}} _{\\rm 2} {\\rm O}_{\\rm 3}} $, $(\\overline 1 012)_{{\\rm GaN}} \\hbox{//}(1\\overline 1 02)_{{\\rm R - Ga}\\,{\\rm Non}\\,{\\rm IS}} \\hbox{//}(\\overline {11} 26)_{ {{\\rm Al}} _{\\rm 2} {\\rm O}_{\\rm 3}} $. In addition, a rotation by 9° between $(10\\overline 1 1)_{{\\rm R - GaN}} $ and $(0002)_{{\\rm GaN}} $ and between $(10\\overline 1 1)_{{\\rm R - GaN}} $ and $(0006)_{ {{\\rm Al}} _{\\rm 2} {\\rm O}_{\\rm 3}} $ was found to reduce the lattice mismatch between the GaN film and the Al2O3 substrate. Many TDs in the GaN film were observed on the FS and TS of Al2O3. However, few TDs were observed on the IS. Most of the TDs generated from the FS of Al2O3 were bent to the inclined facet rather than propagating to the GaN surface, resulting in a reduction in the dislocation density. Most of the TDs generated from the TS of Al2O3 were characterized as edge dislocations.

  8. Identification and characterization of a tandem repeat in exon III of the dopamine receptor D4 (DRD4) gene in cetaceans

    DEFF Research Database (Denmark)

    Mogensen, Line; Kinze, Carl Christian; Werge, Thomas

    2006-01-01

    A large number of mammalian species harbor a tandem repeat in exon III of the gene encoding dopamine receptor D4 (DRD4), a receptor associated with cognitive functions. In this study, a DRD4 gene exon III tandem repeat from the order Cetacea was identified and characterized. Included in our study...... were samples from 10 white-beaked dolphins (Lagenorhynchus albirostris), 10 harbor porpoises (Phocoena phocoena), eight sperm whales (Physeter macrocephalus), and five minke whales (Balaenoptera acutorostrata). Using enzymatic amplification followed by sequencing of amplified fragments, a tandem repeat...... composed of 18-bp basic units was detected in all of these species. The tandem repeats in white-beaked dolphin and harbor porpoise were both monomorphic and consisted of 11 and 12 basic units, respectively. In contrast, the sperm whale harbored a polymorphic tandem repeat with size variants composed...

  9. Synthesis, physicochemical characterization, DFT calculation and biological activities of Fe(III) and Co(II)-omeprazole complexes. Potential application in the Helicobacter pylori eradication

    Science.gov (United States)

    Russo, Marcos G.; Vega Hissi, Esteban G.; Rizzi, Alberto C.; Brondino, Carlos D.; Salinas Ibañez, Ángel G.; Vega, Alba E.; Silva, Humberto J.; Mercader, Roberto; Narda, Griselda E.

    2014-03-01

    The reaction between the antiulcer agent omeprazole (OMZ) with Fe(III) and Co(II) ions was studied, observing a high ability to form metal complexes. The isolated microcrystalline solid complexes were characterized by elemental analysis, X-ray powder diffraction (XRPD), Scanning Electron Microscopy (SEM), magnetic measurements, thermal study, FTIR, UV-Visible, Mössbauer, electronic paramagnetic resonance (EPR), and DFT calculations. The metal-ligand ratio for both complexes was 1:2 determined by elemental and thermal analysis. FTIR spectroscopy showed that OMZ acts as a neutral bidentate ligand through the pyridinic nitrogen of the benzimidazole ring and the oxygen atom of the sulfoxide group, forming a five-membered ring chelate. Electronic, Mössbauer, and EPR spectra together with magnetic measurements indicate a distorted octahedral geometry around the metal ions, where the coordination sphere is completed by two water molecules. SEM and XRPD were used to characterize the morphology and the crystal nature of the complexes. The most favorable conformation for the Fe(III)-OMZ and Co(II)-OMZ complexes was obtained by DFT calculations by using B3LYP/6-31G(d)&LanL2DZ//B3LYP/3-21G(d)&LanL2DZ basis set. Studies of solubility along with the antibacterial activity against Helicobacter pylori for OMZ and its Co(II) and Fe(III) complexes are also reported. Free OMZ and both metal complexes showed antibacterial activity against H. pylori. Co(II)-OMZ presented a minimal inhibitory concentration ˜32 times lower than that of OMZ and ˜65 lower than Fe(III)-OMZ, revealing its promising potential use for the treatment of gastric pathologies associated with the Gram negative bacteria. The morphological changes observed in the cell membrane of the bacteria after the incubation with the metal-complexes were also analyzed by SEM microscopy. The antimicrobial activity of the complexes was proved by the viability test.

  10. Characterization and Properties of Activated Carbon Prepared from Tamarind Seeds by KOH Activation for Fe(III) Adsorption from Aqueous Solution

    Science.gov (United States)

    Mopoung, Sumrit; Moonsri, Phansiri; Palas, Wanwimon; Khumpai, Sataporn

    2015-01-01

    This research studies the characterization of activated carbon from tamarind seed with KOH activation. The effects of 0.5 : 1–1.5 : 1 KOH : tamarind seed charcoal ratios and 500–700°C activation temperatures were studied. FTIR, SEM-EDS, XRD, and BET were used to characterize tamarind seed and the activated carbon prepared from them. Proximate analysis, percent yield, iodine number, methylene blue number, and preliminary test of Fe(III) adsorption were also studied. Fe(III) adsorption was carried out by 30 mL column with 5–20 ppm Fe(III) initial concentrations. The percent yield of activated carbon prepared from tamarind seed with KOH activation decreased with increasing activation temperature and impregnation ratios, which were in the range from 54.09 to 82.03 wt%. The surface functional groups of activated carbon are O–H, C=O, C–O, –CO3, C–H, and Si–H. The XRD result showed high crystallinity coming from a potassium compound in the activated carbon. The main elements found in the activated carbon by EDS are C, O, Si, and K. The results of iodine and methylene blue adsorption indicate that the pore size of the activated carbon is mostly in the range of mesopore and macropore. The average BET pore size and BET surface area of activated carbon are 67.9764 Å and 2.7167 m2/g, respectively. Finally, the tamarind seed based activated carbon produced with 500°C activation temperature and 1.0 : 1 KOH : tamarind seed charcoal ratio was used for Fe(III) adsorption test. It was shown that Fe(III) was adsorbed in alkaline conditions and adsorption increased with increasing Fe(III) initial concentration from 5 to 20 ppm with capacity adsorption of 0.0069–0.019 mg/g. PMID:26689357

  11. Multi-probe microstructure tracking during heat treatment without an in-situ setup: Case studies on martensitic steel, dual phase steel and β-Ti alloy

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Jiali, E-mail: j.zhang@mpie.de; Morsdorf, Lutz, E-mail: l.morsdorf@mpie.de; Tasan, Cemal Cem, E-mail: c.tasan@mpie.de

    2016-01-15

    In-situ scanning electron microscopy observations of the microstructure evolution during heat treatments are increasingly demanded due to the growing number of alloys with complex microstructures. Post-mortem characterization of the as-processed microstructures rarely provides sufficient insight on the exact route of the microstructure formation. On the other hand, in-situ SEM approaches are often limited due to the arising challenges upon using an in-situ heating setup, e.g. in (i) employing different detectors, (ii) preventing specimen surface degradation, or (iii) controlling and measuring the temperature precisely. Here, we explore and expand the capabilities of the “mid-way” solution by step-wise microstructure tracking, ex-situ, at selected steps of heat treatment. This approach circumvents the limitations above, as it involves an atmosphere and temperature well-controlled dilatometer, and high resolution microstructure characterization (using electron channeling contrast imaging, electron backscatter diffraction, atom probe tomography, etc.). We demonstrate the capabilities of this approach by focusing on three cases: (i) nano-scale carbide precipitation during low-temperature tempering of martensitic steels, (ii) formation of transformation-induced geometrically necessary dislocations in a dual-phase steel during intercritical annealing, and (iii) the partial recrystallization of a metastable β-Ti alloy. - Highlights: • A multi-probe method to track microstructures during heat treatment is developed. • It enables the analysis of various complex phenomena, even those at atomistic scale. • It circumvents some of the free surface effects of classical in-situ experiments.

  12. Synthesis, characterization, spectroscopic and catalytic oxidation studies of Fe(III), Ni(II), Co(III), V(IV) and U(VI) Schiff base complexes with N, O donor ligands derived from 2,3-diaminopyridine

    Energy Technology Data Exchange (ETDEWEB)

    Zabardasti, Abedien; Shangaie, Sayed Asad [Lorestan Univ., Khorramabad (Iran, Islamic Republic of). Dept. of Chemistry

    2016-10-15

    Fifteen new complexes of transition metals were designed using three Schiff base ligands and aldol condensation of 2,3-diaminopyridine with 5-R-2-hydroxybenzaldehyde (R = F, Cl, Br) in the 1:2 molar ratio. The tetradentate ligands N,N{sup '}-bis(5-R-2-hydroxybenzaldehyde) pyridine were acquired with the common formula H{sub 2}[(5-R-sal){sub 2}py] and characterized by IR, UV-Vis spectra, {sup 1}H-NMR and elemental analysis. These ligands produce 1:1 complexes M[(5-R-sal){sub 2}py] with Fe(III), Ni(II), Co(III), V(IV) and U(VI) metal ions. The electronic property and nature of complexes were identified by IR, UV-Vis spectra, elemental analysis, X-ray crystallography and cyclic voltammetric methods. The catalytic activity of complexes for epoxidation of styrene with UHP as primary oxidant at minimal temperature (10 C) has been planned. The spectral data of the ligands and their complexes are deliberate in connection with the structural changes which happen due to complex preparation. The electrochemical outcome has good conformability with what suggested for electronic interaction among metal center and ligand by the UV-Vis and IR measurements.

  13. Microstructural Characterization of a Directionally-Solidified Ni-33 (at. %)Al-31Cr-3Mo Eutectic Alloy as a Function of Withdrawal Rate

    Science.gov (United States)

    Raj, S. V.; Locci, I. E.; Whittenberger, J. D.; Salem, J. A.

    2000-01-01

    The Ni-33 (at. %)Al-3lCr-3Mo eutectic alloy was directionally-solidified (DS) at different rates, V(sub I), varying between 2.5 to 508 mm/ h. Detailed qualitative and quantitative metallographic and chemical analyses were conducted on the directionally-solidified rods. The microstructures consisted of eutectic colonies with parallel lamellar NiAl/(Cr,Mo) plates for solidification rates at and below 12.7 mm/ h. Cellular eutectic microstructures were observed at higher solidification rates, where the plates exhibited a radial pattern. The microstructures were demonstrated to be fairly uniform throughout a 100 mm length of the DS zone by quantitative metallography. The average cell size, bar-d, decreased with increasing growth rate to a value of 125 microns at 508 mm/ h according to the relation bar-d (microns) approx. = 465 V(sup -0.22, sub I), where V(sub I) is in mm/ h. Both the average NiAl plate thickness, bar-Delta(sub NiAl), and the interlamellar spacing, bar-lambda, were observed to be constant for V(sub I) less than or = 50.8 mm/ h but decreased with increasing growth rate above this value as 0.93 bar-Delta(sub NiAl)(microns) = 61.2 V(sup -0.93, sub I) and bar-lambda (microns) = 47.7 V(sup -0.64, sub I), respectively. The present results are detailed on a microstructural map. Keywords Optical microscopy, microstructure, compounds intermetallic, directional solidification

  14. AND Dy(III)

    African Journals Online (AJOL)

    userpc

    SYNTHESIS, SPECTROSCOPIC CHARACTERIZATION AND BIOLOGICAL. ACTIVITIES OF Sm(III) AND Dy(III) COMPLEXES WITH SCHIFF BASE DERIVED FROM. 2-HYDROXY-1-NAPHTHALDEHYDE AND 2-AMINOBENZOIC ACID. 1Bashir, S.S. and Abdulhadi, A. 1Department of Chemistry, Rabi'u Musa Kwankwaso ...

  15. Purification and characterization of inulin fructotransferase (DFA III-forming) from Arthrobacter aurescens SK 8.001.

    Science.gov (United States)

    Zhao, Meng; Mu, Wanmeng; Jiang, Bo; Zhou, Leon; Zhang, Tao; Lu, Zhengrong; Jin, Zhengyu; Yang, Ruijin

    2011-01-01

    The soil bacterium Arthrobacter aurescens SK 8.001 produces inulin fructotransferase (IFTase), and liquid chromatography-mass spectrometry (LC-MS) and carbon-13 nuclear magnetic resonance (13C NMR) analysis demonstrated that the main product of the enzyme was difructose anhydride III (DFA III). The IFTase was purified by ethanol precipitation, DEAE Sepharose Fast Flow, and Superdex 200 10/300 GL gel chromatography. Its molecular mass was estimated to be 40 kDa by SDS-PAGE and 35 kDa by gel filtration. The enzyme showed maximum activity at pH 5.5 and 60-70 °C, and retained 86.5% of its initial activity after incubation at 60 °C for 4 h. Chemical modification results suggested that a tryptophan residue is essential to enzyme activity. The N-terminal amino acid sequence was determined as AEGAKASPLNSPNVYDVT. The kinetic values, Km and Vmax, were estimated to be 0.52 mM and 0.3 μmol/ml min. Nystose was observed to be the smallest substrate for the produced IFTase. This IFTase provides a promising way to utilize inulin for the production of DFA III. Copyright © 2010. Published by Elsevier Ltd.

  16. Structural, EPR and Mössbauer Characterization of (μ-Alkoxo)(μ-Carboxylato)Diiron(II,III) Model Complexes for the Active Sites of Mixed-valent Diiron Enzymes

    Science.gov (United States)

    Li, Feifei; Chakrabarti, Mrinmoy; Dong, Yanhong; Kauffmann, Karl; Bominaar, Emile L.; Münck, Eckard; Que, Lawrence

    2012-01-01

    To obtain structural and spectroscopic models for the diiron(II,III) centers in the active sites of diiron enzymes, the (μ-alkoxo)(μ-carboxylato)diiron(II,III) complexes [FeIIFeIII(N-Et-HPTB)(O2CPh)(NCCH3)2](ClO4)3 (1) and [FeIIFeIII(N-Et-HPTB)(O2CPh) (Cl)(HOCH3)](ClO4)2 (2) (N-Et-HPTB = N,N,N′,N′-tetrakis(2-(1-ethyl-benzimidazolylmethyl))-2-hydroxy-1,3-diamino propane), have been prepared and characterized by X-ray crystallography, EPR, and Mössbauer spectroscopy. The Fe1-Fe2 separations are 3.60 Å and 3.63 Å and the Fe1-O1-Fe2 bond angles are 128.0° and 129.4° for 1 and 2, respectively. Mössbauer and EPR studies of 1 show that the FeIII (SA = 5/2) and FeII (SB = 2) sites are antiferromagnetically coupled to yield a ground state with S = 1/2 (g = 1.75, 1.88, 1.96); Mössbauer analysis of solid 1 yields J = 22.5 ± 2 cm−1 for the exchange coupling constant ( = JSA•SB convention). In addition to the S = 1/2 ground state spectrum of 1, the EPR signal for the S = 3/2 excited state of the spin ladder can also be observed, the first time such a signal has been detected for an antiferromagnetically coupled diiron(II,III) complex. The anisotropy of the 57Fe magnetic hyperfine interactions at the FeIII site is larger than normally observed in mononuclear complexes and arises from admixing S > 1/2 excited states into the S = 1/2 ground state by zero-field splittings at the two Fe sites. Analysis of the “D/J” mixing has allowed us to extract the zero-field splitting parameters, local g values, and magnetic hyperfine structural parameters for the individual Fe sites. The methodology developed and followed in this analysis is presented in detail. The spin Hamiltonian parameters of 1 are related to the molecular structure with the help of DFT calculations. Contrary to what was assumed in previous studies, our analysis demonstrates that the deviations of the g-values from the free electron value (g = 2) for the antiferromagnetically coupled diiron(II,III

  17. Synthesis, characterization, cytotoxic and antitubercular activities of new gold(I) and gold(III) complexes containing ligands derived from carbohydrates.

    Science.gov (United States)

    Chaves, Joana Darc Souza; Damasceno, Jaqueline Lopes; Paula, Marcela Cristina Ferreira; de Oliveira, Pollyanna Francielli; Azevedo, Gustavo Chevitarese; Matos, Renato Camargo; Lourenço, Maria Cristina S; Tavares, Denise Crispim; Silva, Heveline; Fontes, Ana Paula Soares; de Almeida, Mauro Vieira

    2015-10-01

    Novel gold(I) and gold(III) complexes containing derivatives of D-galactose, D-ribose and D-glucono-1,5-lactone as ligands were synthesized and characterized by IR, (1)H, and (13)C NMR, high resolution mass spectra and cyclic voltammetry. The compounds were evaluated in vitro for their cytotoxicity against three types of tumor cells: cervical carcinoma (HeLa) breast adenocarcinoma (MCF-7) and glioblastoma (MO59J) and one non-tumor cell line: human lung fibroblasts (GM07492A). Their antitubercular activity was evaluated as well expressed as the minimum inhibitory concentration (MIC90) in μg/mL. In general, the gold(I) complexes were more active than gold(III) complexes, for example, the gold(I) complex (1) was about 8.8 times and 7.6 times more cytotoxic than gold(III) complex (8) in MO59J and MCF-7 cells, respectively. Ribose and alkyl phosphine derivative complexes were more active than galactose and aryl phosphine complexes. The presence of a thiazolidine ring did not improve the cytotoxicity. The study of the cytotoxic activity revealed effective antitumor activities for the gold(I) complexes, being more active than cisplatin in all the tested tumor cell lines. Gold(I) compounds (1), (2), (3), (4) and (6) exhibited relevant antitubercular activity even when compared with first line drugs such as rifampicin.

  18. Crystal and molecular structure of novel binuclear ten coordinated praseodymium(III with octadentateethylenediaminetetraacetate – Synthesis, characterization and antioxidant, antiviral and anticancer activities

    Directory of Open Access Journals (Sweden)

    R. Pradeep

    2017-03-01

    Full Text Available A novel ten coordinated binuclear hydrated praseodymium(III ethylenediaminetetraacetate with phenyl hydrazine has been synthesized and characterized by analytical, spectral and thermal techniques. The structure of the compound determined by X-ray crystallography reveals the binuclear nature of the complex with ten coordination around Pr(III ions. Neutral phenyl hydrazine molecules present outside the coordination sphere and four inner sphere water molecules found to occupy the coordination sites (each Pr(III ions possessing two coordinated water molecules. Among five more water molecules, four are involved in hydrogen bonding with phenyl hydrazine and EDTA4− and hence present in the second sphere. The remaining water molecule is present as bulk water. Interestingly, in the present case EDTA4− ions act as heptadentate ligand with one acetate group from each EDTA4− ion showing novel tridentate bridging behavior. The biological studies such as antioxidantal, antiviral and cytotoxicity studies reveal that this complex indeed shows promising activity.

  19. Removal of arsenic(III,V) by a granular Mn-oxide-doped Al oxide adsorbent: surface characterization and performance.

    Science.gov (United States)

    Wu, Kun; Zhang, Jin; Chang, Bing; Liu, Ting; Zhang, Furong; Jin, Pengkang; Wang, Wendong; Wang, Xiaochang

    2017-06-23

    In order to remove arsenic (As) from contaminated water, granular Mn-oxide-doped Al oxide (GMAO) was fabricated using the compression method with the addition of organic binder. The analysis results of XRD, SEM, and BET indicated that GMAO was microporous with a large specific surface area of 54.26 m(2/)g, and it was formed through the aggregation of massive Al/Mn oxide nanoparticles with an amorphous pattern. EDX, mapping, FTIR, and XPS results showed the uniform distribution of Al/Mn elements and numerous hydroxyl groups on the adsorbent surface. Compression tests indicated a satisfactory mechanical strength of GMAO. Batch adsorption results showed that As(V) adsorption achieved equilibrium faster than As(III), whereas the maximum adsorption capacity of As(III) estimated from the Langmuir isotherm at 25 °C (48.52 mg/g) was greater than that of As(V) (37.94 mg/g). The As removal efficiency could be maintained in a wide pH range of 3~8. The presence of phosphate posed a significant adverse effect on As adsorption due to the competition mechanisms. In contrast, Ca(2+) and Mg(2+) could favor As adsorption via cation-bridge involvement. A regeneration method was developed by using sodium hydroxide solution for As elution from saturated adsorbents, which permitted GMAO to keep over 75% of its As adsorption capacity even after five adsorption-regeneration cycles. Column experiments showed that the breakthrough volumes for the treatment of As(III)-spiked and As(V)-spiked water (As concentration = 100 μg/L) were 2224 and 1952, respectively. Overall, GMAO is a potential adsorbent for effectively removing As from As-contaminated groundwater in filter application.

  20. Evaluation of biofilm production and characterization of genes encoding type III secretion system among Pseudomonas aeruginosa isolated from burn patients.

    Science.gov (United States)

    Jabalameli, Fereshteh; Mirsalehian, Akbar; Khoramian, Babak; Aligholi, Marzieh; Khoramrooz, Seyed Sajjad; Asadollahi, Parisa; Taherikalani, Morovat; Emaneini, Mohammad

    2012-12-01

    Pseudomonas aeruginosa is one of the common pathogenic causes of serious infections in burn patients throughout the world. Type III secretion toxins are thought to promote the dissemination of P. aeruginosa from the site of infection, the bacterial evasion of the host immune response and inhibition of DNA synthesis leading to host cell death. A total of 96 isolates of P. aeruginosa were collected from wound infections of burn patients, from April to July 2010. Antimicrobial susceptibility of the isolates were determined by disk agar diffusion method. Polymerase chain reaction (PCR)-based method was used for targeting the genes encoding the type III secretion toxins. The quantitative determination of biofilm-forming capacity was determined by a colorimetric microtiter plate assay. All the isolates were resistant to cefixime and ceftriaxone. More than 90% of the isolates were resistant to amikacin, carbenicillin, cefepime, cefotaxime, cefpodoxime, gatifloxacin, gentamicin, piperacillin/tazobactam, ticarcillin and tobramycin. All the isolates carried the exoT gene, 95% carried exoY, 64.5% carried exoU and 29% carried the exoS gene. Most of the isolates (58%) carried both exoY and exoU genes while 24% showed the concomitant presence of exoS and exoY and 1% carried both exoS and exoU. Coexistence of exoS, exoY and exoU was seen in 4% of the isolates. Biofilm formation was seen in more than 96% of the isolates among which 47% were strong biofilm producers, 26% were moderate and 22.9% were weak biofilm formers. In conclusion, the findings of this study show that the genes, particularly the exoU gene, encoding the type III secretion toxins, are commonly disseminated among the P. aeruginosa strains isolated from burn patients. Copyright © 2012 Elsevier Ltd and ISBI. All rights reserved.

  1. Synthesis, structure, and characterization of new mononuclear Mn(II) complexes. Electrochemical conversion into new oxo-bridged Mn(2)(III,IV) complexes. Role of chloride ions.

    Science.gov (United States)

    Hureau, Christelle; Blondin, Geneviève; Charlot, Marie-France; Philouze, Christian; Nierlich, Martine; Césario, Michèle; Anxolabéhère-Mallart, Elodie

    2005-05-16

    Two Mn(II) complexes are isolated and X-ray characterized, namely, cis-[(L(2))Mn(II)(Cl)(2)] (1) and [(L(3))Mn(II)Cl(OH(2))](ClO(4)) (2(ClO(4))), where L(2) and L(3) are the well-known tetradentate N,N'-dimethyl-N,N'-bis(2-pyridylmethyl)ethane-1,2-diamine and N,N'-dimethyl-N,N'-bis(2-pyridylmethyl)propane-1,3-diamine ligands, respectively. The crystal structure reveals that whereas the ligand L(2) is in the cis-alpha conformation in complex 1, the ligand L(3) is in the more unusual cis-beta conformation in 2. EPR spectra are recorded on frozen solutions for both complexes and are characteristic of Mn(II) species. Electrochemical behaviors are investigated on acetonitrile solution for both complexes and show that cation 2 exists as closely related Mn(II) species in equilibrium. For both complexes exhaustive bulk electrolyses of acetonitrile solution are performed at oxidative potential in various experimental conditions. In the presence of 2,6-lutidine and after elimination of chloride ligands, the formation of the di-mu-oxo mixed-valent complexes [(L(2))Mn(III)(mu-O)(2)Mn(IV)(L(2))](3+) (3a) and [(L(3))Mn(III)(mu-O)(2)Mn(IV)(L(3))](3+) (4) is confirmed by UV-vis and EPR spectroscopies and cyclic voltammetry. In addition crystals of 4(ClO(4))(3) were isolated, and the X-ray structure reveals the cis-alphaconformation of L(3). In the absence of 2,6-lutidine and without elimination of the exogenous chloride ions, the electrochemical oxidation of 1 leads to the formation of the mononuclear Mn(III) complex, namely, [(L(2))Mn(III)(Cl)(2)](+) (5), as confirmed by UV-vis as well as parallel mode EPR spectroscopy and cyclic voltammetry. In the same conditions, the electrochemical oxidation of complex 2 is more intricate, and a thorough analysis of EPR spectra establishes the formation of the binuclear mono-mu-oxo mixed-valent [(L(3))ClMn(III)(mu-O)Mn(IV)Cl(L(3))](3+) (6) complexes. Electrochemical conversion of Mn(II) complexes into mixed-valent Mn(2)(III,IV) oxo

  2. Structural and Catalytic Characterization of a Heterovalent Mn(II)Mn(III) Complex That Mimics Purple Acid Phosphatases

    OpenAIRE

    Smith, Sarah J.; Riley, Mark J.; Noble, Christopher J.; Hanson, Graeme R.; Stranger, Robert; Jayaratne, Vidura; Cavigliasso, German; Schenk,Gerhard; Gahan, Lawrence R

    2009-01-01

    The binuclear heterovalent manganese model complex [Mn(II)Mn(III)(L1)(OAc)2] ClO4 3 H2O (H2L1 = 2-(((3-((bis- (pyridin-2-ylmethyl)amino)methyl)-2-hydroxy-5-methylbenzyl)(pyridin-2-ylmethyl)amino)-methyl)phenol) has been prepared and studied structurally, spectroscopically, and computationally. The magnetic and electronic properties of the complex have been related to its structure. The complex is weakly antiferromagnetically coupled (J ∼ -5 cm-1, H =-2J S1 3 S2) and the electron p...

  3. Spectroscopic and Kinetic Characterization of Peroxidase-Like π-Cation Radical Pinch-Porphyrin-Iron(III Reaction Intermediate Models of Peroxidase Enzymes

    Directory of Open Access Journals (Sweden)

    Samuel Hernández Anzaldo

    2016-06-01

    Full Text Available The spectroscopic and kinetic characterization of two intermediates from the H2O2 oxidation of three dimethyl ester [(proto, (meso, (deuteroporphyrinato (picdien]Fe(III complexes ([FePPPic], [FeMPPic] and [FeDPPic], respectively pinch-porphyrin peroxidase enzyme models, with s = 5/2 and 3/2 Fe(III quantum mixed spin (qms ground states is described herein. The kinetic study by UV/Vis at λmax = 465 nm showed two different types of kinetics during the oxidation process in the guaiacol test for peroxidases (1–3 + guaiacol + H2O2 → oxidation guaiacol products. The first intermediate was observed during the first 24 s of the reaction. When the reaction conditions were changed to higher concentration of pinch-porphyrins and hydrogen peroxide only one type of kinetics was observed. Next, the reaction was performed only between pinch-porphyrins-Fe(III and H2O2, resulting in only two types of kinetics that were developed during the first 0–4 s. After this time a self-oxidation process was observed. Our hypotheses state that the formation of the π-cation radicals, reaction intermediates of the pinch-porphyrin-Fe(III family with the ligand picdien [N,N’-bis-pyridin-2-ylmethyl-propane-1,3-diamine], occurred with unique kinetics that are different from the overall process and was involved in the oxidation pathway. UV-Vis, 1H-NMR and ESR spectra confirmed the formation of such intermediates. The results in this paper highlight the link between different spectroscopic techniques that positively depict the kinetic traits of artificial compounds with enzyme-like activity.

  4. IR, UV-Vis, magnetic and thermal characterization of chelates of some catecholamines and 4-aminoantipyrine with Fe(III) and Cu(II).

    Science.gov (United States)

    Mohamed, Gehad G; Zayed, M A; El-Dien, F A Nour; El-Nahas, Reham G

    2004-07-01

    The dopamine derivatives participate in the regulation of wide variety of physiological functions in the human body and in medication life. Increase and/or decrease in the concentration of dopamine in human body reflect an indication for diseases such as Schizophrenia and/or Parkinson diseases. Alpha-methyldopa (alpha-MD) in tablets is used in medication of hypertension. The Fe(III) and Cu(II) chelates with coupled products of adrenaline hydrogen tartarate (AHT), levodopa (LD), alpha-MD and carbidopa (CD) with 4-aminoantipyrine (4-AAP) are prepared and characterized. Different physico-chemical methods like IR, magnetic and UV-Vis spectra are used to investigate the structure of these chelates. Fe(III) form 1:2 (M:catecholamines) chelates while Cu(II) form 1:1 chelates. Catecholamines behave as a bidentate mono- or dibasic ligands in binding to the metal ions. IR spectra show that the catecholamines are coordinated to the metal ions in a bidentate manner with O,O donor sites of the phenolic -OH. Magnetic moment measurements reveal the presence of Fe(III) chelates in octahedral geometry while the Cu(II) chelates are square planar. The thermal decomposition of Fe(III) and Cu(II) complexes is studied using thermogravimetric (TGA) and differential thermal analysis (DTA) techniques. The water molecules are removed in the first step followed immediately by decomposition of the ligand molecules. The activation thermodynamic parameters, such as, energy of activation, enthalpy, entropy and free energy change of the complexes are evaluated and the relative thermal stability of the complexes are discussed.

  5. IR, UV-Vis, magnetic and thermal characterization of chelates of some catecholamines and 4-aminoantipyrine with Fe(III) and Cu(II)

    Science.gov (United States)

    Mohamed, Gehad G.; Zayed, M. A.; El-Dien, F. A. Nour; El-Nahas, Reham G.

    2004-07-01

    The dopamine derivatives participate in the regulation of wide variety of physiological functions in the human body and in medication life. Increase and/or decrease in the concentration of dopamine in human body reflect an indication for diseases such as Schizophrenia and/or Parkinson diseases. α-Methyldopa (α-MD) in tablets is used in medication of hypertension. The Fe(III) and Cu(II) chelates with coupled products of adrenaline hydrogen tartarate (AHT), levodopa (LD), α-MD and carbidopa (CD) with 4-aminoantipyrine (4-AAP) are prepared and characterized. Different physico-chemical methods like IR, magnetic and UV-Vis spectra are used to investigate the structure of these chelates. Fe(III) form 1:2 (M:catecholamines) chelates while Cu(II) form 1:1 chelates. Catecholamines behave as a bidentate mono- or dibasic ligands in binding to the metal ions. IR spectra show that the catecholamines are coordinated to the metal ions in a bidentate manner with O,O donor sites of the phenolic - OH. Magnetic moment measurements reveal the presence of Fe(III) chelates in octahedral geometry while the Cu(II) chelates are square planar. The thermal decomposition of Fe(III) and Cu(II) complexes is studied using thermogravimetric (TGA) and differential thermal analysis (DTA) techniques. The water molecules are removed in the first step followed immediately by decomposition of the ligand molecules. The activation thermodynamic parameters, such as, energy of activation, enthalpy, entropy and free energy change of the complexes are evaluated and the relative thermal stability of the complexes are discussed.

  6. Characterization of the chemical composition of PM2.5 emitted from on-road China III and China IV diesel trucks in Beijing, China.

    Science.gov (United States)

    Wu, Bobo; Shen, Xianbao; Cao, Xinyue; Yao, Zhiliang; Wu, Yunong

    2016-05-01

    The composition of diesel exhaust fine particulate matter (PM2.5) is of growing interest because of its impacts on health and climatic factors and its application in source apportionment and aerosol modeling. We characterized the detailed chemical composition of the PM2.5, including the organic carbon (OC), elemental carbon (EC), water-soluble ions (WSIs), and elemental contents, emitted from China III and China IV diesel trucks (nine each) based on real-world measurements in Beijing using a portable emissions measurement system (PEMS). Carbonaceous compounds were the dominant components (totaling approximately 87%) of the PM2.5, similar to the results (greater than 80% of the PM2.5) of our previous study of on-road China III diesel trucks. In general, the amounts of individual component groups (carbonaceous compounds, WSIs, and elements) and PM2.5 emissions for China IV diesel trucks were lower than those of China III diesel trucks of the same size, except for the WSIs and elements for the light- and medium-duty diesel trucks. The EC/OC mass ratios were strongly dependent on the emission standards, and the ratios of China IV diesel trucks were higher than those of China III diesel trucks of the same size. The chemical species in the PM2.5 were significantly affected by the driving conditions. Overall, the emission factors (EFs) of the PM2.5 and OC under non-highway (NHW) driving conditions were higher than those under highway (HW) driving conditions, and the EC/OC mass ratios presented an increasing trend, with decreasing OC/PM2.5 and increasing EC/PM2.5 from NHW to HW driving conditions; similar trends were reported in our previous study. In addition, Pearson's correlation coefficients among the PM2.5 species were analyzed to determine the relationships among the various chemical components. Copyright © 2016 Elsevier B.V. All rights reserved.

  7. Characterization of transition behavior in SA508 Gr.4N Ni-Cr-Mo low alloy steels with microstructural alteration by Ni and Cr contents

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Ki-Hyoung; Park, Sang-gyu [Department of Materials Science and Engineering, KAIST, Daejeon 305-701 (Korea, Republic of); Nuclear Materials Research Division, KAERI, Daejeon 305-353 (Korea, Republic of); Kim, Min-Chul, E-mail: mckim@kaeri.re.kr [Nuclear Materials Research Division, KAERI, Daejeon 305-353 (Korea, Republic of); Lee, Bong-Sang [Nuclear Materials Research Division, KAERI, Daejeon 305-353 (Korea, Republic of); Wee, Dang-Moon [Department of Materials Science and Engineering, KAIST, Daejeon 305-701 (Korea, Republic of)

    2011-11-25

    Highlights: {yields} We offer information for determining optimum alloying contents of SA508 Gr.4N steel. {yields} This study shows improvement of toughness with increasing Ni and Cr contents. {yields} Ni content is more effective on the impact toughness than on the fracture toughness. {yields} Cr content is more effective on the fracture toughness. {yields} We offer detailed information on relationship between toughness and microstructure. - Abstract: SA508 Gr.4N Ni-Cr-Mo low alloy steel, in which Ni and Cr contents are higher than in commercial reactor pressure vessel (RPV) steels, may be a candidate RPV material with the improved strength and toughness due to its tempered martensitic microstructure. This study aims at assessing the effects of microstructural factors with alloying element contents on the transition properties of Ni-Cr-Mo low alloy steels. Model alloys with different Ni and Cr contents were fabricated and their Charpy impact toughness and fracture toughness were examined in the transition region according to ASTM E23 and E1921 standard procedures, respectively. The test results showed extensive improvements of both impact toughness and fracture toughness with increasing Ni and Cr contents. However, Ni content was more effective on the impact toughness than on the fracture toughness, while Cr content was more effective on the fracture toughness. In order to identify a difference in effects of alloying elements contents on the fracture toughness and impact toughness, the relations between the transition properties and the scale of the microstructural features such as packets and carbides are discussed in detail.

  8. Surpassing the Theoretical Limit of Porosity in Conventional Solid-State Foaming: Microstructure Characterization of Length Scales in a Copper Metal Foam

    Science.gov (United States)

    2014-11-01

    time consuming, and in methods such as gas entrapment, there are practical limits to the porosity achievable due to pore coalescence and percolation...Frenkel AI. Reduction of CuO in H2: in situ time-resolved XRD studies. Catalysis Letters. 2003;85(3–4):247–254. 30. Tschopp M, Groeber M, Fahringer R...Scripta Materialia. 2010;62(6):357–360. 33. Torquato S. Random heterogeneous materials: microstructure and macroscopic properties. New York (NY

  9. WRKY domain-encoding genes of a crop legume chickpea (Cicer arietinum): comparative analysis with Medicago truncatula WRKY family and characterization of group-III gene(s).

    Science.gov (United States)

    Kumar, Kamal; Srivastava, Vikas; Purayannur, Savithri; Kaladhar, V Chandra; Cheruvu, Purnima Jaiswal; Verma, Praveen Kumar

    2016-06-01

    The WRKY genes have been identified as important transcriptional modulators predominantly during the environmental stresses, but they also play critical role at various stages of plant life cycle. We report the identification of WRKY domain (WD)-encoding genes from galegoid clade legumes chickpea (Cicer arietinum L.) and barrel medic (Medicago truncatula). In total, 78 and 98 WD-encoding genes were found in chickpea and barrel medic, respectively. Comparative analysis suggests the presence of both conserved and unique WRKYs, and expansion of WRKY family in M. truncatula primarily by tandem duplication. Exclusively found in galegoid legumes, CaWRKY16 and its orthologues encode for a novel protein having a transmembrane and partial Exo70 domains flanking a group-III WD. Genomic region of galegoids, having CaWRKY16, is more dynamic when compared with millettioids. In onion cells, fused CaWRKY16-EYFP showed punctate fluorescent signals in cytoplasm. The chickpea WRKY group-III genes were further characterized for their transcript level modulation during pathogenic stress and treatments of abscisic acid, jasmonic acid, and salicylic acid (SA) by real-time PCR. Differential regulation of genes was observed during Ascochyta rabiei infection and SA treatment. Characterization of A. rabiei and SA inducible gene CaWRKY50 showed that it localizes to plant nucleus, binds to W-box, and have a C-terminal transactivation domain. Overexpression of CaWRKY50 in tobacco plants resulted in early flowering and senescence. The in-depth comparative account presented here for two legume WRKY genes will be of great utility in hastening functional characterization of crop legume WRKYs and will also help in characterization of Exo70Js. © The Author 2016. Published by Oxford University Press on behalf of Kazusa DNA Research Institute.

  10. Characterization of the Multi-Pass Weld Metal and the Effect of Post-Weld Heat Treatment on Its Microstructure and Toughness

    Science.gov (United States)

    Wang, Xuelin; Shang, Chengjia; Wang, Xuemin

    In multi-pass welding process, various thermal cycle of both weld metal (WM) and heat affected zone (HAZ) will be subjected several times. This will make the initial microstructure occur an irreversible transformation. As the transformed microstructure become extremely complex, the mechanical properties, especially the low temperature toughness are very much fluctuant. In this research, the microstructure and low temperature toughness of WM obtained from a real multi-pass weld joint (up to 55 mm) by submerged arc welding have been elaborated. The results indicated that the necklace-type coarse martensite-austenite (M-A) constituent formed in interlayer heat affected zone (IHAZ) of WM and the impact energy of WM at -40 °C was only 39 J. Furthermore, by conventional tempering with holding time of 30 min, the toughness of WM can't be effectively improved. However, by a new developed heat treatment process, the toughness of WM could be significantly improved, and it is believed to be caused by the composition of weld metal and the post-welding heat treatment process. It also shows that the decomposition of M-A constituent and formation of the retained austenite are the mechanism of the improvement of low temperature toughness.

  11. Microstructure and microhardness characterization of Cr{sub 3}C{sub 2}-SiC coatings produced by the plasma transferred arc method

    Energy Technology Data Exchange (ETDEWEB)

    Islak, Serkan [Kastamonu Univ. (Turkey). Cide Rifat Ilgaz Vocational High School; Eski, Oezkan [Kastamonu Univ. (Turkey). Kastamonu Vocational High School; Buytoz, Soner [Firat Univ., Elazig (Turkey). Dept. of Metallurgy and Materials Engineering; Karagoez, Muzaffer [Bartin Univ. (Turkey). Dept. of Metallurgical and Materials Engineering; Stokes, Joseph [Dublin City Univ. (Ireland). School of Mechanical and Manufacturing Engineering

    2012-07-01

    The purpose of this work was to investigate the coatings made of Cr{sub 3}C{sub 2} and SiC powder manufactured on AISI 304 stainless steel applied by the plasma transferred arc (PTA) welding process. SiC content in the produced coated layer was varied between 0-100 wt. % and the effect of SiC concentration on the microstructure and hardness of the coating was measured experimentally. SEM analyses revealed that the composite coatings had a homogeneous, nonporous, and crack-free microstructure. Dendrites and interdendrite eutectics formed on the coating layer, subject to the temperature gradient and the solidification ratio. There was a significant increase in the hardness of coating layers with the effect of the {gamma}-(Fe,Ni), Cr{sub 7}C{sub 3}, Cr{sub 23}C{sub 6}, Fe{sub 5}C{sub 2}, Cr{sub 3}Si, CrSi{sub 2}, Fe{sub 0.64}Ni{sub 0.36}, CFe{sub 15.1}, C-(Fe,Cr)-Si phases formed in the microstructure. In comparison to the substrate, the microhardness of the coatings produced by PTA were 2.5-3.5 times harder. (orig.)

  12. Rapid Solidification of Sn-Cu-Al Alloys for High-Reliability, Lead-Free Solder: Part I. Microstructural Characterization of Rapidly Solidified Solders

    Science.gov (United States)

    Reeve, Kathlene N.; Choquette, Stephanie M.; Anderson, Iver E.; Handwerker, Carol A.

    2016-12-01

    Particles of Cu x Al y in Sn-Cu-Al solders have previously been shown to nucleate the Cu6Sn5 phase during solidification. In this study, the number and size of Cu6Sn5 nucleation sites were controlled through the particle size refinement of Cu x Al y via rapid solidification processing and controlled cooling in a differential scanning calorimeter. Cooling rates spanning eight orders of magnitude were used to refine the average Cu x Al y and Cu6Sn5 particle sizes down to submicron ranges. The average particle sizes, particle size distributions, and morphologies in the microstructures were analyzed as a function of alloy composition and cooling rate. Deep etching of the samples revealed the three-dimensional microstructures and illuminated the epitaxial and morphological relationships between the Cu x Al y and Cu6Sn5 phases. Transitions in the Cu6Sn5 particle morphologies from faceted rods to nonfaceted, equiaxed particles were observed as a function of both cooling rate and composition. Initial solidification cooling rates within the range of 103 to 104 °C/s were found to be optimal for realizing particle size refinement and maintaining the Cu x Al y /Cu6Sn5 nucleant relationship. In addition, little evidence of the formation or decomposition of the ternary- β phase in the solidified alloys was noted. Solidification pathways omitting the formation of the ternary- β phase agreed well with observed room temperature microstructures.

  13. Microstructural processes in irradiated materials

    Energy Technology Data Exchange (ETDEWEB)

    Byun, Thak Sang; Morgan, Dane; Jiao, Zhijie; Almer, Jonathan; Brown, Donald

    2016-04-01

    This is an editorial article (preface) for the publication of symposium papers in the Journal of Nuclear materials: These proceedings contain the papers presented at two symposia, the Microstructural Processes in Irradiated Materials (MPIM) and Characterization of Nuclear Reactor Materials and Components with Neutron and Synchrotron Radiation, held in the TMS 2015, 144th Annual Meeting & Exhibition at Walt Disney World, Orlando, Florida, USA on March 15–19, 2015.

  14. Electronic ceramic structure within the Voronoi cells model and microstructure fractals contacts surfaces new frontier applications

    Directory of Open Access Journals (Sweden)

    Mitić V.V.

    2013-01-01

    Full Text Available In this study, in order to establish grain shapes of sintered ceramics, new approach on correlation between microstructure and doped BaTiO3 -ceramics properties based, on Voronoi model and mathematical statistics calculations on fractal geometry, has been developed. BaTiO3-ceramics doped with Yb2O3 (from 0.1 to 1.0wt% of Yb were prepared by using conventional solid state procedure and were sintered from 1320°C to 1380°C for four hours. The microstructure of sintered specimens was investigated by Scanning electron microscope JEOL-SEM-5300. For better and deeper characterization and understanding of the ceramics material microstructure, the methods which include the fractal nature structure, and also Voronoi model and mathematical statistics calculations, are applied. In our research the Voronoi is one specific interface between fractal structure nature and different stochastically contact surfaces, defined by statistical mathematical methods. Also, the Voronoi model practically provided possibility to control the ceramics microstructure fractal nature. Mathematical statistic methods enabled establishing the real model for the prognosis based on correlation: synthesis-structures-properties. [Projekat Ministarstva nauke Republike Srbije, br. 172057 i br. III44006

  15. Identification and characterization of a class III chitin synthase gene of Moniliophthora perniciosa, the fungus that causes witches' broom disease of cacao.

    Science.gov (United States)

    Souza, Catiane S; Oliveira, Bruno M; Costa, Gustavo G L; Schriefer, Albert; Selbach-Schnadelbach, Alessandra; Uetanabaro, Ana Paula T; Pirovani, Carlos P; Pereira, Gonçalo A G; Taranto, Alex G; Cascardo, Júlio Cézar de M; Góes-Neto, Aristóteles

    2009-08-01

    Chitin synthase (CHS) is a glucosyltransferase that converts UDP-N-acetylglucosamine into chitin, one of the main components of fungal cell wall. Class III chitin synthases act directly in the formation of the cell wall. They catalyze the conversion of the immediate precursor of chitin and are responsible for the majority of chitin synthesis in fungi. As such, they are highly specific molecular targets for drugs that can inhibit the growth and development of fungal pathogens. In this work, we have identified and characterized a chitin synthase gene of Moniliophthora perniciosa (Mopchs) by primer walking. The complete gene sequence is 3,443 bp, interrupted by 13 small introns, and comprises a cDNA with an ORF with 2,739 bp, whose terminal region was experimentally determined, encoding a protein with 913 aa that harbors all the motifs and domains typically found in class III chitin synthases. This is the first report on the characterization of a chitin synthase gene, its mature transcription product, and its putative protein in basidioma and secondary mycelium stages of M. perniciosa, a basidiomycotan fungus that causes witches' broom disease of cacao.

  16. The solid solution Sr3Ti2-xFexO7-δ (x ≤ 0.5: characterization of Fe (III – Fe (IV mixed valences

    Directory of Open Access Journals (Sweden)

    I. Zvereva

    2016-03-01

    Full Text Available The results of a magneto chemical and Mössbauer characterization are reported for the solid solution Sr3Ti2-xFexO7-δ (x ≤ 0.5, the intergrowth of a double perovskite block and one rock-salt layer type. The charge compensation mechanism induced by the introduction of iron atoms in the matrix of Sr3Ti2O7 is sensitive to the conditions of synthesis, namely an oxidation process triggers the formation of mixed Fe(III-Fe(IV valences. The crystallographic characterization - variation of the cell parameters and structure calculations – brings evidence for the respective occurrence of mixed valences and oxygen vacancies which form in the middle plane of the double perovskite block. Ferromagnetic exchange interactions which are absent in the Fe(III containing compositions, appear and progressively strengthen depending on the oxidizing treatment. They are ascribed to the presence of an increasing amount of Fe(IV species. Remarkably, a mixed valence state of iron forms during annealing in air with an increasing contribution of the Fe(IV species for the larger iron contents, as deduced from Mössbauer data.

  17. Synthesis and characterization of dinuclear complexes containing the Fe(III)-F...(H2O)M(II) motif

    DEFF Research Database (Denmark)

    Ghiladi, M; Jensen, K.B.; Jiang, Jianzhong

    1999-01-01

    The dinucleating phenolate-hinged ligand 4-tert-butyl-2,6-bis[bis(2-pyridylmethyl)aminomethyl]phenolate(bpb p) has been used to prepare a series of Fe(III)M(II) complexes containing independent species at the exogenous binding sites. These sites are occupied by fluoride and water ligands and show...... of [(bpbp)Fe(F)2Cu(H2O)][BF4]2-4H2O. The copper(II) and iron(III) atoms are linked asymmetrically by the phenolic oxygen atom hinge of bpbp with Cu-O(phenolato) 2.270(2) and Fe-O(phenolato) 2.041(2) Å with a Cu...Fe distance of 3.828(1) Å. The two terminal fluoride ions are bound to the Fe atom (Fe-F 1.......818(2), 1.902(2) Å) and one of them is strongly hydrogen bonded to the water molecule on the adjacent Cu atom (F-H...O 2.653(4) Å). The metal ions in the aquafluoride complexes [(bpbp)Fe(F)2M(H2O)2][BF4]2, M=Fe or Co, are weakly antiferromagnetically coupled (J=-8 and -10 cm-1 respectively) and in [(bpbp...

  18. Nuclear Magnetic Resonance Characterization of the Type III Secretion System Tip Chaperone Protein PcrG of Pseudomonas aeruginosa.

    Science.gov (United States)

    Chaudhury, Sukanya; Nordhues, Bryce A; Kaur, Kawaljit; Zhang, Na; De Guzman, Roberto N

    2015-11-03

    Lung infection with Pseudomonas aeruginosa is the leading cause of death among cystic fibrosis patients. To initiate infection, P. aeruginosa assembles a protein nanomachine, the type III secretion system (T3SS), to inject bacterial proteins directly into target host cells. An important regulator of the P. aeruginosa T3SS is the chaperone protein PcrG, which forms a complex with the tip protein, PcrV. In addition to its role as a chaperone to the tip protein, PcrG also regulates protein secretion. PcrG homologues are also important in the T3SS of other pathogens such as Yersinia pestis, the causative agent of bubonic plague. The atomic structure of PcrG or any member of the family of tip protein chaperones is currently unknown. Here, we show by circular dichroism and nuclear magnetic resonance (NMR) spectroscopy that PcrG lacks a tertiary structure. However, it is not completely disordered but contains secondary structures dominated by two long α-helices from residue 16 to 41 and from residue 55 to 76. The helices of PcrG are partially formed, have similar backbone dynamics, and are flexible. NMR titrations show that the entire length of PcrG residues from position 9 to 76 is involved in binding to PcrV. PcrG adds to the growing list of partially folded or unstructured proteins with important roles in type III secretion.

  19. Synthesis, Characterization and Thermal Decomposition Studies of Cr(III), Mn(II) and Fe(III) Complexes of N, N '-Bis[1,3-benzodioxol-5-ylmethylene]butane-1,4-diamine

    National Research Council Canada - National Science Library

    Prasad M. Alex; K. K. Aravindakshan

    2009-01-01

    ... (3,4-dioxymethylenebenzaldehyde) with butane-1,4-diamine. Cr(III), Mn(II), Fe(III) complexes of this chelating ligand were synthesised using acetates, chlorides, bromides, nitrates and perchlorates of these metals...

  20. Modeling microstructural evolution of multiple texture components during recrystallization

    DEFF Research Database (Denmark)

    Vandermeer, R.A.; Juul Jensen, D.

    1994-01-01

    Models were formulated in an effort to characterize recrystallization in materials with multiple texture components. The models are based on a microstructural path methodology (MPM). Experimentally the microstructural evolution of conmmercial aluminum during recrystallization was characterized...... using stereological point and lineal measurements of microstructural properties in combination with EBSP analysis for orientation determinations. The potential of the models to describe the observed recrystallization behavior of heavily cold-rolled commercial aluminum was demonstrated. A successful MPM...... model was deduced which, for each texture component-random, rolling and cube orientations, was quantitatively consistent with the measured microstructural properties. Nucleation and growth rates were deduced for each texture component using the model....

  1. Tailored Gallium(III) chelator NOPO: synthesis, characterization, bioconjugation, and application in preclinical Ga-68-PET imaging.

    Science.gov (United States)

    Simeček, Jakub; Zemek, Ondřej; Hermann, Petr; Notni, Johannes; Wester, Hans-Jürgen

    2014-11-03

    The bifunctional chelator NOPO (1,4,7-triazacyclononane-1,4-bis[methylene(hydroxymethyl)phosphinic acid]-7-[methylene(2-carboxyethyl)phosphinic acid]) shows remarkably high Ga(III) complexation efficiency and comprises one carboxylic acid moiety which is not involved into metal ion coordination. An improved synthetic protocol affords NOPO with 45% overall yield. Stepwise protonation constants (log Ka), determined by potentiometry, are 11.96, 5.22, 3.77, and 1.54; the stability constant of the Ga(III) complex is log KGaL = 25.0. Within 5 min, (68)Ga(III) incorporation by NOPO is virtually quantitative at room temperature between pH 3 and 4, and at 95 °C at pH ranging from 0.5 to 7, at NOPO concentrations of 30 μM and 10 μM, respectively. During amide bond formation at the distant carboxylate using the HATU coupling reagent, an intramolecular phosphinic acid ester (phosphilactone) is formed, which is cleaved during (68)Ga complexation or in acidic media, such as trifluoroacetic acid (TFA). Phosphilactone formation can also be suppressed by complexation of Zn(2+) prior to conjugation, the resulting zinc-containing conjugates nevertheless being suitable for direct (68)Ga-labeling. In AR42J (rat pancreatic carcinoma) xenografted CD-1 nude mice, (68)Ga-labeled NOPO-NaI(3)-octreotide conjugate ((68)Ga-NOPO-NOC) showed high and fully blockable tumor uptake (13.9 ± 5% ID/g, 120 min p.i., compared to 0.9 ± 0.4% ID/g with 5 mg/kg of nonlabeled peptide). Uptake in other tissues was generally below 3% ID/g, except appearance of excretion-related activity accumulation in kidneys. NOPO-functionalized compounds tend to be more hydrophilic than the corresponding DOTA- and NODAGA-conjugates, thus promoting fast and extensive renal excretion of (68)Ga-NOPO-radiopharmaceuticals. NOPO-functionalized peptides provide suitable pharmacokinetics in vivo and meet all requirements for efficient (68)Ga-labeling even at room temperature in a kit-like manner.

  2. Synthesis, Characterization, and Catalytic Studies of Mn(III-Schiff Base-Dicyanamide Complexes: Checking the Rhombicity Effect in Peroxidase Studies

    Directory of Open Access Journals (Sweden)

    Manuel R. Bermejo

    2017-01-01

    Full Text Available The condensation of 3-methoxy-2-hydroxybenzaldehyde and the diamines 1,2-diphenylendiamine, 1,2-diamine-2-methylpropane and 1,3-propanediamine yielded the dianionic tetradentate Schiff base ligands N,N′-bis(2-hydroxy-4-methoxybenzylidene-1,2-diphenylendiimine (H2L1, N,N′-bis(2-hydroxy-4-methoxybenzylidene-1,2-diamino-2-methylpropane (H2L2 and N,N′-bis(2-hydroxy-4-methoxybenzylidene-1,3-diaminopropane (H2L3 respectively. The organic compounds H2L1 and H2L2 have been characterized by elemental analysis, IR, 1H and 13C NMR spectroscopies and mass spectrometry electrospray (ES. The crystal structure of H2L2 in solid state, solved by X-ray crystallography, is highly conditioned in the solid state by two N-H•••N intramolecular interactions. The synthesis of three new manganese(III complexes 1–3, incorporating these ligands, H2L1–H2L3, and dicyanamide (DCA, is reported. The complexes 1–3 have been physicochemically characterized by elemental analysis, IR and paramagnetic 1H NMR spectroscopy, ESI mass spectrometry, magnetic moment at room temperature and conductivity measurements. Complex 1 has been crystallographically characterized. The X-ray structure shows the self-assembly of the Mn(III-Schiff base-DCA complex through µ-aquo bridges between neighbouring axial water molecules and also by π-π stacking interactions, establishing a dimeric structure. The manganese complexes were also tested as peroxidase mimics for the H2O2-mediated reaction with the water-soluble trap ABTS, showing complexes 1-2 relevant peroxidase activity in contrast with 3. The rhombicity around the metal ion can explain this catalytic behaviour.

  3. Structural, magnetic, EPR, and electrochemical characterizations of a spin-frustrated trinuclear Cr(III) polyoxometalate and study of its reactivity with lanthanum cations.

    Science.gov (United States)

    Compain, Jean-Daniel; Mialane, Pierre; Dolbecq, Anne; Mbomekallé, Israël Martyr; Marrot, Jérôme; Sécheresse, Francis; Duboc, Carole; Rivière, Eric

    2010-03-15

    The asymmetric Cr(III) polyoxometalate complex Cs(10)[(gamma-SiW(10)O(36))(2)(Cr(OH)(H(2)O))(3)] x 17 H(2)O (1) has been synthesized in water under atmospheric pressure from the trinuclear precursor [Cr(3)(CH(3)COO)(7)(OH)(2)] and the divacant ligand [gamma-SiW(10)O(36)](8-). Complex 1 is built up of two [gamma-SiW(10)O(36)](8-) Keggin units sandwiching a trinuclear {(Cr(III)(OH)(H(2)O))(3)} fragment where the paramagnetic centers are bridged by three mu-OH ligands forming a nearly isosceles triangle. The magnetic properties of this spin-frustrated system have thus been interpreted considering a 2-J Hamiltonian showing that the Cr(III) ions are antiferromagnetically coupled and that 1 possesses an S = 3/2 ground state with an S = 1/2 first excited state located at 11 cm(-1). These results have been confirmed by EPR spectroscopy measurements (Q-band), which have also enabled the quantification of the electronic parameters characterizing the quadruplet spin ground state. The magnitude of the magnetic exchange interactions and the nature of the ground state are discussed in light of previously reported isosceles triangular S = 3/2 clusters. UV-visible and electrochemical studies have shown that 1 is stable in aqueous media in a 1-7 pH range. This stability is chemically confirmed by the study of the reactivity of 1 with La(III) cations, which has allowed the isolation of the Cs(4)[(gamma-SiW(10)O(36))(2)(Cr(OH)(H(2)O))(3)(La(H(2)O)(7))(2)] x 20 H(2)O compound (2). Indeed, during the synthetic process of this 3d-4f system, the integrity of the [(gamma-SiW(10)O(36))(2)(Cr(OH)(H(2)O))(3)](10-) building unit constituting 1 is maintained despite the high oxophilic character of the La(III) ions. The single crystal X-ray diffraction study of 2 has revealed that in the solid state the rare earth cations connect these subunits, affording a 3d-4f double-chain monodimensional system.

  4. Red-luminescent europium (III) doped silica nanoshells: synthesis, characterization, and their interaction with HeLa cells

    Science.gov (United States)

    Yang, Jian; Sandoval, Sergio; Alfaro, Jesus G.; Aschemeyer, Sharraya; Liberman, Alex; Martin, David T.; Makale, Milan; Kummel, Andrew C.; Trogler, William C.

    2011-01-01

    A simple method to fabricate Eu3+ doped silica nanoshells particles with 100 and 200 nm diameters is reported. Amino polystyrene beads were used as templates, and an 8 to 10 nm thick silica gel coating was formed by the sol-gel reaction. After removing the template by calcination, porous dehydrated silica gel nanoshells of uniform size were obtained. The Eu3+ doped silica nanoshells exhibited a red emission at 615 nm on UV excitation. The porous structure of the silica shell wall was characterized by transmission electron microscopy measurements, while particle size and zeta potentials of the particles suspended in aqueous solution were characterized by dynamic light scattering. Two-photon microscopy was used to image the nanoshells after assimilation by HeLa cancer cells. PMID:21721813

  5. Biocatalysis of a Paclitaxel Analogue: Conversion of Baccatin III to N-Debenzoyl-N-(2-furoyl)paclitaxel and Characterization of an Amino Phenylpropanoyl CoA Transferase.

    Science.gov (United States)

    Thornburg, Chelsea K; Walter, Tyler; Walker, Kevin D

    2017-11-07

    In this study, we demonstrate an enzyme cascade reaction using a benzoate CoA ligase (BadA), a modified nonribosomal peptide synthase (PheAT), a phenylpropanoyltransferase (BAPT), and a benzoyltransferase (NDTNBT) to produce an anticancer paclitaxel analogue and its precursor from the commercially available biosynthetic intermediate baccatin III. BAPT and NDTNBT are acyltransferases on the biosynthetic pathway to the antineoplastic drug paclitaxel in Taxus plants. For this study, we addressed the recalcitrant expression of BAPT by expressing it as a soluble maltose binding protein fusion (MBP-BAPT). Further, the preparative-scale in vitro biocatalysis of phenylisoserinyl CoA using PheAT enabled thorough kinetic analysis of MBP-BAPT, for the first time, with the cosubstrate baccatin III. The turnover rate of MBP-BAPT was calculated for the product N-debenzoylpaclitaxel, a key intermediate to various bioactive paclitaxel analogues. MBP-BAPT also converted, albeit more slowly, 10-deacetylbaccatin III to N-deacyldocetaxel, a precursor of the pharmaceutical docetaxel. With PheAT available to make phenylisoserinyl CoA and kinetic characterization of MBP-BAPT, we used Michaelis-Menten parameters of the four enzymes to adjust catalyst and substrate loads in a 200-μL one-pot reaction. This multienzyme network produced a paclitaxel analogue N-debenzoyl-N-(2-furoyl)paclitaxel (230 ng) that is more cytotoxic than paclitaxel against certain macrophage cell types. Also in this pilot reaction, the versatile N-debenzoylpaclitaxel intermediate was made at an amount 20-fold greater than the N-(2-furoyl) product. This reaction network has great potential for optimization to scale-up production and is attractive in its regioselective O- and N-acylation steps that remove protecting group manipulations used in paclitaxel analogue synthesis.

  6. A new strontium antimonate{sup III} Sr{sub 5}Sb{sub 22}O{sub 38}: Synthesis, crystal structure and characterizations

    Energy Technology Data Exchange (ETDEWEB)

    Geng, Lei, E-mail: lgeng.cn@gmail.com [Department of Physics and Electronic Information, Huaibei Normal University, Huaibei, Anhui 235000 (China); Meng, Chang-Yu [Department of Chemistry and Materials, Yulin Normal University, Yulin, Guangxi 537000 (China); Lin, Chen-Sheng [State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fuzhou, Fujian 350002 (China); Cheng, Wen-Dan, E-mail: cwd@fjirsm.ac.cn [State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fuzhou, Fujian 350002 (China)

    2013-07-15

    A new strontium antimonate{sup III}, Sr{sub 5}Sb{sub 22}O{sub 38}, has been hydrothermally synthesized and structurally characterized by single crystal X-ray diffraction. It crystallizes in the P2{sub 1}/n space group of the monoclinic system with a=11.739(9) Å, b=12.014(10) Å, c=16.412(13) Å, β=91.460(8)°, V=2314.0(3) Å{sup 3}. The crystal structure is built of seven trigonal–pyramidal SbO{sub 3} and four sphenoid SbO{sub 4} polyhedra which are connected through sharing corner-oxygen atoms to form the complex three-dimensional {sub ∞}{sup 3}[Sb{sub 22}O{sub 38}]{sup 10−} anionic network with two different intersectant tunnels along the [111-bar ] and [11-bar 1-bar ] directions accommodating the electric charge balanced Sr{sup 2+} cations. First-principles electronic structure calculations based on the density functional theory (DFT) and the UV–vis diffuse reflectance spectroscopy measurements both indicate that the compound belongs to a direct band insulator with an optical gap value of 3.3 eV. - Graphical abstract: The 2D Sb–O slabs are stacked through sharing oxygen atoms to form the 3D network structure of the new strontium antimonate{sup III} Sr{sub 5}Sb{sub 22}O{sub 38}. - Highlights: • A new strontium antimonate{sup III}, Sr{sub 5}Sb{sub 22}O{sub 38}, has been hydrothermally synthesized. • The single crystal structure was determined by X-ray diffraction. • The powder XRD and UV–vis absorption spectroscopy were studied. • Theoretical studies interpret the relationships between optical absorption and crystal structure.

  7. Increasing Heavy Oil Reserves in the Wilmington Oil Field Through Advanced Reservoir Characterization and Thermal Production Technologies, Class III

    Energy Technology Data Exchange (ETDEWEB)

    City of Long Beach; Tidelands Oil Production Company; University of Southern California; David K. Davies and Associates

    2002-09-30

    The objective of this project was to increase the recoverable heavy oil reserves within sections of the Wilmington Oil Field, near Long Beach, California through the testing and application of advanced reservoir characterization and thermal production technologies. The successful application of these technologies would result in expanding their implementation throughout the Wilmington Field and, through technology transfer, to other slope and basin clastic (SBC) reservoirs.

  8. Increasing Heavy Oil Reserves in the Wilmington Oil Field Through Advanced Reservoir Characterization and Thermal Production Technologies, Class III

    Energy Technology Data Exchange (ETDEWEB)

    City of Long Beach; Tidelands Oil Production Company; University of Southern California; David K. Davies and Associates

    2002-09-30

    The objective of this project was to increase the recoverable heavy oil reserves within sections of the Wilmington Oil Field, near Long Beach, California through the testing and application of advanced reservoir characterization and thermal production technologies. It was hoped that the successful application of these technologies would result in their implementation throughout the Wilmington Field and, through technology transfer, will be extended to increase the recoverable oil reserves in other slope and basin clastic (SBC) reservoirs.

  9. α-N-heterocyclic thiosemicarbazone Fe(III) complex: Characterization of its antitumor activity and identification of anticancer mechanism.

    Science.gov (United States)

    Gou, Yi; Wang, Jun; Chen, Shifang; Zhang, Zhan; Zhang, Yao; Zhang, Wei; Yang, Feng

    2016-11-10

    We synthesized an α-N-heterocyclic thiosemicarbazone ligand (L) and its Fe complex (C1) and assessed their chemical and biological properties in order to understand their marked activity. Electrochemical studies and ascorbate oxidation studies demonstrated that C1 shows considerable redox activity, and Fe(III/II) redox potentials was within the range accessible to cellular oxidants and reductants. Absorption spectral, emission spectral and viscosity analysis reveal that L and C1 interacted with DNA through intercalation and C1 exhibited a higher DNA binding ability. Agarose gel electrophoresis experiments indicated that C1 exhibited the highest pBR322 DNA cleaving ability. In vitro, C1 showed significantly more anticancer activity than the ligand alone. Moreover, C1 induces production of reactive oxygen species (ROS) and DNA damage, resulting in activation of the p53 pathway, cell cycle arrest at the S phase, and mitochondria-mediated apoptosis by regulating the expression of Bcl-2 family proteins. Copyright © 2016 Elsevier Masson SAS. All rights reserved.

  10. Characterization of a Novel Polysaccharide-Iron(III) Complex and Its Anti-Anemia and Nonspecific Immune Regulating Activities.

    Science.gov (United States)

    Zhang, Yun; Ma, Fanyi; Zhu, Jinhua; Du, Zuliang; Zhao, Ying-Yong; Liu, Xiuhua

    2017-01-01

    Dioscorea opposita Thunb is the famous food and traditional medicine in China and it was rich in polysaccharides. Polysaccharides of Dioscorea Opposita Thunb possess immunoregulatory activity, free radical scavenging activity and anti-diabetic activity. A novel polysaccharide- iron(III) complex (CYPIC) was synthesized by using crude polysaccharide extracted from Dioscorea opposita Thunb. The component, structure, morphology and molecular weights of CYPIC were analysed, and the anti-anemia, acute toxicity and nonspecific immune regulating activities of CYPIC were assayed. The results showed that CYPIC could increase red blood cell count (RBC), hemoglobin (Hb), hematocrit (HCT), thymus and spleen index of mice with iron deficiency anemia (IDA). Although the structure and deeper mechanisms of CYPIC should be further studied, CYPIC has the potential to be used as an iron supplement for the treatment of iron deficiency anemia. The large scale industrial production was suggested due to the simple preparation processing of CYPIC. Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.

  11. Evaluation of aggregate microstructures following natural regeneration in bauxite residue as characterized by synchrotron-based X-ray micro-computed tomography.

    Science.gov (United States)

    Zhu, Feng; Liao, Jiaxin; Xue, Shengguo; Hartley, William; Zou, Qi; Wu, Hao

    2016-12-15

    Bauxite residue often has poor physical conditions which impede plant growth. Native plant encroachment on a bauxite residue disposal area in Central China reveals that natural regeneration may improve its physicochemical properties. Residue samples collected from three different disposal ages were assessed to evaluate residue micromorphology and three-dimensional (3D) aggregate microstructure under natural regeneration. The residue aggregates in different disposal ages were divided in two sections: macro-aggregate (2-1mm) and micro-aggregate (0.25-0.05mm). Residue aggregate micromorphology was determined by scanning electron microscope and energy dispersive X-ray spectroscopy, and the residue aggregate microstructure was determined by synchrotron-based X-ray micro-computed tomography (SR-μCT) and image analysis techniques. Natural regeneration may improve residue aggregate stability and form a stable aggregate structure. Calcium content increased whilst sodium content decreased significantly on the surface of residue aggregates. Under natural soil-forming processes bauxite residue porosity, specific surface area, average length of paths, and average tortuosity of paths all significantly increased. This demonstrated that natural regeneration may stimulate the formation of stable aggregate structure in residues. Further understanding should focus on particle interaction forces and agglomeration mechanisms with the addition of external ameliorations. Copyright © 2016 Elsevier B.V. All rights reserved.

  12. Characterization of new medium-chain alcohol dehydrogenases adds resolution to duplications of the class I/III and the sub-class I genes.

    Science.gov (United States)

    Cederlund, Ella; Hedlund, Joel; Hjelmqvist, Lars; Jonsson, Andreas; Shafqat, Jawed; Norin, Annika; Keung, Wing-Ming; Persson, Bengt; Jörnvall, Hans

    2011-05-30

    Four additional variants of alcohol and aldehyde dehydrogenases have been purified and functionally characterized, and their primary structures have been determined. The results allow conclusions about the structural and evolutionary relationships within the large family of MDR alcohol dehydrogenases from characterizations of the pigeon (Columba livia) and dogfish (Scyliorhinus canicula) major liver alcohol dehydrogenases. The pigeon enzyme turns out to be of class I type and the dogfish enzyme of class III type. This result gives a third type of evidence, based on purifications and enzyme characterization in lower vertebrates, that the classical liver alcohol dehydrogenase originated by a gene duplication early in the evolution of vertebrates. It is discernable as the major liver form at about the level in-between cartilaginous and osseous fish. The results also show early divergence within the avian orders. Structures were determined by Edman degradations, making it appropriate to acknowledge the methodological contributions of Pehr Edman during the 65 years since his thesis at Karolinska Institutet, where also the present analyses were performed. Copyright © 2011. Published by Elsevier Ireland Ltd.

  13. Graphite nodules in fatigue-tested cast iron characterized in 2D and 3D

    DEFF Research Database (Denmark)

    Mukherjee, Krishnendu; Fæster, Søren; Hansen, Niels

    2017-01-01

    Thick-walled ductile iron casts have been studied by applying (i) cooling rate calculations by FVM, (ii) microstructural characterization by 2D SEM and 3D X-ray tomography techniques and (iii) fatigue testing of samples drawn from components cast in sand molds and metal molds. An analysis has shown...... correlations between cooling rate, structure and fatigue strengths demonstrating the benefit of 3D structural characterization to identify possible causes of premature fatigue failure of ductile cast iron....

  14. Iron(III and copper(II complexes bearing 8-quinolinol with amino-acids mixed ligands: Synthesis, characterization and antibacterial investigation

    Directory of Open Access Journals (Sweden)

    Saliu A. Amolegbe

    2015-09-01

    Full Text Available Four d-orbital metal complexes with mixed ligands derived from 8-hydroxyquinoline (HQ and amino acids (AA: l-alanine and methionine have been synthesized through a mild reflux in alkaline solution and characterized by elemental analyses, infrared, electronic transition, and temperature dependant magnetic susceptibility. The IR spectroscopy revealed that iron and copper ions coordinated through carbonyl (CO, hydroxyl group (OH of the amino acids, N-pyridine ring of hydroxyquinoline. The elemental analysis measurement with other obtained data suggested an octahedral geometry for the iron(III complexes and tetrahedral geometry for the copper(II complexes. From the molar magnetic susceptibility measurement, the iron(III system (S = 5/2 d5 (non-degenerate 6A1 with χmT = 0.38 cm3 Kmol−1 showed an antiferromagnetic while Cu2+ ions system (S = ½ (2T2g has χmT = 4.77 cm3 Kmol−1 described as paramagnetic behaviour. In vitro antimicrobial investigations of the metal complexes against standard bacteria species gave significant inhibition with, copper complex showing highest inhibitions against Pseudomonas aeruginosa (ATCC27853 of 43 mm at 10 μg/ml signalling its potential as pharmaceutical or chemotherapeutic agents.

  15. Ruthenium(III Complexes of Heterocyclic Tridentate (ONN Schiff Base: Synthesis, Characterization and its Biological Properties as an Antiradical and Antiproliferative Agent

    Directory of Open Access Journals (Sweden)

    Ikechukwu P. Ejidike

    2016-01-01

    Full Text Available The current work reports the synthesis, spectroscopic studies, antiradical and antiproliferative properties of four ruthenium(III complexes of heterocyclic tridentate Schiff base bearing a simple 2′,4′-dihydroxyacetophenone functionality and ethylenediamine as the bridging ligand with RCHO moiety. The reaction of the tridentate ligands with RuCl3·3H2O lead to the formation of neutral complexes of the type [Ru(LCl2(H2O] (where L = tridentate NNO ligands. The compounds were characterized by elemental analysis, UV-vis, conductivity measurements, FTIR spectroscopy and confirmed the proposed octahedral geometry around the Ru ion. The Ru(III compounds showed antiradical potentials against 2,2-Diphenyl-1-Picrylhydrazyl (DPPH and 2,2′-azinobis-(3-ethylbenzothiazoline-6-sulfonic acid (ABTS radicals, with DPPH scavenging capability in the order: [(PAEBODRuCl2] > [(BZEBODRuCl2] > [(MOABODRuCl2] > [Vit. C] > [rutin] > [(METBODRuCl2], and ABTS radical in the order: [(PAEBODRuCl2] < [(MOABODRuCl2] < [(BZEBODRuCl2] < [(METBODRuCl2]. Furthermore, in vitro anti-proliferative activity was investigated against three human cancer cell lines: renal cancer cell (TK-10, melanoma cancer cell (UACC-62 and breast cancer cell (MCF-7 by SRB assay.

  16. Synthesis and characterization of μ-hydroxido- and μ-polycarboxylato-bridged iron(III complexes with 2,2’-bipyridine

    Directory of Open Access Journals (Sweden)

    Tasić Nikola

    2014-01-01

    Full Text Available Four novel polymeric iron(III complexes with 2,2’-bipyridine (bipy and different aromatic polycarboxylato ligands as anions of phthalic (pht, isophthalic (ipht, terephthalic (tpht and pyromellitic (pyr acid were synthesized by ligand exchange reaction. The complexes were characterized by elemental and TG/DSC analysis, FTIR and diffuse reflectance UV-VIS-NIR spectroscopy and magnetic susceptibility measurements. Based on analytical and spectral data the formulae of the complexes are {[Fe4(bipy2 (H2O2(OH6(pht3]•2H2O}n (1, {[Fe4(bipy2(Hipht2(ipht2(OH6]•4H2O}n (2, {[Fe4(bipy2(Htpht2(OH6(tpht2]•4H2O}n (3 and {[Fe4(bipy(H2O8(OH4 (pyr2]•H2O}n (4. All complexes are red brown and low-spin with a distorted octahedral geometry and FeO6 or FeN2O4 chromophore. Polycarboxylato ligands have a bridging role in all cases, whereas monodentate COO groups are present in 2 and 3, bridging and chelate COO groups are established in 1 and 4. The thermal behaviour of 1-4 was investigated in detail and the molar dehydration enthalpies were calculated. According to the all those results, the structural formulae of the complexes 1-4 were proposed. [Projekat Ministarstva nauke Republike Srbije, br. III45007

  17. Dynamics characterization of microstructural changes in bars of duplex steels SAF 2205 using the information dimension; Caracterizacion dinamica de los cambios microestructurales en barras de aceros duplex SAF 2205 utilizando la dimension de informacion

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    Rodriguez, E.; Suarez, K.; Amorer, L.; Silva, J.

    2014-04-01

    This study evaluates the ultrasonic signals behavior of a duplex stainless steel SAF 2205 (UNS S31803) after aging treatments at 875 and 950 degree centigrade. The first treatment promotes the precipitation of the sigma phase and the second, its dissolution. The microstructural evaluation was carried out by optical microscopy. The results showed an increase of the sigma phase fraction and the secondary austenite with the time of aging treatment at 875 degree centigrade. On the other hand, increasing the time of treatment at 950 degree centigrade promotes a reduction of the sigma phase and the corresponding increase of the ferrite phase fraction. The study proposed to evaluate in the dynamical system field the influence of microstructural phases in the signals behavior and their dependence on the energy losses occurring in system during heat treatment, by deterministic chaos theory. To accomplish characterization, algorithm employs the representation of dynamic phase space and the information dimension estimate. The results show a higher correlation between the information dimension and the attenuation coefficient in comparison with the phase fractions. However, the efficiency of this type of study will depend on the frequency selected for the evaluation of the material. (Author)