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Sample records for paranitrophenol-an xrd tem

  1. Changes in the surfaces on DDOAB organoclays adsorbed with paranitrophenol-An XRD, TEM and TG study

    SciTech Connect

    Zhou Qin; He Hongping; Frost, Ray L. Xi Yunfei

    2008-12-01

    The adsorption of paranitrophenol on organoclays synthesised by the ion exchange of the surfactant molecule dimethyldioctadecylammonium bromide (DDOAB) of formula (CH{sub 3}(CH{sub 2}){sub 17}){sub 2}NBr(CH{sub 3}){sub 2} has been studied by X-ray diffraction (XRD), transmission electron microscopy (TEM) and thermogravimetric analysis. The expansion of the montmorillonite depends on the loading of the montmorillonite with dimethyldioctadecylammonium bromide and is related to the arrangement of the surfactant molecules within the clay interlayer. This expansion is altered by the adsorbed paranitrophenol and is observed in the transmission electron microscopic images of the organoclay with adsorbed paranitrophenol. Changes in the surfactant molecular arrangements were analysed by thermogravimetry. The paranitrophenol is sublimed simultaneously with the loss of surfactant. The dehydroxylation temperature of the montmorillonite is decreased upon adsorption of the paranitrophenol indicating a bonding between the paranitrophenol and the hydroxyl units of the montmorillonite.

  2. Characterization of crystallite morphology for doped strontium fluoride nanophosphors by TEM and XRD

    NASA Astrophysics Data System (ADS)

    O'Connell, J. H.; Lee, M. E.; Yagoub, M. Y. A.; Swart, H. C.; Coetsee, E.

    2016-01-01

    Crystallite morphology for Eu-doped and undoped SrF2 nanophosphors have been determined by X-ray diffraction (XRD) and transmission electron microscopy (TEM). The values for average crystallite size obtained by the application of the Scherrer equation and the full width at half maximum (FWHM) values for XRD peaks are compared to the results obtained using the hollow cone dark field (HCDF) TEM imaging technique. In the case of the TEM analysis, a bimodal crystallite size distribution was revealed with one of the distributions having a measured range of crystallite sizes which was in good agreement with the XRD data. HCDF in combination with FIB specimen preparation was found to be a promising technique for the determination of crystallite size distributions in nanophosphors which might facilitate a better understanding of their scintillation properties.

  3. TEM, XRD and nanoindentation characterization of Xenon ion irradiation damage in austenitic stainless steels

    NASA Astrophysics Data System (ADS)

    Huang, H. F.; Li, J. J.; Li, D. H.; Liu, R. D.; Lei, G. H.; Huang, Q.; Yan, L.

    2014-11-01

    Cross-sectional and bulk specimens of a 20% cold-worked 316 austenitic stainless steel (CW 316 SS) has been characterized by TEM, XRD and nanoindentation to determine the microstructural evolution and mechanical property changes of 316 SS after irradiation with 7 MeV Xe26+ ions. TEM results reveal the presence of dislocation loops with a number density of approximately 3 × 1022 m-3 and sizes between 3 to 10 nm due to the collapse of vacancy rich cores inside displacement cascades. Peak broadening observed in XRD diffraction patters reveal systematic changes to lattice parameters due to irradiation. The calculated indentation values in irradiated 316 SS were found to be much higher in comparison to the unirradiated specimen, indicating the dose dependent effect of irradiation on hardness. The relationship between irradiation induced microstructural evolution and the changes to the mechanical properties of CW 316 SS are discussed in the context of fluence and irradiation temperature.

  4. XRD, TEM, IR, Raman and NMR Spectroscopy of In Situ Crystallization of Lithium Disilicate Glass

    NASA Technical Reports Server (NTRS)

    Fuss, T.; Mogus-Milankovic, A.; Ray, C. S.; Lesher, C. E.; Youngman, R.; Day, D. E.

    2006-01-01

    The structure of a Li2O-2SiO2 (LS2) glass was investigated as a function of pressure and temperature up to 6 GPa and 750 C respectively, using XRD, TEM, IR, Raman and NMR spectroscopy. Glass densified at 6 GPa has an average Si-O-Si bond angle approx.7deg lower than that found in glass processed at 4.5 GPa. At 4.5 GPa, lithium disilicate crystallizes from the glass, while at 6 GPa a new high pressure form of lithium metasilicate crystallizes. The new phase, while having lithium metasilicate crystal symmetry, contains at least 4 different Si sites. NMR results for 6 GPa sample indicate the presence of Q4 species with (Q(sup 4))Si-O-Si(Q(sup 4)) bond angles of approx.157deg. This is the first reported occurrence of Q(sup 4) species with such large bond angles in alumina free alkali silicate glass. No five- or six- coordinated Si are found.

  5. Swelling induced by alpha decay in monazite and zirconolite ceramics: A XRD and TEM comparative study

    NASA Astrophysics Data System (ADS)

    Deschanels, X.; Seydoux-Guillaume, A. M.; Magnin, V.; Mesbah, A.; Tribet, M.; Moloney, M. P.; Serruys, Y.; Peuget, S.

    2014-05-01

    Zirconolite and monazite matrices are potential ceramics for the containment of actinides (Np, Cm, Am, Pu) which are produced over the reprocessing of spent nuclear fuel. Actinides decay mainly through the emission of alpha particles, which in turn causes most ceramics to undergo structural and textural changes (amorphization and/or swelling). In order to study the effects of alpha decays on the above mentioned ceramics two parallel approaches were set up. The first involved the use of an external irradiation source, Au, which allowed the deposited recoil energy to be simulated. The second was based on short-lived actinide doping with 238Pu, (i.e. an internal source), via the incorporation of plutonium oxide into both the monazite and zirconolite structures during synthesis. In both types of irradiation experiments, the zirconolite samples became amorphous at room temperature with damage close to 0.3 dpa; corresponding to a critical dose of 4 × 1018 α g-1 (i.e. ∼1.3 × 1021 keV cm-3). Both zirconolite samples also showed the same degree of macroscopic swelling at saturation (∼6%), with ballistic processes being the predominant damaging effect. In the case of the monazite however, the macroscopic swelling and amorphization were dependent on the nature of the irradiation. Externally, (Au), irradiated samples became amorphous while also demonstrating a saturation swelling of up to 8%. In contrast to this, the swelling of the 238Pu doped samples was much smaller at ∼1%. Also, unlike the externally (Au) irradiated monazite these 238Pu doped samples remained crystalline up to 7.5 × 1018 α g-1 (0.8 dpa). XRD, TEM and swelling measurements were used to fully characterize and interpret this behavior. The low swelling and the conservation of the crystalline state of 238Pu doped monazite samples indicates that alpha annealing took place within this material.

  6. Swelling of ion-irradiated 3C-SiC characterized by synchrotron radiation based XRD and TEM

    NASA Astrophysics Data System (ADS)

    Lin, Yan-Ru; Ho, Chun-Yu; Chuang, Wei-Tsung; Ku, Ching-Shun; Kai, Ji-Jung

    2014-12-01

    An experimental technique was established to characterize irradiation-induced volume swelling through a combined utilization of synchrotron radiation-based X-ray diffraction (XRD) and transmission electron microscopy (TEM). 3C-SiC specimens were irradiated by Si2+ ions (5 MeV) with fluences up to 5 × 1017 ion/cm2 at 1000 °C. In order to avoid the accumulation of implanted Si ions in the SiC layer, specific thicknesses of the epitaxy layer and implanted ion energy were chosen. Unresolvable black spot defects were studied by TEM, and the average size and density were calculated. XRD radial scan results of surface (0 0 2), (1 1 1), (0 2 2), (1 1 3), and (2 0 0) including peak shift and asymmetry peak broadening were observed. Different interplanar spacing information of single crystal SiC can be obtained from this XRD measurement method, making it possible to investigate the lattice expansion and volume swelling more precisely. While TEM provided a direct visualization of the microstructures and the interplanar spacing was measured from HRTEM images. It is suggested that irradiation induced point defects and compressive stress from the Si substrate were the cause of anisotropic (a = b < c) volume swelling of irradiated 3C-SiC in this study.

  7. Mössbauer, TEM/SAED and XRD investigation on waste dumps of the Valea lui Stan gold mines

    NASA Astrophysics Data System (ADS)

    Constantinescu, Serban Grigore; Udubasa, Sorin S.; Udubasa, Gheorghe; Kuncser, Victor; Popescu-Pogrion, Nicoleta; Mercioniu, Ionel; Feder, Marcel

    2012-03-01

    The complementary investigation techniques, Mössbauer spectroscopy, transmission electron microscopy with selected area electron diffraction (TEM/SAED), X-ray diffraction (XRD) have been used to investigate the fate of the Valea lui Stan, Romania, gold-ore nanoscale-minerals during the long time of residence in the waste dumps. The preliminary investigations showed such waste dumps to contain significant amount of metals which cannot be identified by conventional methods. An intense research activity started up in order to evaluate the possibilities to recycle Valea lui Stan waste dumps and to recover metals by chemical or phytoextraction procedures. The waste dumps naturally show different mineral constituents with clay minerals as major phases, observed by XRD-technique. Although the waste dumps materials have whitish-yellowish colours, MÖSSBAUER technique evidences the presence of the finely dispersed iron bearing minerals. The authors are focusing to inspect and analyze Fe-compounds in the samples collected from Valea lui Stan's waste dumps in order to identify the magnetic phases by Mössbauer technique.

  8. NGR, XRD and TEM/SAED investigations on waste dumps materials with a view to recover precious metals

    NASA Astrophysics Data System (ADS)

    Udubasa, S. S.; Constantinescu, S.; Popescu-Pogrion, N.; Feder, M.; Udubasa, G.

    2010-03-01

    Two types of ores were selected for the investigation of the fate of the ore minerals during relatively long time of residence in the waste dumps (active mining: 25 years ago in the Badeanca Valley and some 50 years ago in the Valea lui Stan area). The pentametallic ores (Co-Ni-Bi-Ag-U) in the Leaota Mts. contain a great number of primary minerals of Cu, As etc. Although the waste dumps materials have whitish-yellowish colors their NGR spectra show the presence of iron minerals very finely dispersed. In the gold ores of Valea lui Stan deposit numerous minerals were identified, such as arsenopyrite, pyrite, pyrrhotite, etc., as major gold bearing sulfides. The waste dumps materials naturally show different mineral constituents, with clay minerals as major phases. Detailed NGR investigations show however Mössbauer spectra pointing out the presence of finely dispersed iron or iron-bearing minerals. Under supergene conditions gold is commonly sequestrated by iron hydroxydes; further TEM/SAED and XRD investigations are contributing to localize the gold. In some samples Mössbauer spectra resembling those of greigite have been obtained. Greigite is also a principal concentrator of gold under supergene conditions.

  9. Formation of TEM- and XRD-undetectable gold clusters accompanying big gold particles on TiO 2-SiO 2 supports

    NASA Astrophysics Data System (ADS)

    Bogdanchikova, N.; Pestryakov, A.; Farias, M. H.; Diaz, J. A.; Avalos, M.; Navarrete, J.

    2008-07-01

    Sol-gel method allows obtaining complex Ti-Si oxide supports possessing the effect of strong metal-support interaction and favouring the stabilisation of gold in the form of small charged gold clusters. TEM and XRD measurements show the samples containing big gold particles with average size more than 90 nm. However, Rietveld XRD refinement revealed a very low (≤5%) relative amount of large particles on mixed oxide supports. Highly dispersed gold species undetectable by XRD and TEM on TiSi supports provide the main contribution to total amount of gold due to extremely high surface area of these mixed oxides. The combination of DRS, Rietveld XRD analysis and XPS methods was effective for registration and characterisation of these dispersed gold species. The formation of such gold species should be taken into account when studying the nature of gold active sites, as they can be the participants of the catalytic process instead of TEM-detectable metal particles or along with them.

  10. Crystal structure of La 0.4Sr 0.6CoO 2.71 investigated by TEM and XRD

    NASA Astrophysics Data System (ADS)

    Gspan, C.; Grogger, W.; Bitschnau, B.; Bucher, E.; Sitte, W.; Hofer, F.

    2008-11-01

    The structure of the oxygen-deficient perovskite La 0.4Sr 0.6CoO 3-δ ( δ=0.29) was investigated by transmission electron microscopy (TEM) and X-ray powder diffraction (XRD). Domains between 50 and 250 nm in size were observed in the electron microscope. Weak superstructure reflections were found with both X-ray and electron diffraction. Investigations of these superstructure reflections by selected area electron diffraction (SAED) and convergent beam electron diffraction (CBED) showed that the domains in a crystal are orientated in a 90° relationship. High-resolution transmission electron microscopy (HRTEM) images from the domain boundary also revealed a 90° orientation dependency. Using the symmetry of CBED patterns, the point group 4/ mmm was determined. By comparing reflections from the SAED pattern with possible reflections, the space group I4/ mmm (No. 139) could be isolated and finally the crystal structure was refined by Rietveld refinement.

  11. Crystal structure of La{sub 0.4}Sr{sub 0.6}CoO{sub 2.71} investigated by TEM and XRD

    SciTech Connect

    Gspan, C. Grogger, W.; Bitschnau, B.; Bucher, E.; Sitte, W.; Hofer, F.

    2008-11-15

    The structure of the oxygen-deficient perovskite La{sub 0.4}Sr{sub 0.6}CoO{sub 3-{delta}} ({delta}=0.29) was investigated by transmission electron microscopy (TEM) and X-ray powder diffraction (XRD). Domains between 50 and 250 nm in size were observed in the electron microscope. Weak superstructure reflections were found with both X-ray and electron diffraction. Investigations of these superstructure reflections by selected area electron diffraction (SAED) and convergent beam electron diffraction (CBED) showed that the domains in a crystal are orientated in a 90 deg. relationship. High-resolution transmission electron microscopy (HRTEM) images from the domain boundary also revealed a 90 deg. orientation dependency. Using the symmetry of CBED patterns, the point group 4/mmm was determined. By comparing reflections from the SAED pattern with possible reflections, the space group I4/mmm (No. 139) could be isolated and finally the crystal structure was refined by Rietveld refinement. - Graphical abstract: Two adjacent domains show different orientation of the c-axis of the tetragonal unit cell in the according convergent beam electron diffraction patterns.

  12. Alteration history of mudrock samples from the San Andreas Fault Observatory at Depth (SAFOD) drill hole: a TEM-XRD study

    NASA Astrophysics Data System (ADS)

    Schleicher, A. M.; van der Pluijm, B. A.; Warr, L. N.

    2006-12-01

    Studying rock alteration in active fault zones is key to understanding fault history and the interaction with mechanical, hydrological and mineralogical processes. In the SAFOD mudrocks at 3064 and 3436 m depths, abundant clay mineral phases, including mixed-layered varieties, occur in the matrix. At present, little is known about the mechanism and timing of their formation in relation to the faulting process. Based on a detailed TEM-XRD study, a preliminary assessment of the alteration history of the clay-rich rock chips is made by studying mineral character, hydration behavior, fabric and textural relationships. The mudrocks contain detrital grains of chlorite, muscovite and biotite, along with a range of authigenic illite, illite-smectite, chlorite- smectite and smectite. The predominant clay minerals are small illite packets (20-30 nm thickness) of a 1Md polytype. The illite constitutes about 75 percent of the illite-smectite mixed layer particles, showing a long- range ordering (R greater than 3). These authigenic mineral phases are probably formed during the movement of aqueous fluids along permeable fractures and veins by dissolution-precipitation reactions, and partly at the expense of larger (about 150 nm thick), deformed, detrital packets. The chlorite-smectite mixed layered phases formed via similar mechanisms, but in this case by direct alteration of detrital chlorite and biotite grains. Preliminary DTA heat flow results from a whole rock mudstone indicate a total loss of about 6 percent of total volatiles (about 2 percent interlayer water, about 4 percent crystalline water), most of which occurs during the dehydroxylation of clays (400-600 C). The timing of authigenic mineral growth in the matrix assemblages is considered to be coeval or older than localized mineralization along open fractures. The fracture precipitations are notably smectite rich and can be taken as an indication of more recent low temperature fluids of varying composition or more

  13. Temperature-dependent XRD, IR, magnetic, SEM and TEM studies of Jahn–Teller distorted NiCr{sub 2}O{sub 4} powders

    SciTech Connect

    Ptak, M. Maczka, M.; Gągor, A.; Pikul, A.; Macalik, L.; Hanuza, J.

    2013-05-15

    In the present work we report detailed structural, magnetic and phonon properties of NiCr{sub 2}O{sub 4} powders synthesized via a simple coprecipitation method. Temperature-dependent XRD as well as temperature-dependent IR studies reveal that cubic to tetragonal phase transition is lowered due to size effects. Observed changes in the IR spectra indicate that the paramagnetic–ferrimagnetic phase transition taking place at 74 K is related to further lowering of symmetry to orthorhombic system. Assignment of modes was proposed and factor group analyses in three possible symmetries were carried out. Our results show strong anomalies due to the Jahn–Teller tetragonal distortion and weak due to the orthorhombic distortion and onset of collinear ferrimagnetic order. Shifts of wavenumbers observed below 31 K, where the onset of antiferromagnetic ordering occurs, were attributed to spin–phonon interactions. - Graphical abstract: XRD pattern of NiCr{sub 2}O{sub 4} sample synthesized via a coprecipitation method followed by calcination at 1000 {sup o}C. - Highlights: • NiCr{sub 2}O{sub 4} starts to crystallize near 750 °C. • Coexistence of cubic and tetragonal phases of NiCr{sub 2}O{sub 4} was revealed. • Temperature of the Jahn–Teller distortion is lowered due to the size effects. • Evidences of tetragonal and orthorhombic distortions were found. • Weak spin–phonon interactions were evidenced.

  14. Temperature-dependent XRD, IR, magnetic, SEM and TEM studies of Jahn-Teller distorted NiCr2O4 powders

    NASA Astrophysics Data System (ADS)

    Ptak, M.; Maczka, M.; Gągor, A.; Pikul, A.; Macalik, L.; Hanuza, J.

    2013-05-01

    In the present work we report detailed structural, magnetic and phonon properties of NiCr2O4 powders synthesized via a simple coprecipitation method. Temperature-dependent XRD as well as temperature-dependent IR studies reveal that cubic to tetragonal phase transition is lowered due to size effects. Observed changes in the IR spectra indicate that the paramagnetic-ferrimagnetic phase transition taking place at 74 K is related to further lowering of symmetry to orthorhombic system. Assignment of modes was proposed and factor group analyses in three possible symmetries were carried out. Our results show strong anomalies due to the Jahn-Teller tetragonal distortion and weak due to the orthorhombic distortion and onset of collinear ferrimagnetic order. Shifts of wavenumbers observed below 31 K, where the onset of antiferromagnetic ordering occurs, were attributed to spin-phonon interactions.

  15. TEM Video Compressive Sensing

    SciTech Connect

    Stevens, Andrew J.; Kovarik, Libor; Abellan, Patricia; Yuan, Xin; Carin, Lawrence; Browning, Nigel D.

    2015-08-02

    One of the main limitations of imaging at high spatial and temporal resolution during in-situ TEM experiments is the frame rate of the camera being used to image the dynamic process. While the recent development of direct detectors has provided the hardware to achieve frame rates approaching 0.1ms, the cameras are expensive and must replace existing detectors. In this paper, we examine the use of coded aperture compressive sensing methods [1, 2, 3, 4] to increase the framerate of any camera with simple, low-cost hardware modifications. The coded aperture approach allows multiple sub-frames to be coded and integrated into a single camera frame during the acquisition process, and then extracted upon readout using statistical compressive sensing inversion. Our simulations show that it should be possible to increase the speed of any camera by at least an order of magnitude. Compressive Sensing (CS) combines sensing and compression in one operation, and thus provides an approach that could further improve the temporal resolution while correspondingly reducing the electron dose rate. Because the signal is measured in a compressive manner, fewer total measurements are required. When applied to TEM video capture, compressive imaging couled improve acquisition speed and reduce the electron dose rate. CS is a recent concept, and has come to the forefront due the seminal work of Candès [5]. Since the publication of Candès, there has been enormous growth in the application of CS and development of CS variants. For electron microscopy applications, the concept of CS has also been recently applied to electron tomography [6], and reduction of electron dose in scanning transmission electron microscopy (STEM) imaging [7]. To demonstrate the applicability of coded aperture CS video reconstruction for atomic level imaging, we simulate compressive sensing on observations of Pd nanoparticles and Ag nanoparticles during exposure to high temperatures and other environmental

  16. TEM turbulence optimisation in stellarators

    NASA Astrophysics Data System (ADS)

    Proll, J. H. E.; Mynick, H. E.; Xanthopoulos, P.; Lazerson, S. A.; Faber, B. J.

    2016-01-01

    With the advent of neoclassically optimised stellarators, optimising stellarators for turbulent transport is an important next step. The reduction of ion-temperature-gradient-driven turbulence has been achieved via shaping of the magnetic field, and the reduction of trapped-electron mode (TEM) turbulence is addressed in the present paper. Recent analytical and numerical findings suggest TEMs are stabilised when a large fraction of trapped particles experiences favourable bounce-averaged curvature. This is the case for example in Wendelstein 7-X (Beidler et al 1990 Fusion Technol. 17 148) and other Helias-type stellarators. Using this knowledge, a proxy function was designed to estimate the TEM dynamics, allowing optimal configurations for TEM stability to be determined with the STELLOPT (Spong et al 2001 Nucl. Fusion 41 711) code without extensive turbulence simulations. A first proof-of-principle optimised equilibrium stemming from the TEM-dominated stellarator experiment HSX (Anderson et al 1995 Fusion Technol. 27 273) is presented for which a reduction of the linear growth rates is achieved over a broad range of the operational parameter space. As an important consequence of this property, the turbulent heat flux levels are reduced compared with the initial configuration.

  17. Evolution of extended defects in polycrystalline UO2 under heavy ion irradiation: combined TEM, XRD and Raman study

    NASA Astrophysics Data System (ADS)

    Onofri, C.; Sabathier, C.; Palancher, H.; Carlot, G.; Miro, S.; Serruys, Y.; Desgranges, L.; Legros, M.

    2016-05-01

    A well-suited way to understand the behavior under irradiation of the UO2 nuclear fuel is to use ion implantations and further analyze the microstructure. The present work is focused on the characteristics of extended defects created by Kr implantations in UO2 polycrystals. The influence of many parameters on these extended defects has been studied separately: irradiation temperature (room temperature, 500 and 600 °C), ion fluence (5 × 1015 and 1.26 × 1017 i/cm2), ion energy (4 and 27 MeV) and conditions of subsequent thermal annealing. The evolution of extended defects characteristics and density was determined using transmission electron microscopy and additional damage characterizations were performed by X-ray diffraction and Raman spectroscopy. Results obtained by the different analytical techniques are shown to be in excellent agreement and to complement literature data. In addition, this work presents the extended defect transformation induced by fluence (dislocation loops and lines → tangled dislocation network) and shows that temperature influences directly their evolution kinetics. Moreover we demonstrate that the temperature to allow extended defects mobility is different during irradiation and under thermal annealing conditions. Finally dislocation line density and swelling obtained from this study are found in the same order of magnitude as the ones obtained from in pile irradiations.

  18. Characterization of magnetite in silico-aluminous fly ash by SEM, TEM, XRD, magnetic susceptibility, and Moessbauer spectroscopy

    SciTech Connect

    Gomes, S.; Francois, M.; Abdelmoula, M.; Refait, P.; Pellissier, C.; Evrard, O.

    1999-11-01

    Spinel magnetite contained in a silico-aluminous fly ash (originating from la Maxe's power plant, near Metz in the east of France) issued from bituminous coal combustion has been studied by scanning and transmission electron microscopy linked with energy dispersive spectroscopy. X-ray diffraction, susceptibility measurements, and Moessbauer spectroscopy. The results show that in this magnetite Mg is strongly substituted for Fe and the chemical formula is closer to MgFe{sub 2}O{sub 4} than Fe{sub 3}O{sub 4}. Magnetite also contains Mn, Ca, and Si elements, but at a lower proportion. The results are compatible with the chemical formula Fe{sub 2.08}Mg{sub 0.75}Mn{sub 0.11}Ca{sub 0.04}Si{sub 0.02}O{sub 4} and crystallochemical formula [Fe{sup 2{minus}}{sub 0.92}Ca{sup 2+}{sub 0.06}Si{sup 4+}{sub 0.02}]{sup tetra}[Fe{sup 3+}Fe{sup 2+}{sub 0.16}Mg{sup 2+}{sub 0.73}Mn{sup 2+}{sub 0.11}]{sup octa}O{sub 4}, showing the cation distribution on octahedral and tetrahedral sites of the spinel structure. The reason Mg element is not incorporated in soluble surface salt and in glass composition of the silico-aluminous fly ashes is now understood.

  19. Cluster formation, evolution and size distribution in Fe-Cu alloy: Analysis by XAFS, XRD and TEM

    NASA Astrophysics Data System (ADS)

    Cammelli, S.; Degueldre, C.; Cervellino, A.; Abolhassani, S.; Kuri, G.; Bertsch, J.; Lützenkirchen-Hecht, D.; Frahm, R.

    2010-03-01

    Fe-Cu alloys containing 1.3 at.% copper were studied as model systems for cluster formation in reactor pressure vessel steels. The samples were annealed at 775 K for different times and subsequently analyzed using X-ray absorption fine structure spectroscopy at the Cu-K-edge, X-ray diffraction and transmission electron microscopy. The results show that copper cluster formation might occur even with short annealing times. These clusters of about 1 nm size can switch easily from bcc iron-like structures to fcc copper, if the local copper concentration is high enough. While a short annealing time of 2.5 h at 775 K maintains a good dilution of copper in the bcc iron matrix, annealing for 312 h leads to large fcc copper precipitates. A linear combination analysis suggests that in the sample annealed 8 h, copper clusters are mostly formed with the same structure as the matrix. A co-existence of bcc and fcc clusters is obtained for 115 h of annealing. Transmission electron microscopy indicates the presence of precipitates as large as 60 nm size for an annealing time of 312 h, and X-ray diffraction provided complementary data about the clusters size distributions in all of the four samples.

  20. Technical Evaluation Motor No. 7 (TEM-7)

    NASA Technical Reports Server (NTRS)

    Hughes, Phil

    1991-01-01

    The Technical Evaluation Motor No. 7 (TEM-7) test was a full-scale, full duration static test firing of a high performance motor-configuration solid rocket motor with nozzle vectoring. The final test report documents the procedures, performance, and results of the static test firing of TEM-7. All observations, discussions, conclusions, and recommendations included in the report are complete and final except for the TEM-7 fixed housing unbond investigation. A presentation and discussion of TEM-7 performance, anomalies, and test result concurrence with the objectives outlined in CTP-0107, Rev A, Space Shuttle Technical Evaluation Motor No. 7 (TEM-7) Static Fire Test Plan are included.

  1. Technical Evaluation Motor No. 10 (TEM-10)

    NASA Technical Reports Server (NTRS)

    1993-01-01

    Technical Evaluation Motor No. 10 (TEM-10) was static fired on 27 Apr. 1993 at the Thiokol Corporation full-scale motor static test bay, T-24. This final test report documents the procedures, performance, and results of the static test firing of TEM-10. All observations, discussions, conclusions, and recommendations contained are final. Included is a presentation and discussion of TEM-10 performance, anomalies, and test results in concurrence with the objectives outlined in CTP-0110, Revision D, Space Shuttle Technical Evaluation Motor No. 10 (TEM-10) Static Fire Test Plan.

  2. Technical Evaluation Motor no. 5 (TEM-5)

    NASA Technical Reports Server (NTRS)

    Cook, M.

    1990-01-01

    Technical Evaluation Motor No. 5 (TEM-5) was static test fired at the Thiokol Corporation Static Test Bay T-97. TEM-5 was a full scale, full duration static test fire of a high performance motor (HPM) configuration solid rocket motor (SRM). The primary purpose of TEM static tests is to recover SRM case and nozzle hardware for use in the redesigned solid rocket motor (RSRM) flight program. Inspection and instrumentation data indicate that the TEM-5 static test firing was successful. The ambient temperature during the test was 41 F and the propellant mean bulk temperature (PMBT) was 72 F. Ballistics performance values were within the specified requirements. The overall performance of the TEM-5 components and test equipment was nominal. Dissembly inspection revealed that joint putty was in contact with the inner groove of the inner primary seal of the ignitor adapter-to-forward dome (inner) joint gasket; this condition had not occurred on any previous static test motor or flight RSRM. While no qualification issues were addressed on TEM-5, two significant component changes were evaluated. Those changes were a new vented assembly process for the case-to-nozzle joint and the installation of two redesigned field joint protection systems. Performance of the vented case-to-nozzle joint assembly was successful, and the assembly/performance differences between the two field joint protection system (FJPS) configurations were compared.

  3. Technical Evaluation Motor No. 7 (TEM-07)

    NASA Technical Reports Server (NTRS)

    Hugh, Phil

    1991-01-01

    Technical Evaluation Motor Number 7 (TEM-7) was a full scale, full-duration static test firing of a high performance motor (HPM) configuration solid rocket motor (SRM) with nozzle vectoring. The static test fire occurred on 11 December 1990 at the Thiokol Corporation Static Test Bay T-97. Documented here are the procedures, performance, and results available through 22 January 1991. Critical post test hardware activities and assessment of the test data are not complete. A completed test report will be submitted 60 days after the test date. Included here is a presentation and discussion of the TEM-7 performance, anomalies, and test result concurrence with the objectives outlined in CTP-0107 Revision A, Space Shuttle Technical Evaluation Motor number 7 (TEM-07) Static Fire Test Plan.

  4. Analysis of Open TEM-Waveguide Structures

    NASA Astrophysics Data System (ADS)

    Rambousky, R.; Garbe, H.

    This work belongs to a research project on the analysis and characterization of higher order modes occurring in open TEM-waveguide structures. An open TEM waveguide, derived from a conventional GTEM cell by removing the sidewalls, is investigated. The intrinsic resonances of the electromagnetic field occurring in the test volume of the waveguide are analyzed in frequency domain by computer simulation and measurement. This resonance behavior is compared to that of more simplified wire models, describing just the planar septum of the original TEM waveguide. The influence of the number of wires used in the wire model is investigated with respect to the resonant behavior. The use of wire structures is a prerequisite for application of transmission-line super theory (TLST) for further analysis.

  5. TEM-nanoindentation studies of semiconducting structures.

    PubMed

    Le Bourhis, E; Patriarche, G

    2007-01-01

    This paper reviews the application of nanoindentation coupled with transmission electron microscopy (TEM) to investigations of the plastic behaviour of semiconducting structures and its implication for device design. Instrumented nanoindentation has been developed to extract the mechanical behaviour of small volumes scaled to those encountered in semiconductor heterostructures. We illustrate that TEM is a powerful complementary tool for the study of local plasticity induced by nanoindentation. TEM-nanoindentation allows for detailed understanding of the plastic deformation in semiconducting structures and opens practical routes for improvement of devices. Performances of heterostructures are deteriously affected by dislocations that relax the lattice mismatched layers. Different ways to obtain compliant substructures are being developed in order to concentrate the plastic relaxation underneath the heterostructure. Such approaches allow for mechanical design of micro- and opto-electronic devices to be considered throughout the fabrication process. PMID:16901706

  6. Simple XRD algorithm for direct determination of cotton crystallinity

    NASA Astrophysics Data System (ADS)

    Liu, Yongliang; Thibodeaux, Devron; Gamble, Gary; Bauer, Philip; VanDerveer, Don

    2012-06-01

    Traditionally, XRD had been used to study the crystalline structure of cotton celluloses. Despite considerable efforts in developing the curve-fitting protocol to evaluate the crystallinity index (CI), in its present state, XRD measurement can only provide a qualitative or semi-quantitative assessment of the amounts of crystalline and amorphous cellulosic components in a sample. The greatest barrier to establish quantitative XRD is the lack of appropriate cellulose standards needed to calibrate the measurements. In practical, samples with known CIs are very difficult to be prepared or determined. As an approach, we might assign the samples with reported CIs from FT-IR procedure, in which the threeband ratios were first calculated and then were converted into CIs within a large and diversified pool of cotton fibers. This study reports the development of simple XRD algorithm, over time-consuming and subjective curve-fitting process, for direct determination of cotton cellulose CI by correlating XRD with the FT-IR CI references.

  7. Silver Trees: Chemistry on a TEM Grid

    EPA Science Inventory

    The copper/carbon substrate of a TEM grid reacted with aqueous silver nitrate solution within minutes to yield spectacular tree-like silver dendrites, without using any added capping or reducing reagents. These results demonstrate a facile, aqueous, room temperature synthesis of...

  8. Test for English Majors (TEM) in China

    ERIC Educational Resources Information Center

    Jin, Yan; Fan, Jinsong

    2011-01-01

    The purpose of the Test for English Majors (TEM) is to measure the English proficiency of Chinese university undergraduates majoring in English Language and Literature and to examine whether these students meet the required levels of English language abilities as specified in the National College English Teaching Syllabus for English Majors…

  9. LLNL Workshop on TEM of Pu

    SciTech Connect

    King, W.E.

    1996-09-10

    On Sept. 10, 1996, LLNL hosted a workshop aimed at answering the question: Is it possible to carry out transmission electron microscopy (TEM) on plutonium metal in an electron microscope located outside the LLNL plutonium facility. The workshop focused on evaluation of a proposed plan for Pu microscopy both from a technical and environment, health, and safety point of view. After review and modification of the plan, workshop participants unanimously concluded that: (1) the technical plan is sound, (2) this technical plan, including a proposal for a new TEM, provides significant improvements and unique capabilities compared with the effort at LANL and is therefore complementary, (3) there is no significant environment, health, and safety obstacle to this plan.

  10. FTIR and XRD study of PMMA/PCTFE blend films

    SciTech Connect

    Tripathi, S. Shripathi, T.; Tripathi, J.; Agrawal, A.; Sharma, A.

    2014-04-24

    The results are reported on solution cast PMMA-PCTFE blend films characterized using x-ray diffraction and FTIR. The nanocrystalline nature of PMMA is still seen in the blends, however, the bond modifications are clearly observed. The addition of PCTFE results in the modification in structural properties, as reflected in the XRD and FTIR spectra showing modifications in bonding as a function of PCTFE percentage.

  11. Technical Evaluation Motor 3 (TEM-3)

    NASA Technical Reports Server (NTRS)

    Garecht, Diane

    1989-01-01

    A primary objective of the technical evaluation motor program is to recover the case, igniter and nozzle hardware for use on the redesigned solid rocket motor flight program. Two qualification objectives were addressed and met on TEM-3. The Nylok thread locking device of the 1U100269-03 leak check port plug and the 1U52295-04 safe and arm utilizing Krytox grease on the barrier-booster shaft O-rings were both certified. All inspection and instrumentation data indicate that the TEM-3 static test firing conducted 23 May 1989 was successful. The test was conducted at ambient conditions with the exception of the field joints (set point of 121 F, with a minimum of 87 F at the sensors), igniter joint (set point at 122 F with a minimum of 87 F at sensors) and case-to-nozzle joint (set point at 114 F with a minimum of 87 F at sensors). Ballistics performance values were within specification requirements. Nozzle performance was nominal with typical erosion. The nozzle and the case joint temperatures were maintained at the heaters controlling set points while electrical power was supplied. The water and the CO2 quench systems prevented damage to the metal hardware. All other test equipment performed as planned, contributing to a successful motor firing. All indications are that the test was a success, and all expected hardware will be refurbished for the RSRM program.

  12. Graphene nanoscrolls and live TEM imaging

    NASA Astrophysics Data System (ADS)

    Mokkapati, Venkata; Mirsaidov, Utkur; Matsudaira, Paul; Oezyilmaz, Barbaros; Graphene research laboratory Team; Centerbio-imaging sciences/Mechanobiology institute Team

    2013-03-01

    It has been theoretically hypothesized and predicted that graphene when in contact with water, wraps itself around the droplets and forms graphene nanoscrolls. Studying the applications of these nanoscrolls can open a new area of research especially in the bio-medical field. Here we present a method where partially suspended graphene nanoscrolls were fabricated on carbon mesh attached to a gold TEM grid. The process involves sandwiching of two graphene layers with water being encapsulated within these nanoscrolls. Gold nanoparticles were encapsulated and live imaging of water and gold nanoparticles was carried out under the TEM. The dynamics of the encapsulated water and nanobubbles is being studied. The encapsulated water within these graphene nanoscrolls lasted for more than three months (till the date of publication). It was also realized that the formation/abundance of these nanoscrolls is concentration dependent of the etching solution (Ammonium persulfate) with a saturation point. Large area, uniform, monolayer graphene films can also be produced by varying the concentration of Ammonium persulfate. Further studies are being carried out to live image TMV/protein and liposome encapsulated drugs using nanoscrolls and films respectively. The authors would like to acknowledge A*Star for funding this research

  13. Qualitative soil mineral analysis by EDXRF, XRD and AAS probes

    NASA Astrophysics Data System (ADS)

    Singh, Virendra; Agrawal, H. M.

    2012-12-01

    Soil minerals study is vital in terms of investigating the major soil forming compounds and to find out the fate of minor and trace elements, essential for the soil-plant interaction purpose. X-ray diffraction (XRD) has been a popular technique to search out the phases for different types of samples. For the soil samples, however, employing XRD is not so straightforward due to many practical problems. In the current approach, principal component analysis (PCA) has been used to have an idea of the minerals present, in qualitative manner, in the soil under study. PCA was used on the elemental concentrations data of 17 elements, determined by the energy dispersive X-ray fluorescence (EDXRF) technique. XRD analysis of soil samples has been done also to identify the minerals of major elements. Some prior treatments, like removal of silica by polytetrafluoroethylene (PTFE) slurry and grinding with alcohol, were given to samples to overcome the peak overlapping problems and to attain fine particle size which is important to minimize micro-absorption corrections, to give reproducible peak intensities and to minimize preferred orientation. A 2θ step of 0.05°/min and a longer dwell time than normal were used to reduce interferences from background noise and to increase the counting statistics. Finally, the sequential extraction procedure for metal speciation study has been applied on soil samples. Atomic absorption spectroscopy (AAS) was used to find the concentrations of metal fractions bound to various forms. Applying all the three probes, the minerals in the soils can be studied and identified, successfully.

  14. Silver Accumulation in the Green Microalga Coccomyxa actinabiotis: Toxicity, in Situ Speciation, and Localization Investigated Using Synchrotron XAS, XRD, and TEM.

    PubMed

    Leonardo, Thomas; Farhi, Emmanuel; Pouget, Stéphanie; Motellier, Sylvie; Boisson, Anne-Marie; Banerjee, Dipanjan; Rébeillé, Fabrice; den Auwer, Christophe; Rivasseau, Corinne

    2016-01-01

    Microalgae are good candidates for toxic metal remediation biotechnologies. This study explores the cellular processes implemented by the green microalga Coccomyxa actinabiotis to take up and cope with silver over the concentration range of 10(-7) to 10(-2) M Ag(+). Understanding these processes enables us to assess the potential of this microalga for applications for bioremediation. Silver in situ speciation and localization were investigated using X-ray absorption spectroscopy, X-ray diffraction, and transmission electron microscopy. Silver toxicity was evaluated by monitoring microalgal growth and photochemical parameters. Different accumulation mechanisms were brought out depending on silver concentration. At low micromolar concentration, microalgae fixed all silver initially present in solution, trapping it inside the cells into the cytosol, mainly as unreduced Ag(I) bound with molecules containing sulfur. Silver was efficiently detoxified. When concentration increased, silver spread throughout the cell and particularly entered the chloroplast, where it damaged the photosystem. Most silver was reduced to Ag(0) and aggregated to form crystalline silver nanoparticles of face-centered cubic structure with a mean size of 10 nm. An additional minor interaction of silver with molecules containing sulfur indicated the concomitant existence of the mechanism observed at low concentration or nanoparticle capping. Nanoparticles were observed in chloroplasts, in mitochondria, on the plasma membrane, on cytosolic membrane structures, and in vacuoles. Above 10(-4) M Ag(+), damages were irreversible, and photosynthesis and growth were definitely inhibited. However, high silver amounts remained confined inside microalgae, showing their potential for the bioremediation of contaminated water. PMID:26606242

  15. 4-D XRD for strain in many grains using triangulation

    SciTech Connect

    Bale, Hrishikesh A.; Hanan, Jay C.; Tamura, Nobumichi

    2006-12-31

    Determination of the strains in a polycrystalline materialusing 4-D XRD reveals sub-grain and grain-to-grain behavior as a functionof stress. Here 4-D XRD involves an experimental procedure usingpolychromatic micro-beam X-radiation (micro-Laue) to characterizepolycrystalline materials in spatial location as well as with increasingstress. The in-situ tensile loading experiment measured strain in a modelaluminum-sapphire metal matrix composite using the Advanced Light Source,Beam-line 7.3.3. Micro-Laue resolves individual grains in thepolycrystalline matrix. Results obtained from a list of grains sorted bycrystallographic orientation depict the strain states within and amongindividual grains. Locating the grain positions in the planeperpendicular to the incident beam is trivial. However, determining theexact location of grains within a 3-D space is challenging. Determiningthe depth of the grains within the matrix (along the beam direction)involved a triangulation method tracing individual rays that producespots on the CCD back to the point of origin. Triangulation wasexperimentally implemented by simulating a 3-D detector capturingmultiple diffraction images while increasing the camera to sampledistance. Hence by observing the intersection of rays from multiple spotsbelonging to the corresponding grain, depth is calculated. Depthresolution is a function of the number of images collected, grain to beamsize ratio, and the pixel resolution of the CCD. The 4DXRD methodprovides grain morphologies, strain behavior of each grain, andinteractions of the matrix grains with each other and the centrallylocated single crystal fiber.

  16. Quantifying Nonspecific TEM β-Lactamase (blaTEM) Genes in a Wastewater Stream▿

    PubMed Central

    Lachmayr, Karen L.; Kerkhof, Lee J.; DiRienzo, A. Gregory; Cavanaugh, Colleen M.; Ford, Timothy E.

    2009-01-01

    To control the antibiotic resistance epidemic, it is necessary to understand the distribution of genetic material encoding antibiotic resistance in the environment and how anthropogenic inputs, such as wastewater, affect this distribution. Approximately two-thirds of antibiotics administered to humans are β-lactams, for which the predominant bacterial resistance mechanism is hydrolysis by β-lactamases. Of the β-lactamases, the TEM family is of overriding significance with regard to diversity, prevalence, and distribution. This paper describes the design of DNA probes universal for all known TEM β-lactamase genes and the application of a quantitative PCR assay (also known as Taqman) to quantify these genes in environmental samples. The primer set was used to study whether sewage, both treated and untreated, contributes to the spread of these genes in receiving waters. It was found that while modern sewage treatment technologies reduce the concentrations of these antibiotic resistance genes, the ratio of blaTEM genes to 16S rRNA genes increases with treatment, suggesting that bacteria harboring blaTEM are more likely to survive the treatment process. Thus, β-lactamase genes are being introduced into the environment in significantly higher concentrations than occur naturally, creating reservoirs of increased resistance potential. PMID:18997031

  17. A Combined XRD/XRF Instrument for Lunar Resource Assessment

    NASA Technical Reports Server (NTRS)

    Vaniman, D. T.; Bish, D. L.; Chipera, S. J.; Blacic, J. D.

    1992-01-01

    Robotic surface missions to the Moon should be capable of measuring mineral as well as chemical abundances in regolith samples. Although much is already known about the lunar regolith, our data are far from comprehensive. Most of the regolith samples returned to Earth for analysis had lost the upper surface, or it was intermixed with deeper regolith. This upper surface is the part of the regolith most recently exposed to the solar wind; as such it will be important to resource assessment. In addition, it may be far easier to mine and process the uppermost few centimeters of regolith over a broad area than to engage in deep excavation of a smaller area. The most direct means of analyzing the regolith surface will be by studies in situ. In addition, the analysis of the impact-origin regolith surfaces, the Fe-rich glasses of mare pyroclastic deposits, are of resource interest, but are inadequately known; none of the extensive surface-exposed pyroclastic deposits of the Moon have been systematically sampled, although we know something about such deposits from the Apollo 17 site. Because of the potential importance of pyroclastic deposits, methods to quantify glass as well as mineral abundances will be important to resource evaluation. Combined x ray diffraction (XRD) and x ray fluorescence (XRF) analysis will address many resource characterization problems on the Moon. XRF methods are valuable for obtaining full major-element abundances with high precision. Such data, collected in parallel with quantitative mineralogy, permit unambiguous determination of both mineral and chemical abundances where concentrations are high enough to be of resource grade. Collection of both XRD and XRF data from a single sample provides simultaneous chemical and mineralogic information. These data can be used to correlate quantitative chemistry and mineralogy as a set of simultaneous linear equations, the solution of which can lead to full characterization of the sample. The use of

  18. A-10/TF34 Turbine Engine Monitoring System (TEMS)

    NASA Technical Reports Server (NTRS)

    Christopher, R. G.

    1981-01-01

    The hardware and software development of the A-10/TF34 turbine engine monitoring system (TEMS) is described. The operation and interfaces of the A-10/TF34 TEMS hardware are discussed with particular emphasis on function, capabilities, and limitations. The TEMS data types are defined and the various data acquisition modes are explained. Potential data products are also discussed.

  19. Motorized manipulator for positioning a TEM specimen

    DOEpatents

    Schmid, Andreas Karl; Andresen, Nord

    2010-12-14

    The invention relates to a motorized manipulator for positioning a TEM specimen holder with sub-micron resolution parallel to a y-z plane and rotating the specimen holder in the y-z plane, the manipulator comprising a base (2), and attachment means (30) for attaching the specimen holder to the manipulator, characterized in that the manipulator further comprises at least three nano-actuators (3.sup.a, 3.sup.b, 3.sup.c) mounted on the base, each nano-actuator showing a tip (4.sup.a, 4.sup.b, 4.sup.c), the at least three tips defining the y-z plane, each tip capable of moving with respect to the base in the y-z plane; a platform (5) in contact with the tips of the nano-actuators; and clamping means (6) for pressing the platform against the tips of the nano-actuators; as a result of which the nano-actuators can rotate the platform with respect to the base in the y-z plane and translate the platform parallel to the y-z plane.

  20. SIMS and TEM Analysis of Niobium Bicrystals

    SciTech Connect

    Maheshwari, P; Griffis, D P; Stevie, F A; Zhou, C; Ciovati, G; Myneni, R; Spradlin, J K

    2011-07-01

    The behaviour of interstitial impurities(C,O,N,H) on the Nb surface with respect to grain boundaries may affect cavity performance. Large grain Nb makes possible the selection of bicrystal samples with a well defined grain boundary. In this work, Dynamic SIMS was used to analyze two Nb bicrystal samples, one of them heat treated and the other non heat treated (control). H levels were found to be higher for the non heat treated sample and a difference in the H intensity and sputtering rate was also observed across the grain boundary for both the samples. TEM results showed that the bicrystal interface showed no discontinuity and the oxide layer was uniform across the grain boundary for both the samples. TOF-SIMS imaging was also performed to analyze the distribution of the impurities across the grain boundary in both the samples. C was observed to be segregated along the grain boundary for the control sample, while H and O showed a difference in signal intensity across the grain boundary. Crystal orientation appears to have an important role in the observed sputtering rate and impurity ion signal differences both across the grain boundary and between samples

  1. Rapid approximate inversion of airborne TEM

    NASA Astrophysics Data System (ADS)

    Fullagar, Peter K.; Pears, Glenn A.; Reid, James E.; Schaa, Ralf

    2015-11-01

    Rapid interpretation of large airborne transient electromagnetic (ATEM) datasets is highly desirable for timely decision-making in exploration. Full solution 3D inversion of entire airborne electromagnetic (AEM) surveys is often still not feasible on current day PCs. Therefore, two algorithms to perform rapid approximate 3D interpretation of AEM have been developed. The loss of rigour may be of little consequence if the objective of the AEM survey is regional reconnaissance. Data coverage is often quasi-2D rather than truly 3D in such cases, belying the need for `exact' 3D inversion. Incorporation of geological constraints reduces the non-uniqueness of 3D AEM inversion. Integrated interpretation can be achieved most readily when inversion is applied to a geological model, attributed with lithology as well as conductivity. Geological models also offer several practical advantages over pure property models during inversion. In particular, they permit adjustment of geological boundaries. In addition, optimal conductivities can be determined for homogeneous units. Both algorithms described here can operate on geological models; however, they can also perform `unconstrained' inversion if the geological context is unknown. VPem1D performs 1D inversion at each ATEM data location above a 3D model. Interpretation of cover thickness is a natural application; this is illustrated via application to Spectrem data from central Australia. VPem3D performs 3D inversion on time-integrated (resistive limit) data. Conversion to resistive limits delivers a massive increase in speed since the TEM inverse problem reduces to a quasi-magnetic problem. The time evolution of the decay is lost during the conversion, but the information can be largely recovered by constructing a starting model from conductivity depth images (CDIs) or 1D inversions combined with geological constraints if available. The efficacy of the approach is demonstrated on Spectrem data from Brazil. Both separately and in

  2. Reactivity of some vanadium oxides: An EPR and XRD study

    SciTech Connect

    Occhiuzzi, Manlio

    2005-05-15

    V{sub 2}O{sub 5}, VO{sub 2} and V{sub 2}O{sub 3} fresh samples and at different times after purchase or preparation (aged samples) were investigated by chemical analysis, redox treatments, XRD and EPR. The ageing process through a reaction with water and oxygen slowly oxidize crystalline VO{sub 2} and V{sub 2}O{sub 3}, leading to a quasi-amorphous phase with bariandite structure (V{sub 10}O{sub 24}.12H{sub 2}O). The role of water is the progressive demolition of the compact structures and formation of hydrated phase. Kinetic study of VO{sub 2} oxidation by O{sub 2} and O{sub 2}+H{sub 2}O mixture indicates that increasing the temperature up to 723K the effect of water becomes less important. The reaction leads to partially oxidized products with decreasing water content: bariandite at room temperature, V{sub 3}O{sub 7}.H{sub 2}O at 383K and V{sub 3}O{sub 7} at 723K. Kinetic investigation of V{sub 2}O{sub 5} reduction by CO at 633-723K showed that the reduction process proceeds trough the formation of V{sup 4+} and of electrons delocalized in the conduction band.

  3. RBS and XRD Characterization of Yttrium Iron Garnet Thin Films

    NASA Astrophysics Data System (ADS)

    Mansour, M.; Roumie, M.; Abdel Samad, B.; Basma, H.; Korek, M.

    2015-03-01

    Magnetic materials such as yttrium iron garnet (YIG or Y3Fe5O12) present a great importance for their magneto-optic properties. They are potential materials used for applications in the domain of optical telecommunications for example. In this work, we have investigated YIG thin films deposited on substrates of quartz and GGG (gadolinium gallium garnet or Gd3Ga5O12). Using Rutherford backscattering spectrometry (RBS) we characterized the performed layers (thickness and stoichiometry) in order to correlate the films preparation conditions with the quality of the final material. We determined the optimal energy of the alpha particles beam used for RBS measurements and we fitted the experimental spectra using the SIMNRA simulated code. Our RBS results showed that the films have a stoichiometry close to that of the starting material. In addition, we found that the film thickness is proportional to deposition time but inversely proportional to the substrate temperature. Moreover, using x-ray diffraction (XRD) we determined the annealing effect on the structure of the profile of our thin films.

  4. Substitution of Thr for Ala-237 in TEM-17, TEM-12 and TEM-26: alterations in beta-lactam resistance conferred on Escherichia coli.

    PubMed

    Giakkoupi, P; Hujer, A M; Miriagou, V; Tzelepi, E; Bonomo, R A; Tzouvelekis, L S

    2001-07-10

    Non-naturally occurring mutants of TEM-17 (E104K), TEM-12 (R164S) and TEM-26 (E104K:R164S) extended-spectrum (ES) beta-lactamases bearing threonine at position 237 were constructed by site-specific mutagenesis and expressed under isogenic conditions in Escherichia coli. Quantification of beta-lactamase activities and immunoblotting indicated that Ala-237-->Thr did not significantly affect expression levels of these ES enzymes. Minimum inhibitory concentrations of beta-lactam antibiotics showed that the presence of threonine at position 237 exerted a dominant effect increasing the enzymes' preference for various early generation cephalosporins over penicillins. Activity against broad-spectrum oxyimino-beta-lactams was also changed. The effect of Ala-237-->Thr on the activity against ceftazidime, aztreonam, cefepime and cefpirome of all three ES TEM enzymes was detrimental. Introduction of Thr-237 improved activity against cefotaxime and ceftriaxone in TEM-12 and TEM-26, but not in TEM-17. PMID:11445164

  5. XRD studies of chitin-based polyurethane elastomers.

    PubMed

    Zia, Khalid Mahmood; Bhatti, Ijaz Ahmad; Barikani, Mehdi; Zuber, Mohammad; Sheikh, Munir Ahmad

    2008-08-15

    Chitin-based polyurethane elastomers (PUEs) were synthesized by step growth polymerization techniques using poly(epsilon-caprolactone) (PCL) varying diisocyanate and chain extender structures. The viscosity average molecular weight (M(v)) of chitin was deduced from the intrinsic viscosity and found; M(v)=6.067 x 10(5). The conventional spectroscopic characterization of the samples with FTIR, (1)H NMR and (13)C NMR were in accordance with proposed PUEs structure. The crystalline behavior of the synthesized polymers were investigated by X-ray diffraction (XRD), differential scanning calorimetery (DSC) and loss tangent curves (tan delta peaks). The observed patterns of the crystalline peaks for the lower angle for chitin in the 2theta range were indexed as 9.39 degrees, 19.72 degrees, 20.73 degrees, 23.41 degrees and 26.39 degrees. Results showed that crystallinity of the synthesized PUEs samples was affected by varying the structure of the diisocyanate and chain extender. Crystallinity decreased from aliphatic to aromatic characters of the diisocyanates used in the final PU. The presence of chitin also favors the formation of more ordered structure, as higher peak intensities was obtained from the PU extended with chitin than 1,4-butane diol (BDO). The value of peak enthalpy (DeltaH) of chitin was found to be 47.13 J g(-1). The higher DeltaH value of 46.35 J g(-1) was found in the samples extended with chitin than BDO (39.73 J g(-1)). PMID:18495239

  6. XRD and Mössbauer studies on Pt Fe nano-particles synthesized by polyol method for cathode catalyst of PEFCS

    NASA Astrophysics Data System (ADS)

    Toriyama, T.; Kawahara, N.; Maeda, Y.; Suruga, T.; Wakabayashi, H.; Takagi, Y.

    2008-04-01

    Pt50 Fe50 nanoparticles were synthesized by the chemically wet process for developing a new high efficiency cathode catalyst in PEFCs. The particle morphology and crystal structure of as synthesized Pt Fe particles, and electronic state of Fe atoms in them were evaluated using transmission electron microscopy(TEM), X-ray diffraction(XRD) and transmission Mössbauer spectroscopy (TMS), respectively. They are confirmed to be of chemically disordered fcc structure from XRD pattern and the average diameter of them was estimated to be 3.1 nm from both TEM and the width of (111) peak in XRD pattern. From TMS spectrum, it was concluded to consist of mainly the component of Fe oxides connected with the organic ligands according to XPS results mentioned below. But, probably it contains the component for superparamagnetic Pt Fe nanoparticles. Also the electrocatalytic activity and a hydrogen adsorption/desorption behavior for as synthesized Pt Fe nanoparticles was observed by cyclic voltammetry and the oxidation of Fe atoms in as synthesized Pt Fe nanoparticles, Fe metal and Fe oxides were measured.

  7. Transmission Electron Microscopy (TEM) Sample Preparation of Si(1-x)Gex in c-Plane Sapphire Substrate

    NASA Technical Reports Server (NTRS)

    Kim, Hyun Jung; Choi, Sang H.; Bae, Hyung-Bin; Lee, Tae Woo

    2012-01-01

    The National Aeronautics and Space Administration-invented X-ray diffraction (XRD) methods, including the total defect density measurement method and the spatial wafer mapping method, have confirmed super hetero epitaxy growth for rhombohedral single crystalline silicon germanium (Si1-xGex) on a c-plane sapphire substrate. However, the XRD method cannot observe the surface morphology or roughness because of the method s limited resolution. Therefore the authors used transmission electron microscopy (TEM) with samples prepared in two ways, the focused ion beam (FIB) method and the tripod method to study the structure between Si1-xGex and sapphire substrate and Si1?xGex itself. The sample preparation for TEM should be as fast as possible so that the sample should contain few or no artifacts induced by the preparation. The standard sample preparation method of mechanical polishing often requires a relatively long ion milling time (several hours), which increases the probability of inducing defects into the sample. The TEM sampling of the Si1-xGex on sapphire is also difficult because of the sapphire s high hardness and mechanical instability. The FIB method and the tripod method eliminate both problems when performing a cross-section TEM sampling of Si1-xGex on c-plane sapphire, which shows the surface morphology, the interface between film and substrate, and the crystal structure of the film. This paper explains the FIB sampling method and the tripod sampling method, and why sampling Si1-xGex, on a sapphire substrate with TEM, is necessary.

  8. The Structural Bases of Antibiotic Resistance in the Clinically Derived Mutant beta-Lactamases TEM-30, TEM-32, and TEM-34

    SciTech Connect

    Wang, Xiaojun; Minasov, George; Shoichet, Brian K.

    2010-03-08

    Widespread use of {beta}-lactam antibiotics has promoted the evolution of {beta}-lactamase mutant enzymes that can hydrolyze ever newer classes of these drugs. Among the most pernicious mutants are the inhibitor-resistant TEM {beta}-lactamases (IRTs), which elude mechanism-based inhibitors, such as clavulanate. Despite much research on these IRTs, little is known about the structural bases of their action. This has made it difficult to understand how many of the resistance substitutions act as they often occur far from Ser-130. Here, three IRT structures, TEM-30 (R244S), TEM-32 (M69I/M182T), and TEM-34 (M69V), are determined by x-ray crystallography at 2.00, 1.61, and 1.52 {angstrom}, respectively. In TEM-30, the Arg-244 {yields} Ser substitution (7.8 {angstrom} from Ser-130) displaces a conserved water molecule that usually interacts with the {beta}-lactam C3 carboxylate. In TEM-32, the substitution Met-69 {yields} Ile (10 {angstrom} from Ser-130) appears to distort Ser-70, which in turn causes Ser-130 to adopt a new conformation, moving its O{gamma} further away, 2.3 {angstrom} from where the inhibitor would bind. This substitution also destabilizes the enzyme by 1.3 kcal/mol. The Met-182 {yields} Thr substitution (20 {angstrom} from Ser-130) has no effect on enzyme activity but rather restabilizes the enzyme by 2.9 kcal/mol. In TEM-34, the Met-69 {yields} Val substitution similarly leads to a conformational change in Ser-130, this time causing it to hydrogen bond with Lys-73 and Lys-234. This masks the lone pair electrons of Ser-130 O{gamma}, reducing its nucleophilicity for cross-linking. In these three structures, distant substitutions result in accommodations that converge on the same point of action, the local environment of Ser-130. TEM-1 {beta}-lactamase is the predominant source of resistance to {beta}-lactams, such as the penicillins. TEM-1 and related class A {beta}-lactamases confer resistance by hydrolyzing the {beta}-lactam ring of these antibiotics

  9. XRD measurement of mean crystallite thickness of illite and illite/smectite: Reappraisal of the Kubler index and the Scherrer equation

    USGS Publications Warehouse

    Drits, V.; Srodon, J.; Eberl, D.D.

    1997-01-01

    The standard form of the Scherrer equation, which has been used to calculate the mean thickness of the coherent scattering domain (CSD) of illite crystals from X-ray diffraction (XRD) full width data at half maximum (FWHM) intensity, employs a constant, Ksh, of 0.89. Use of this constant is unjustified, even if swelling has no effect on peak broadening, because this constant is valid only if all CSDs have a single thickness. For different thickness distributions, the Scherrer "constant" has very different values. Analysis of fundamental particle thickness data (transmission electron microscopy, TEM) for samples of authigenic illite and illite/smectite from diagenetically altered pyroclastics and filamentous illites from sandstones reveals a unique family of lognormal thickness distributions for these clays. Experimental relations between the distributions' lognormal parameters and mean thicknesses are established. These relations then are used to calculate the mean thickness of CSDs for illitic samples from XRD FWHM, or from integral XRD peak widths (integrated intensity/maximum intensity). For mixed-layer illite/smectite, the measured thickness of the CSD corresponds to the mean thickness of the mixed-layer crystal. Using this measurement, the mean thickness of the fundamental particles that compose the mixed-layer crystals can be calculated after XRD determination of precent smectitic interlayers. The effect of mixed layering (swelling) on XRD peak width for these samples is eliminated by using the 003 reflection for glycolated samples, and the 001, 002 or 003 reflection for dehydrated, K-saturated samples. If this technique is applied to the 001 reflection of air-dried samples (Kubler index measurement), mean CSD thicknesses are underestimated due to the mixed-layering effect. The technique was calibrated using NEWMOD ??-simulated XRD profiles of illite, and then tested on well-characterized illite and illite/smectite smaples. The XRD measurements are in good

  10. Recognition and Resistance in TEM [superscript beta]-Lactamase

    SciTech Connect

    Wang, Xiaojun; Minasov, George; Blazquez, Jesus; Caselli, Emilia; Prati, Fabio; Shoichet, Brian K.

    2010-03-08

    Developing antimicrobials that are less likely to engender resistance has become an important design criterion as more and more drugs fall victim to resistance mutations. One hypothesis is that the more closely an inhibitor resembles a substrate, the more difficult it will be to develop resistant mutations that can at once disfavor the inhibitor and still recognize the substrate. To investigate this hypothesis, 10 transition-state analogues, of greater or lesser similarity to substrates, were tested for inhibition of TEM-1 beta-lactamase, the most widespread resistance enzyme to penicillin antibiotics. The inhibitors were also tested against four characteristic mutant enzymes: TEM-30, TEM-32, TEM-52, and TEM-64. The inhibitor most similar to the substrate, compound 10, was the most potent inhibitor of the WT enzyme, with a K(i) value of 64 nM. Conversely, compound 10 was the most susceptible to the TEM-30 (R244S) mutant, for which inhibition dropped by over 100-fold. The other inhibitors were relatively impervious to the TEM-30 mutant enzyme. To understand recognition and resistance to these transition-state analogues, the structures of four of these inhibitors in complex with TEM-1 were determined by X-ray crystallography. These structures suggest a structural basis for distinguishing inhibitors that mimic the acylation transition state and those that mimic the deacylation transition state; they also suggest how TEM-30 reduces the affinity of compound 10. In cell culture, this inhibitor reversed the resistance of bacteria to ampicillin, reducing minimum inhibitory concentrations of this penicillin by between 4- and 64-fold, depending on the strain of bacteria. Notwithstanding this activity, the resistance of TEM-30, which is already extant in the clinic, suggests that there can be resistance liabilities with substrate-based design.

  11. Multiplexed TEM Specimen Preparation and Analysis of Plasmonic Nanoparticles

    PubMed Central

    Cheng, Anchi; Crum, John; Jain, Tilak; Duggan, Erika; Liu, Er; Nolan, John P.; Carragher, Bridget; Potter, Clinton S.

    2015-01-01

    We describe a system for rapidly screening hundreds of nanoparticle samples using transmission electron microscopy (TEM). The system uses a liquid handling robot to place up to 96 individual samples onto a single standard TEM grid at separate locations. The grid is then transferred into the TEM and automated software is used to acquire multi-scale images of each sample. The images are then analyzed to extract metrics on the size, shape, and morphology of the nanoparticles. The system has been used to characterize plasmonically-active nanomaterials. PMID:26223550

  12. Multiplexed TEM Specimen Preparation and Analysis of Plasmonic Nanoparticles.

    PubMed

    Mulligan, Sėan K; Speir, Jeffrey A; Razinkov, Ivan; Cheng, Anchi; Crum, John; Jain, Tilak; Duggan, Erika; Liu, Er; Nolan, John P; Carragher, Bridget; Potter, Clinton S

    2015-08-01

    We describe a system for rapidly screening hundreds of nanoparticle samples using transmission electron microscopy (TEM). The system uses a liquid handling robot to place up to 96 individual samples onto a single standard TEM grid at separate locations. The grid is then transferred into the TEM and automated software is used to acquire multiscale images of each sample. The images are then analyzed to extract metrics on the size, shape, and morphology of the nanoparticles. The system has been used to characterize plasmonically active nanomaterials. PMID:26223550

  13. Novel Sample-handling Approach for XRD Analysis with Minimal Sample Preparation

    NASA Technical Reports Server (NTRS)

    Sarrazin, P.; Chipera, S.; Bish, D.; Blake, D.; Feldman, S.; Vaniman, D.; Bryson, C.

    2004-01-01

    Sample preparation and sample handling are among the most critical operations associated with X-ray diffraction (XRD) analysis. These operations require attention in a laboratory environment, but they become a major constraint in the deployment of XRD instruments for robotic planetary exploration. We are developing a novel sample handling system that dramatically relaxes the constraints on sample preparation by allowing characterization of coarse-grained material that would normally be impossible to analyze with conventional powder-XRD techniques.

  14. Coordinated Isotopic and TEM Studies of Presolar Graphites from Murchison

    NASA Astrophysics Data System (ADS)

    Croat, T. K.; Stadermann, F. J.; Zinner, E.; Bernatowicz, T. J.

    2004-03-01

    TEM and NanoSIMS investigations of the same presolar Murchison KFC graphites revealed high Zr, Mo, and Ru content in refractory carbides within the graphites. Along with isotopically light carbon, these suggest a low-metallicity AGB source.

  15. Instability of nanoscale metallic particles under electron irradiation in TEM

    NASA Astrophysics Data System (ADS)

    Chen, X. Y.; Zhang, S. G.; Xia, M. X.; Li, J. G.

    2016-03-01

    The stability of nano metallic glass under electron beam in transmission electron microscope (TEM) was investigated. The most common voltage of TEM used in metallic materials characterization was either 200 kV or 300 kV. Both situations were investigated in this work. An amorphous metallic particle with a dimension of a few hundred nanometers was tested under 300 keV electron irradiation. New phase decomposed from the parent phase was observed. Moreover, a crystal particle with the same composition and dimension was tested under 200 keV irradiation. Decomposition process also occurred in this situation. Besides, crystal orientation modification was observed during irradiation. These results proved that the electron beam in TEM have an effect on the stability of nanoscale samples during long time irradiation. Atomic displacement was induced and diffusion was enhanced by electron irradiation. Thus, artifacts would be induced when a nanoscale metallic sample was characterized in TEM.

  16. TEM Study of Internal Crystals in Supernova Graphites

    NASA Astrophysics Data System (ADS)

    Croat, T. K.; Bernatowicz, T.; Stadermann, F. J.; Messenger, S.; Amari, S.

    2003-03-01

    A coordinated TEM and isotopic study of ten supernova (SN) graphites from the Murchison meteorite has revealed many internal grains, mostly titanium carbides (TiCs) and TiC-kamacite composite grains, which were accreted during the graphite growth.

  17. Preparation of carbon-free TEM microgrids by metal sputtering.

    PubMed

    Janbroers, S; de Kruijff, T R; Xu, Q; Kooyman, P J; Zandbergen, H W

    2009-08-01

    A new method for preparing carbon-free, temperature-stable Transmission Electron Microscope (TEM) grids is presented. An 80% Au/20% Pd metal film is deposited onto a 'holey' microgrid carbon supported on standard mixed-mesh Au TEM grids. Subsequently, the carbon film is selectively removed using plasma cleaning. In this way, an all-metal TEM film is made containing the 'same' microgrid as the original carbon film. Although electron transparency of the foil is reduced significantly, the open areas for TEM inspection of material over these areas are maintained. The metal foil can be prepared with various thicknesses and ensures good electrical conductivity. The new Au/Pd grids are stable to at least 775K under vacuum conditions. PMID:19450927

  18. Phase velocity of the TEM (1,0)+TEM (0,1) mode laser and electron accelerations in vacuum

    SciTech Connect

    Wu, L.; Kong, Q.; Ho, Y. K.; Wang, P. X.; Xu, J. J.; Lin, D.; Kawata, S.

    2007-04-01

    Unlike at any single TEM (n, m) mode laser, there is a subluminous phase velocity region located along the central region of a TEM (1,0)+TEM (0,1) mode laser. In conjunction with the high longitudinal electric field in this region, it forms another acceleration channel, which also locates inside the transverse ponderomotive potential trap. Through simulation, it is found that relativistic electrons injected into this acceleration channel can stand at the acceleration phase for a long time and be synchronously accelerated to high energies. Also, the accelerated electrons can be well confined inside the trap avoiding the transverse scattering problem.

  19. Experimental verification of the SP-100 TEM pump analytical models

    SciTech Connect

    Salamah, S.A.; Miller, D.D.; Sinha, U.N.; Narkiewicz, R.S. )

    1993-01-15

    Validation of the TEM pump analytical model is conducted via experimental verification of the model prediction. Two key tests that have provided essential information toward this objective are the Magnetic Bench Test (MBT) and the ElectroMagnetic Integration Test (EMIT). The tests are briefly described and experimental results are compared with predictions of simulation models that form part of overall TEM pump performance model.

  20. Remote In-Situ Quantitative Mineralogical Analysis Using XRD/XRF

    NASA Technical Reports Server (NTRS)

    Blake, D. F.; Bish, D.; Vaniman, D.; Chipera, S.; Sarrazin, P.; Collins, S. A.; Elliott, S. T.

    2001-01-01

    X-Ray Diffraction (XRD) is the most direct and accurate method for determining mineralogy. The CHEMIN XRD/XRF instrument has shown promising results on a variety of mineral and rock samples. Additional information is contained in the original extended abstract.

  1. Novel sample preparation for operando TEM of catalysts.

    PubMed

    Miller, Benjamin K; Barker, Trevor M; Crozier, Peter A

    2015-09-01

    A new TEM sample preparation method is developed to facilitate operando TEM of gas phase catalysis. A porous Pyrex-fiber pellet TEM sample was produced, allowing a comparatively large amount of catalyst to be loaded into a standard Gatan furnace-type tantalum heating holder. The increased amount of catalyst present inside the environmental TEM allows quantitative determination of the gas phase products of a catalytic reaction performed in-situ at elevated temperatures. The product gas concentration was monitored using both electron energy loss spectroscopy (EELS) and residual gas analysis (RGA). Imaging of catalyst particles dispersed over the pellet at atomic resolution is challenging, due to charging of the insulating glass fibers. To overcome this limitation, a metal grid is placed into the holder in addition to the pellet, allowing catalyst particles dispersed over the grid to be imaged, while particles in the pellet, which are assumed to experience identical conditions, contribute to the overall catalytic conversion inside the environmental TEM cell. The gas within the cell is determined to be well-mixed, making this assumption reasonable. PMID:25974880

  2. Detecting flaws in Portland cement concrete using TEM horn antennae

    NASA Astrophysics Data System (ADS)

    Al-Qadi, Imad L.; Riad, Sedki M.; Su, Wansheng; Haddad, Rami H.

    1996-11-01

    To understand the dielectric properties of PCC and better correlate them with type and severity of PCC internal defects, a study was conducted to evaluate PCC complex permittivity and magnetic permeability over a wideband of frequencies using both time domain and frequency domain techniques. Three measuring devices were designed and fabricated: a parallel plate capacitor, a coaxial transmission line, and transverse electromagnetic (TEM) horn antennae. The TEM horn antenna covers the microwave frequencies. The measurement technique involves a time domain setup that was verified by a frequency domain measurement. Portland cement concrete slabs, 60 by 75 by 14 cm, were cast; defects include delamination, delamination filled with water, segregation, and chloride contamination. In this paper, measurements using the TEM horn antennae and the feasibility of detecting flaws at microwave frequency are presented.

  3. Complete Tem-Tomography: 3D Structure of Gems Cluster

    NASA Technical Reports Server (NTRS)

    Matsuno, J.; Miyake, A.; Tsuchiyama, A.; Messenger, S.; Nakamura-Messenger, K.

    2015-01-01

    GEMS (glass with embedded metal and sulfide) grains in interplanetary dust particles (IDPs) are considered to be one of the ubiquitous and fundamental building blocks of solids in the Solar System. They have been considered to be interstellar silicate dust that survived various metamorphism or alteration processes in the protoplanetary disk but the elemental and isotopic composition measurements suggest that most of them have been formed in the protoplanetary disk as condensates from high temperature gas. This formation model is also supported by the formation of GEMS-like grains with respect to the size, mineral assemblage, texture and infrared spectrum by condensation experiments from mean GEMS composition materials. Previous GEMS studies were performed only with 2D observation by transmission electron microscopy (TEM) or scanning TEM (STEM). However, the 3D shape and structure of GEMS grains and the spatial distribution of Fe/FeS's has critical information about their formation and origin. Recently, the 3D structure of GEMS grains in ultrathin sections of cluster IDPs was revealed by electron tomography using a TEM/STEM (JEM-2100F, JEOL). However, CT images of thin sections mounted on Cu grids acquired by conventional TEM-tomography are limited to low tilt angles (e. g., less than absolute value of 75 deg. In fact, previous 3D TEM observations of GEMS were affected by some artifacts related to the limited tilt range in the TEM used. Complete tomographic images should be acquired by rotating the sample tilt angle over a range of more than absolute value of 80 deg otherwise the CT images lose their correct structures. In order to constrain the origin and formation process of GEMS grains more clearly, we performed complete electron tomography for GEMS grains. Here we report the sample preparation method we have developed for this study, and the preliminary results.

  4. Investigating materials formation with liquid-phase and cryogenic TEM

    NASA Astrophysics Data System (ADS)

    de Yoreo, J. J.; N. A. J. M., Sommerdijk

    2016-08-01

    The recent advent of liquid-phase transmission electron microscopy (TEM) and advances in cryogenic TEM are transforming our understanding of the physical and chemical mechanisms underlying the formation of materials in synthetic, biological and geochemical systems. These techniques have been applied to study the dynamic processes of nucleation, self-assembly, crystal growth and coarsening for metallic and semiconductor nanoparticles, (bio)minerals, electrochemical systems, macromolecular complexes, and organic and inorganic self-assembling systems. New instrumentation and methodologies that are currently on the horizon promise new opportunities for advancing the science of materials synthesis.

  5. Below-Band-Gap Laser Ablation Of Diamond For TEM

    NASA Technical Reports Server (NTRS)

    George, Thomas; Foote, Marc C.; Vasquez, Richard P.; Fortier, Edward P.; Posthill, John B.

    1995-01-01

    Thin, electron-transparent layers of diamond for examination in transmission electron microscope (TEM) fabricated from thicker diamond substrates by using laser beam to ablate surface of substrate. Involves use of photon energy below band gap. Growing interest in use of diamond as bulk substrate and as coating material in variety of applications has given rise to increasing need for TEM for characterization of diamond-based materials. Below-band-gap laser ablation method helps to satisfy this need. Also applied in general to cutting and etching of diamonds.

  6. RECENT DEVELOPMENT IN TEM CHARACTERIZATION OF IRRADIATED RERTR FUELS

    SciTech Connect

    J. Gan; B.D. Miller; D.D. Keiser Jr.; A.B. Robinson; J.W. Madden; P.G. Medvedev; D.M. Wachs

    2011-10-01

    The recent development on TEM work of irradiated RERTR fuels includes microstructural characterization of the irradiated U-10Mo/alloy-6061 monolithic fuel plate, the RERTR-7 U-7Mo/Al-2Si and U-7Mo/Al-5Si dispersion fuel plates. It is the first time that a TEM sample of an irradiated nuclear fuel was prepared using the focused-ion-beam (FIB) lift-out technical at the Idaho National Laboratory. Multiple FIB TEM samples were prepared from the areas of interest in a SEM sample. The characterization was carried out using a 200kV TEM with a LaB6 filament. The three dimensional orderings of nanometer-sized fission gas bubbles are observed in the crystalline region of the U-Mo fuel. The co-existence of bubble superlattice and dislocations is evident. Detailed microstructural information along with composition analysis is obtained. The results and their implication on the performance of these fuels are discussed.

  7. Unexpected Enzyme TEM-126: Role of Mutation Asp179Glu

    PubMed Central

    Delmas, J.; Robin, F.; Bittar, F.; Chanal, C.; Bonnet, R.

    2005-01-01

    The clinical isolate Escherichia coli CF884 exhibited low-level resistance to ceftazidime (4 μg/ml) by a positive double-disk synergy test and apparent susceptibility to cefuroxime, cefotaxime, cefepime, cefpirome, and aztreonam. The enzyme implicated in this phenotype was a novel 180-kb plasmid-encoded TEM-type extended-spectrum β-lactamase designated TEM-126 which harbors the mutations Asp179Glu and Met182Thr. TEM-126 exhibited significant hydrolytic activity (kcat, 2 s−1) and a Km value of 82 μM against ceftazidime. Molecular dynamics simulations suggested that the substitution Asp179Glu induces subtle conformational changes to the omega loop which may favor the insertion of ceftazidime in the binding site and the correct positioning of the crucial residue Glu166. Overall, these results highlight the remarkable plasticity of TEM enzymes, which can expand their activity against ceftazidime by the addition of one carbon atom in the side chain of residue 179. PMID:16189109

  8. Imaging and diffraction of protein crystallization using TEM.

    PubMed

    Gomery, Kathryn; Humphrey, Elaine C; Herring, Rodney

    2013-06-01

    Structural biology relies on good-quality protein crystals in order for structure determination. Many factors affect the growth process of a protein crystal including the way it nucleates and the types of damage and contamination during its growth. Although the nucleation process and quality of a crystal is vital to structure determination, they are both under-studied areas of research. Our research begins to explore ways of measuring the quality of protein crystals, using TEM, thus overcoming the problems associated with viewing wet specimens in a vacuum. Our current understanding of nucleation is that it is a two-step mechanism involving the formation of nuclei from dense liquid clusters; however; it is still unclear whether nuclei first start as amorphous aggregates or as crystalline lattices. Potentially, electron diffraction may be capable of uncovering this process. Using TEM imaging and diffraction of lysozyme as a model protein crystal, we report the internal two-dimensional strain and the density of crystallites in a protein crystal, at a resolution never seen before. The TEM diffraction shows unique features of crystal mosaicity that can be directly correlated to TEM images. PMID:23250893

  9. Properties of linear microwave plasma sustained by coaxial TEM waveguide

    NASA Astrophysics Data System (ADS)

    Han, Moon-Ki; Seo, Kwon-Sang; Kim, Dong Hyun; Lee, Hae June; Lee, Ho-Jun

    2013-09-01

    A linear 2.45GHz microwave plasma sustained by coaxial circular TEM waveguide has been developed for the low temperature large area plasma enhanced chemical vapor deposition application. TE-TEM microwave power coupling was achieved by copper rod located at λg/4 from short-end of TE10 waveguide. TEM waveguide consists of quartz tube surrounded by plasma and copper rod electrode. TEM waveguide is 60 cm in length and 3 cm in diameter, which is terminated with shorted metal cap. For the operation condition of 300 W input power and Ar pressure of 200 mTorr, a clear standing wave pattern with wavelength of 10 cm was observed. Measured plasma density and temperature at 5 cm from quartz wall was 1.2 × 1017/cm3 and 1.7 eV respectively. Density non-uniformity was less than 6% along quartz tube in spite of standing wave set-up. In addition, properties of the microwave source are also investigated through electromagnetic field simulation coupled with drift-diffusion approximation of plasma. Calculated and measured standing wave pattern was almost identical. Electron density and temperature distribution show similar behavior with experimental results. S11 value of input port of TE10 waveguide was calculated as 17dB.

  10. Dopant profiling in the TEM, progress towards quantitative electron holography

    SciTech Connect

    Cooper, David; Truche, Robert; Chabli, Amal; Twitchett-Harrison, Alison C.; Midgley, Paul A.; Dunin-Borkowski, Rafal E.

    2007-09-26

    Off-axis electron holography has been used to characterise the dopant potential in GaAs p-n junctions. We show that the measured potential across the junctions is affected by both FIB specimen preparation and by charging in the TEM and suggest methods that can be used to minimise these problems.

  11. A versatile and inexpensive XRD sample holder for highly radioactive or hazardous samples.

    SciTech Connect

    Strachan, Denis M.); Schaef, Herbert T.); Schweiger, Michael J.); Simmons, Kevin L.); Woodcock, Leslie J.); Krouse, Michael K.)

    2003-03-15

    Two XRD sample holders have been designed for use with highly radioactive samples. An injection mold that allows us to produce the holders inexpensively has been constructed for one of the holders. These holders are suitable for single-time use. The ease of use and the disposable nature have resulted in a dramatic reduction in personnel exposure and an uncontaminated XRD unit. A second holder, based on the design of the first, is used to obtain XRD patterns from powders where preferred orientation is an issue and from clays. Both holders result in negligible background, since the sample is essentially levitated in the x-ray beam. This is a benefit over other methods, such as collodion, that introduce significant background to the XRD pattern.

  12. Hollow nitrogen-containing core/shell fibrous carbon nanomaterials as support to platinum nanocatalysts and their TEM tomography study

    NASA Astrophysics Data System (ADS)

    Zhou, Cuifeng; Liu, Zongwen; Du, Xusheng; Mitchell, David Richard Graham; Mai, Yiu-Wing; Yan, Yushan; Ringer, Simon

    2012-03-01

    Core/shell nanostructured carbon materials with carbon nanofiber (CNF) as the core and a nitrogen (N)-doped graphitic layer as the shell were synthesized by pyrolysis of CNF/polyaniline (CNF/PANI) composites prepared by in situ polymerization of aniline on CNFs. High-resolution transmission electron microscopy (TEM), X-ray diffraction (XRD), Fourier transform infrared and Raman analyses indicated that the PANI shell was carbonized at 900°C. Platinum (Pt) nanoparticles were reduced by formic acid with catalyst supports. Compared to the untreated CNF/PANI composites, the carbonized composites were proven to be better supporting materials for the Pt nanocatalysts and showed superior performance as catalyst supports for methanol electrochemical oxidation. The current density of methanol oxidation on the catalyst with the core/shell nanostructured carbon materials is approximately seven times of that on the catalyst with CNF/PANI support. TEM tomography revealed that some Pt nanoparticles were embedded in the PANI shells of the CNF/PANI composites, which might decrease the electrocatalyst activity. TEM-energy dispersive spectroscopy mapping confirmed that the Pt nanoparticles in the inner tube of N-doped hollow CNFs could be accessed by the Nafion ionomer electrolyte, contributing to the catalytic oxidation of methanol.

  13. Hollow nitrogen-containing core/shell fibrous carbon nanomaterials as support to platinum nanocatalysts and their TEM tomography study

    PubMed Central

    2012-01-01

    Core/shell nanostructured carbon materials with carbon nanofiber (CNF) as the core and a nitrogen (N)-doped graphitic layer as the shell were synthesized by pyrolysis of CNF/polyaniline (CNF/PANI) composites prepared by in situ polymerization of aniline on CNFs. High-resolution transmission electron microscopy (TEM), X-ray diffraction (XRD), Fourier transform infrared and Raman analyses indicated that the PANI shell was carbonized at 900°C. Platinum (Pt) nanoparticles were reduced by formic acid with catalyst supports. Compared to the untreated CNF/PANI composites, the carbonized composites were proven to be better supporting materials for the Pt nanocatalysts and showed superior performance as catalyst supports for methanol electrochemical oxidation. The current density of methanol oxidation on the catalyst with the core/shell nanostructured carbon materials is approximately seven times of that on the catalyst with CNF/PANI support. TEM tomography revealed that some Pt nanoparticles were embedded in the PANI shells of the CNF/PANI composites, which might decrease the electrocatalyst activity. TEM-energy dispersive spectroscopy mapping confirmed that the Pt nanoparticles in the inner tube of N-doped hollow CNFs could be accessed by the Nafion ionomer electrolyte, contributing to the catalytic oxidation of methanol. PMID:22385930

  14. In situ TEM studies of carbon and gold nanostructures

    NASA Astrophysics Data System (ADS)

    Casillas Garcia, Gilberto

    Properties of matter change as structures go down in size to the nanoscale, creating new possibilities for creating new functional materials with better properties than the bulk. In situ TEM techniques were used to probe the properties of two different materials: atomic carbon chains and gold nanoparticles. Carbon chains were synthesized by in situ TEM electron beam irradiation from few-layers-graphene (FLG) flakes. Several chains up to 5 nm long were observed. Aberration corrected TEM confirmed the dimerization of the linear chain as predicted by Peierls. Moreover, it was observed that two linear carbon chains can cross-bond every 9 atoms, and it was confirmed by DFT calculations. Five-fold nanoparticles are not supposed to be stable beyond 5 nm size. Here, decahedra with high index facets in the order of 300 nm were studied by TEM. It was found that the high index facets were only stable by adding a capping agent, otherwise, smooth edges were observed. In this case, a (5x1) hexagonal surface reconstruction was observed on the {001} surfaces, with the hexagonal strings along a [110] and a [410] direction. Additionally, mechanical properties of gold nanoparticles, with and without twin boundaries, under 100 nm were measured by in situ TEM compression experiments. All of the nanoparticles presented yield strengths in the order of GPa. Multi twinned nanoparticles were found to be more malleable, reaching real compressing strains of 100 %, while the single crystal nanoparticle presented less plastic flow. Molecular dynamics simulations revealed that the twin boundaries contribute to the malleability of the nanoparticles, at the same time it provides a mechanism to stop dislocations, hence, strain hardening the nanoparticle at later stages of compression. Finally, the behavior of a single grain boundary was studied by in situ TEM manipulation of nanoparticles. A liquid-like behavior of a grain boundary is observed after two 40 nm gold nanoparticles are brought to

  15. The mineralogy and chemistry analyser (MARS-XRD) for the ExoMars 2018 mission

    NASA Astrophysics Data System (ADS)

    Marinangeli, L.; Hutchinson, I. B.; Stevoli, A.; Adami, G.; Ambrosi, R.; Amils, R.; Assis Fernandes, V.; Baliva, A.; Basilevsky, A. T.; Benedix, G.; Bland, P.; Böttger, A. J.; Bridges, J.; Caprarelli, G.; Cressey, G.; Critani, F.; D'Alessandro, N.; Delhez, R.; Domeneghetti, C.; Fernandez-Remolar, D.; Filippone, R.; Fioretti, A. M.; Garcia Ruiz, J. M.; Gilmore, M.; Hansford, G. M.; Iezzi, G.; Ingley, R.; Ivanov, M.; Marseguerra, G.; Moroz, L.; Pelliciari, C.; Petrinca, P.; Piluso, E.; Pompilio, L.; Sykes, J.; Westall, F.

    2011-10-01

    The Mineralogy and Chemistry Analyser (MARSXRD) is a miniaturised X-ray diffraction and fluorescence (XRD/XRF) spectrometer aimed to the mineralogical characterisation of Martian rocks. Simultaneously, MARS-XRD is able to acquire the diffraction pattern for mineralogical phases identification and the X-ray fluorescence spectrum for the chemical species, providing a complete rock characterization. The X-ray diffractometer (XRD) is the routine instrument used in every Earth Science laboratory to provide the mineralogical composition of rocks. XRD produces unequivocal results because it is based on the recognition of the geometrical properties of the crystal lattice. This kind of investigation is an extremely useful tool to define the textural and petro-mineralogical characteristics of the Martian rocks or soils and provide information on the past Martian environment conditions related to life. The analytic range we plan to cover includes all the silicate minerals, from clays or other phyllosilicates characterised by high interplanar lattice distance, to oxide and carbonates or evaporates (mainly sulphates). This rock spectrum is what we expect to be the target for exobiological exploration. These data will be integrated with those obtained by elemental analysis, in order to determine the exact elemental chemistry characterization of rock components. As mineralogy can be unambiguously derived from XRD analysis, it is probably our most powerful tool for distinguishing targets of biologic importance. In summary, the main scientific objectives of the proposed XRD/XRF instrument, Mars-XRD, are: - In situ determination of the mineral paragenesis of rock samples; - The characterization of the origin of rock samples; - Determination of alteration processes; - Understanding the exobiological potential of the samples. The hardware is developed by the Thales Alenia Space Italia with an important contribution of the Univ. of Leicester for the detection system.

  16. Effects of diagnostic ionizing radiation on pregnancy via TEM

    NASA Astrophysics Data System (ADS)

    Mohammed, W. H.; Artoli, A. M.

    2008-08-01

    In Sudan, X-rays are routinely used at least once for measurements of pelvis during the gestation period, though this is highly prohibited worldwide, except for a few life threatening cases. To demonstrate the effect of diagnostic ionizing radiation on uterus, fetus and neighboring tissues to the ovaries, two independent experiments on pregnant rabbits were conducted. The first experiment was a proof of concept that diagnostic ionizing radiation is hazardous throughout the gestation period. The second experiment was done through Transmission Electron Microscopy (TEM) to elucidate the morphological changes in the ultra structure of samples taken from irradiated pregnant rabbits. This study uses TEM to test the effect of diagnostic radiation of less than 0.6 Gray on the cellular level. Morphological changes have been captured and the images were analyzed to quantify these effects.

  17. Plastic deformation in zirconium nitride observed by nanoindentation and TEM

    NASA Astrophysics Data System (ADS)

    Egeland, G. W.; Wheeler, K.; Peralta, P.; McClellan, K. J.; Maloy, S. A.; Bond, G. M.

    2011-09-01

    A study on zirconium nitride using TEM and nanoindentation was performed to assess the significant surface plasticity found to be introduced by sample polishing. Cross-sectional TEM results show strong evidence of plasticity via dislocations produced directly from surface grinding and polishing. These dislocations were found to glide on the {0 1 1}<0 1¯ 1> slip system. Using nanoindentation to observe the effects of surface dislocation density, a critical shear stress was found that relates to dislocations nucleation and multiplication. Continued chemo-mechanical polishing increased the critical shear stress to approximately 1600 mN by reducing surface dislocations. It is postulated that vacancy clusters and oxide microcrystallites produced during surface processing provide dislocation nucleation and/or multiplication sites. Gentle chemo-mechanical polishing for several hours greatly reduced or eliminated preexisting dislocations such that the critical shear stress for nucleation approaches the theoretical limit (˜ G/5).

  18. Development of an analytical environmental TEM system and its application.

    PubMed

    Kishita, Keisuke; Sakai, Hisashi; Tanaka, Hiromochi; Saka, Hiroyasu; Kuroda, Kotaro; Sakamoto, Masayuki; Watabe, Akira; Kamino, Takeo

    2009-12-01

    Many automotive materials, such as catalysts and fuel cell materials, undergo significant changes in structure or properties when subjected to temperature change or the addition of a gas. For this reason, in the development of these materials, it is important to study the behavior of the material under controlled temperatures and gaseous atmospheres. Recently, a new environmental transmission electron microscope (TEM) has been developed for observation with a high resolution at high temperatures and under gaseous atmospheres, thus making it possible to analyze reaction processes in details. Also, the new TEM provides a high degree of reproducibility of observation conditions, thus making it possible to compare and validate observation of various specimens under a given set of conditions. Furthermore, easiness of gas condition and temperature control can provide a powerful tool for the studying of the mechanism of material change, such as oxidation and reduction reactions. PMID:19520735

  19. Comparing Time Domain Electromagnetics (TEM) and Early-Time TEM for Mapping Highly Conductive Groundwater in Mars Analog Environments

    NASA Astrophysics Data System (ADS)

    Jernsletten, J. A.

    2005-05-01

    Introduction: The purpose of this study is to evaluate the use of (diffusive) Time Domain Electromagnetics (TEM) for sounding of subsurface water in conductive Mars analog environments. To provide a baseline for such studies, I show data from two field studies: 1) Diffusive sounding data (TEM) from Pima County, Arizona; and 2) Shallower sounding data using the Fast-Turnoff TEM method from Peña de Hierro in the Rio Tinto region of Spain. The latter is data from work conducted under the auspices of the Mars Analog Research and Technology Experiment (MARTE). Pima County TEM Survey: A TEM survey was carried out in Pima County, Arizona, in January 2003. Data was collected using 100 m Tx loops and a ferrite-cored magnetic coil Rx antenna, and processed using commercial software. The survey used a 16 Hz sounding frequency, which is sensitive to slightly salty groundwater. Prominent features in the data from Arizona are the ~500 m depth of investigation and the ~120 m depth to the water table, confirmed by data from four USGS test wells surrounding the field area. Note also the conductive (~20-40 ω m) clay-rich soil above the water table. Rio Tinto Fast-Turnoff TEM Survey: During May and June of 2003, a Fast-Turnoff (early time) TEM survey was carried out at the Peña de Hierro field area of the MARTE project, near the town of Nerva, Spain. Data was collected using 20 m and 40 m Tx loop antennae and 10 m loop Rx antennae, with a 32 Hz sounding frequency. Data from Line 4 (of 16) from this survey, collected using 40 m Tx loops, show ~200 m depth of investigation and a conductive high at ~90 m depth below Station 20 (second station of 10 along this line). This is the water table, matching the 431 m MSL elevation of the nearby pit lake. The center of the "pileup" below Station 60 is spatially coincident with the vertical fault plane located here. Data from Line 15 and Line 14 of the Rio Tinto survey, collected using 20 m Tx loops, achieve ~50 m depth of investigation and

  20. Microstructural Study of Superhard Coatings With TEM And SEM

    SciTech Connect

    Chaliampalias, D.; Vourlias, G.; Pistofidis, N.; Tsiaoussis, I.; Pavlidou, E.; Stergioudis, G.; Polychroniadis, E. K.; Kolaklieva, L.; Kakanakov, R.

    2007-04-23

    In the present work, TiN was deposited on stainless steel (SS420) using the cathode-spot arc method and the effect of the N2 flow and the chamber pressure on the coating microstructure was studied. TEM examination showed a columnar growth of TiN crystals with different size, while the average thickness was about 0.7 to 1.05 {mu}m and increased as the chamber pressure increased.

  1. Application of particle analysis to transmission electron microscopy (TEM)

    NASA Astrophysics Data System (ADS)

    DaPonte, J.; Sadowski, T.; Broadbridge, C. C.; Day, D.; Lehman, A. H.; Krishna, D.; Marinella, L.; Munhutu, P.; Sawicki, M.

    2007-04-01

    Nanoparticles, particles with a diameter of 1-100 nanometers (nm), are of interest in many applications including device fabrication, quantum computing, and sensing because their size may give them properties that are very different from bulk materials. Further advancement of nanotechnology cannot be obtained without an increased understanding of nanoparticle properties such as size (diameter) and size distribution frequently evaluated using transmission electron microscopy (TEM). In the past, these parameters have been obtained from digitized TEM images by manually measuring and counting many of these nanoparticles, a task that is highly subjective and labor intensive. More recently, computer imaging particle analysis has emerged as an objective alternative by counting and measuring objects in a binary image. This paper will describe the procedures used to preprocess a set of gray scale TEM images so that they could be correctly thresholded into binary images. This allows for a more accurate assessment of the size and frequency (size distribution) of nanoparticles. Several preprocessing methods including pseudo flat field correction and rolling ball background correction were investigated with the rolling ball algorithm yielding the best results. Examples of particle analysis will be presented for different types of materials and different magnifications. In addition, a method based on the results of particle analysis for identifying and removing small noise particles will be discussed. This filtering technique is based on identifying the location of small particles in the binary image and removing them without affecting the size of other larger particles.

  2. TEM and XPS studies on CdS/CIGS interfaces

    NASA Astrophysics Data System (ADS)

    Han, Jun-feng; Liao, Cheng; Cha, Li-mei; Jiang, Tao; Xie, Hua-mu; Zhao, Kui; Besland, M.-P.

    2014-12-01

    Copper indium gallium selenide (CIGS) was deposited by metallic precursors sputtering and subsequently submitted to a selenization process. The upper CdS layers were deposited by chemical bath deposition (CBD) technique. The CdS/CIGS interfaces were investigated by Transmission Electron Microscopy (TEM) and X-ray Photoelectron Spectroscopy (XPS). As checked by XPS analysis, the CIGS surface exhibited a hydroxide-terminated CdSe layer when treated with Cd Partial Electrolyte solution (Cd PE). Its thickness was roughly estimated to several nanometers. A 100 nm thick CdS layer was deposited onto CIGS surface. The TEM images revealed a clear and sharp interface between CdS and CIGS. XPS analysis showed a CIGS surface covered by a pinhole free and homogeneous CdS layer. XPS depth profile measurement of the CdS/CIGS interface did not evidence elemental inter-diffusion between the CIGS and CdS layers, in very good agreement with TEM observations.

  3. Characterization of some biological specimens using TEM and SEM

    NASA Astrophysics Data System (ADS)

    Ghosh, Nabarun; Smith, Don W.

    2009-05-01

    The advent of novel techniques using the Transmission and Scanning Electron Microscopes improved observation on various biological specimens to characterize them. We studied some biological specimens using Transmission and Scanning Electron Microscopes. We followed negative staining technique with Phosphotungstic acid using bacterial culture of Bacillus subtilis. Negative staining is very convenient technique to view the structural morphology of different samples including bacteria, phage viruses and filaments in a cell. We could observe the bacterial cell wall and flagellum very well when trapped the negative stained biofilm from bacterial culture on a TEM grid. We cut ultra thin sections from the fixed root tips of Pisum sativum (Garden pea). Root tips were pre fixed with osmium tetroxide and post fixed with uranium acetate and placed in the BEEM capsule for block making. The ultrathin sections on the grid under TEM showed the granular chromatin in the nucleus. The protein bodies and large vacuoles with the storage materials were conspicuous. We followed fixation, critical point drying and sputter coating with gold to view the tissues with SEM after placing on stubs. SEM view of the leaf surface of a dangerous weed Tragia hispida showed the surface trichomes. These trichomes when break on touching releases poisonous content causing skin irritation. The cultured tissue from in vitro culture of Albizia lebbeck, a tree revealed the regenerative structures including leaf buds and stomata on the tissue surface. SEM and TEM allow investigating the minute details characteristic morphological features that can be used for classroom teaching.

  4. Observations from TEM Analysis of Swift Creek Samples

    NASA Astrophysics Data System (ADS)

    Harris, J. R.

    2012-12-01

    Samples analyzed by transmission electron microscopy (TEM) from suspended sediments in Swift Creek have unique characteristics compared to other naturally occurring asbestos (NOA) sites across the country. Our first introduction to the uniqueness of the Swift Creek site came about when we analyzed soil sediments by polarized light microscopy (PLM) and found relatively low or nonexistent levels of chrysotile asbestos. Upon submission of these samples for TEM analysis, we found that the samples were literally filled with small chrysotile fibers and bundles. We also notice a high number of dark, rounded particles which were not asbestiform. Out of curiosity, we viewed the surface features of one of these particles using scanning electron microscopy to find compacted chrysotile fibers bundled inside these particles. These particles contained the vast majority of chrysotile in the sample. This finding began our approach to provide more advanced TEM/SEM methods for identifying and characterizing complex arrangements of asbestos from NOA sites. We will present some of our experiences and methods for characterizing these types of particles common to NOA sites.

  5. A TEM study of samples from acid mine drainage systems: metal-mineral association with implications for transport

    NASA Astrophysics Data System (ADS)

    Hochella, Michael F.; Moore, Johnnie N.; Golla, Ute; Putnis, Andrew

    1999-10-01

    Transmission electron microscopy (TEM), with energy dispersive X-ray (EDX) analysis and energy filtered transmission electron microscopy/electron energy loss spectroscopy (EFTEM/EELS), as well as powder X-ray diffraction (XRD) and scanning electron microscopy (SEM), have been used to study bed sediments from two acid mine drainage (AMD) sites in western Montana, USA. TEM and associated techniques, including sample preparation via epoxy impregnation and ultramicrotome sectioning, afford the opportunity to better interpret and understand complex water-rock interactions in these types of samples. For the sample taken from the first site (Mike Horse mine), ferrihydrite is the dominant phase, Si and Zn are the most abundant elements sorbed to ferrihydrite surfaces, and Pb is notably absent from ferrihydrite association. Three additional important metal-containing phases (gahnite, hydrohetaerolite, and plumbojarosite), that were not apparent in the powder XRD pattern because of their relatively low concentration, were identified in the TEM. The presence of these phases is important, because, for example, gahnite and plumbojarosite act as sinks for Zn and Pb, respectively. Therefore, the mobility of Pb from this part of the drainage system depends on the stability of plumbojarosite and the ability of ferrihydrite to sorb the released Pb. From thermodynamic data in the literature, we predict that Pb will be released by the dissolution of plumbojarosite above a pH of 4 to 5, but it will then be recaptured by ferrihydrite if the pH continues to rise to 5.5 and higher, irrespective of competition effects from other metals. Therefore, only a relatively narrow pH window exists in which Pb can escape this portion of the system as an aqueous species. For the sample taken from the other site included in this study (the Carbonate mine), jarosite and quartz are the dominant phases. Interestingly, however, the jarosites are both Pb-poor and Pb-enriched. In addition, TEM reveals the

  6. Response Time Measurements of the NIF DANTE XRD-31 X-Ray Diodes (Pre-print)

    SciTech Connect

    Don Pellinen and Michael Griffin

    2009-01-23

    The XRD-31 is a fast, windowless X-ray vacuum photodiode developed by EG&G. It is currently the primary fast X-ray detector used to diagnose the X-rays on NIF and OMEGA on the multichannel DANTE spectrometer. The XRD-31 has a dynamic range of less than 1e-12 amps to more than 10 amps. A technique is described to measure the impulse response of the diodes to a 150 fs pulse of 200 nm laser light and a method to calculate the “risetime” for a square pulse and compare it with the computed electron transit time from the photocathode to the anode. Measured response time for 5 XRD-31s assembled in early 2004 was 149.7 ps +-2.75 ps.

  7. Definitive Mineralogical Analysis of Mars Analog Rocks Using the CheMin XRD/XRF Instrument

    NASA Technical Reports Server (NTRS)

    Blake, D. F.; Sarrazin, P.; Bish, D. L.; Feldman, S.; Chipera, S. J.; Vaniman, D. T.; Collins, S.

    2004-01-01

    Mineral identification is a critical component of Mars Astrobiological missions. Chemical or elemental data alone are not definitive because a single elemental or chemical composition or even a single bonding type can represent a range of substances or mineral assemblages. Minerals are defined as unique structural and compositional phases that occur naturally. There are about 15,000 minerals that have been described on Earth, all uniquely identifiable via diffraction methods. There are likely many minerals yet undiscovered on Earth, and likewise on Mars. If an unknown phase is identified on Mars, it can be fully characterized by structural (X-ray Diffraction, XRD) and elemental analysis (X-ray Fluorescence, XRF) without recourse to other data because XRD relies on the principles of atomic arrangement for its determinations. XRD is the principal means of identification and characterization of minerals on Earth.

  8. Data acquisition and control software for XRD beamline at Indus-2

    NASA Astrophysics Data System (ADS)

    Kane, Sanjeev R.; Garg, C. K.; Sinha, A. K.

    2010-06-01

    X-ray diffraction (XRD) beamline is under commissioning on Indus-2 synchrotron radiation facility. The experimental setup of XRD beamline consists of a six-circle diffractometer and various detector systems such as scintillation detector, ionization chamber and image plate. The diffractometer can be controlled via EIA232 serial interface or Ethernet. Standard data acquisition software with a graphical user interface has been developed using LabVIEW. A firm safety and error handling scheme is implemented for failsafe operation of the experimental station. This paper describes in detail the data acquisition and control software for the experimental station.

  9. Data acquisition and control software for XRD beamline at Indus-2

    SciTech Connect

    Kane, Sanjeev R.; Garg, C. K.; Sinha, A. K.

    2010-06-23

    X-ray diffraction (XRD) beamline is under commissioning on Indus-2 synchrotron radiation facility. The experimental setup of XRD beamline consists of a six-circle diffractometer and various detector systems such as scintillation detector, ionization chamber and image plate. The diffractometer can be controlled via EIA232 serial interface or Ethernet. Standard data acquisition software with a graphical user interface has been developed using LabVIEW. A firm safety and error handling scheme is implemented for failsafe operation of the experimental station. This paper describes in detail the data acquisition and control software for the experimental station.

  10. Hydride phase formation in carbon supported palladium hydride nanoparticles by in situ EXAFS and XRD

    NASA Astrophysics Data System (ADS)

    Bugaev, A. L.; Guda, A. A.; Lomachenko, K. A.; Lazzarini, A.; Srabionyan, V. V.; Vitillo, J. G.; Piovano, A.; Groppo, E.; Bugaev, L. A.; Soldatov, A. V.; Dmitriev, V. P.; Pellegrini, R.; van Bokhoven, J. A.; Lamberti, C.

    2016-05-01

    In the current work we present a detailed analysis of the hydride phase formation in industrial Pd/C nanocatalysts by means of combined in situ X-ray absorption spectroscopy (EXAFS), X-ray diffraction (XRD) and volumetric measurements for the temperatures from - 10 to 50 °C in the hydrogen pressure range from 0 to 1000 mbar. α- and β- hydride phases are clearly distinguished in XRD. For the first time, H/Pd atomic ratio were obtained by theoretical fitting of the near-edge region of the absorption spectra (XANES) and compared with volumetric measurements.

  11. TEM Pump With External Heat Source And Sink

    NASA Technical Reports Server (NTRS)

    Nesmith, Bill J.

    1991-01-01

    Proposed thermoelectric/electromagnetic (TEM) pump driven by external source of heat and by two or more heat pipe radiator heat sink(s). Thermoelectrics generate electrical current to circulate liquid metal in secondary loop of two-fluid-loop system. Intended for use with space and terrestrial dual loop liquid metal nuclear reactors. Applications include spacecraft on long missions or terrestrial beacons or scientific instruments having to operate in remote areas for long times. Design modified to include multiple radiators, converters, and ducts, as dictated by particular application.

  12. Modeling of planar quasi-TEM superconducting transmission lines

    NASA Technical Reports Server (NTRS)

    Antsos, Dimitrios; Chew, Wilbert; Riley, A. L.; Hunt, Brian D.; Foote, Marc C.; Bajuk, Louis J.; Rascoe, Daniel L.; Cooley, Thomas W.

    1992-01-01

    An application of the phenomenological loss equivalence method (Lee and Itoh, 1989) in modeling the microwave behavior of planar quasi-TEM superconducting transmission lines is presented. For validation of the model, data are used from measurements of a YBCO superconducting thin-film coplanar-waveguide lowpass filter on a lanthanum aluminate substrate. Measured and modeled S-parameters of an existing superconducting coplanar waveguide lowpass filter agree to within 0.3 dB in magnitude and 0.5 radians in phase. Extracted values for penetration depth and real part of the conductivity of the superconducting film are within 10 percent of other researchers' findings.

  13. Preparation of TEM samples for hard ceramic powders.

    PubMed

    Xu, Qiang; Kumar, Vikas; de Kruijff, Tom; Jansen, Jacob; Zandbergen, Henny W

    2008-12-01

    It is challenging to prepare a good sample for high-resolution electron microscopy of polycrystalline ceramic powders containing hard particles or particles with a strong preferential cleavage. Here we demonstrate that embedding the particles in a Cu matrix in a pressed pellet allows for straightforward conventional ion milling. The method is applied to powders of Mg10Ir19B16 and Na0.5CoO2 to show its feasibility, whereby transmission electron microscopy (TEM) samples with crystalline areas thinner than 10 nm can be obtained easily. PMID:18722061

  14. TEM investigations on the local microstructure of electrodeposited galfenol nanowires.

    PubMed

    Pohl, D; Damm, C; Pohl, D; Schultz, L; Schlörb, H

    2016-01-22

    The local microstructure of Fe-Ga nanowires is investigated considering dependence on the deposition technique. Using a complexed electrolyte, smooth and homogeneous Fe80Ga20 nanowires are deposited into anodic aluminum oxide templates by either applying pulse potential or potentiostatic deposition technique. At optimized deposition conditions the wires show the desired composition of Fe80±2Ga20±2 without a gradient along the growth direction. Composition distribution, structure and microstructure are examined in detail and reveal only minor differences. Line EELS and crystal lattice measurements reveal a negligible oxygen content for both preparation routines. Neither Fe/Ga oxides nor hydroxides were found. Both potentiostatically deposited as well as pulse deposited nanowires exhibit a preferred 〈110〉orientation, the latter with slightly larger crystals. Different contrast patterns were found by TEM that appear more pronounced in the case of pulse deposited wires. High resolution transmission electron microscopy analysis and comparison of differently prepared focused ion beam lamellas reveal that these contrasts are caused by defects in the alternating potential deposition itself and are not induced during the TEM preparation process. The alternating potential mode causes periodic growth thereby inducing different layers with reduced wire thickness/defects at the layer interfaces. PMID:26651087

  15. TEM investigations on the local microstructure of electrodeposited galfenol nanowires

    NASA Astrophysics Data System (ADS)

    Pohl, D.; Damm, C.; Pohl, D.; Schultz, L.; Schlörb, H.

    2016-01-01

    The local microstructure of Fe-Ga nanowires is investigated considering dependence on the deposition technique. Using a complexed electrolyte, smooth and homogeneous Fe80Ga20 nanowires are deposited into anodic aluminum oxide templates by either applying pulse potential or potentiostatic deposition technique. At optimized deposition conditions the wires show the desired composition of Fe80±2Ga20±2 without a gradient along the growth direction. Composition distribution, structure and microstructure are examined in detail and reveal only minor differences. Line EELS and crystal lattice measurements reveal a negligible oxygen content for both preparation routines. Neither Fe/Ga oxides nor hydroxides were found. Both potentiostatically deposited as well as pulse deposited nanowires exhibit a preferred <110> orientation, the latter with slightly larger crystals. Different contrast patterns were found by TEM that appear more pronounced in the case of pulse deposited wires. High resolution transmission electron microscopy analysis and comparison of differently prepared focused ion beam lamellas reveal that these contrasts are caused by defects in the alternating potential deposition itself and are not induced during the TEM preparation process. The alternating potential mode causes periodic growth thereby inducing different layers with reduced wire thickness/defects at the layer interfaces.

  16. Performance of membrane filters used for TEM analysis of asbestos.

    PubMed

    Webber, James S; Czuhanich, Alex G; Carhart, Laurie J

    2007-10-01

    This article presents findings related to characteristics of membrane filters that can affect the recovery of asbestos and the quality of preparations for transmission electron microscopy (TEM) analysis. Certain applications and preparation steps can lead to unacceptable performance of membrane filters used in analysis of asbestos by TEM. Unless substantial care is used in the collapsing of mixed-cellulose ester (MCE) filters with an acetone hot block, grid preparations can suffer and fiber recoveries can be compromised. Calibration of the etching depth of MCE filters, especially at differing locations in an asher's chamber, is critical for reliable fiber recovery. Excessive etching of MCE filters with aerosol-deposited asbestos can lead to loss of short fibers, while insufficient etching of MCE filters with aqueous-deposited asbestos can, paradoxically, also lead to loss of short fibers. Interlaboratory precision on MCE filters is improved by aerosol-deposited asbestos, as opposed to aqueous deposition. In comparison, straightforward preparation, improved solvents, and reduced contamination make PC filters an increasingly acceptable alternative. Variations in the geometric configuration during application of carbon films can lead to fiber loss and unacceptable grid quality for either type of filter. PMID:17763069

  17. Studying dynamic processes in liquids by TEM/STEM/DTEM

    NASA Astrophysics Data System (ADS)

    Abellan, Patricia; Evans, James; Woehl, Taylor; Jungjohann, Katherine; Parent, Lucas; Arslan, Ilke; Ristenpart, William; Browning, Nigel; Mater. Sci. Group Team; Microsc. Group Team; Catal. Sci. Group Collaboration; Ristenpart Res. Group Collaboration

    2013-03-01

    In order to study dynamic phenomena such as corrosion or catalysis, extreme environmental conditions must be reproduced around the specimen - these include high-temperatures, high-pressures, specific oxidizing/reducing atmospheres or a liquid environment. The use of environmental stages specifically designed to fit in any transmission electron microscope (TEM) allows us to apply the distinct capabilities of each instrument to study dynamic processes. Localized gas/fluid conditions are created around the sample and separated from the high vacuum inside the microscope using hermetically sealed windowed-cells. Advanced capabilities of these techniques include spatial resolutions of ~1 Angstrom or better in aberration corrected instruments or temporal resolutions in the microsecond-nanosecond range in a dynamic TEM (DTEM). Here, unique qualities of the DTEM that benefit the in-situ experiments with gas/fluid environmental cells will be discussed. We also present our results with a liquid stage allowing atomic resolution imaging of nanomaterials in a colloidal suspension, core EEL spectra acquisition, continuous flow, controlled growth of nanocrystals and systematic calibration of the effect of the electron dose on silver nuclei formation.

  18. (S)TEM analysis of functional transition metal oxides

    NASA Astrophysics Data System (ADS)

    Chi, Miaofang

    Perovskite vanadates (AVO3) form an ideal family to study the structure-property relationships in transition metal oxides because their physical properties can easily be tailored by varying the A-site cations. (S)TEM is an ideal tool for this type of study due to its capacity for simultaneous imaging and chemical analysis. Determination of the oxidation state of vanadium in complex oxides have been carried out by electron energy loss spectroscopy. SrVO3/LaAlO3 is then studied both experimentally and theoretically as a prototype system. Extra electrons have been detected on the interface layer, and further proven to originate mainly from a change in the local bonding configuration of V at the La-O terminated substrate surface. Cr-containing stainless steel deposited with a LaCrO3 thin-film layer is a promising interconnect material of Solid Oxide Fuel Cells (SOFC). Our investigation on its microstructural evolution reveals that the LaCrO 3 thin film plays a role in inhibiting the growth of an oxide layer on the metal surface and thus protects the surface of the stainless steel. Ca-doped LaCoO3 is a promising SOFC cathode material. The domain structures and the oxidation state of Co in Ca-doped LaCoO3, which are directly related to its mechanical properties and electronic conductivity, are investigated by in-situ TEM and EELS. The formation of microcracks is observed during thermal cycles. Ca-doping in LaCoO3 is shown to not only improve the electronic conductivity of the material, but is also likely to strengthen the grain boundaries. The realization of its application in SOFCs depends on depressing the ferroelastisity to reduce strain formation during thermal cycles. The application of the (S)TEM techniques used for studying the perovskite systems are further extended to other compounds containing transition metal elements. The refractory minerals from Comet 81 P/Wild-2 are studied to investigate the formation of the early solar system. A relatively high Ti3+/Ti 4

  19. A TEM analysis of nanoparticulates in a Polar ice core

    SciTech Connect

    Esquivel, E.V.; Murr, L.E

    2004-03-15

    This paper explores the prospect for analyzing nanoparticulates in age-dated ice cores representing times in antiquity to establish a historical reference for atmospheric particulate regimes. Analytical transmission electron microscope (TEM) techniques were utilized to observe representative ice-melt water drops dried down on carbon/formvar or similar coated grids. A 10,000-year-old Greenland ice core was melted, and representative water drops were transferred to coated grids in a clean room environment. Essentially, all particulates observed were aggregates and either crystalline or complex mixtures of nanocrystals. Especially notable was the observation of carbon nanotubes and related fullerene-like nanocrystal forms. These observations are similar with some aspects of contemporary airborne particulates including carbon nanotubes and complex nanocrystal aggregates.

  20. Analysis of the Tem Mode Linearly Tapered Slot Antenna

    NASA Technical Reports Server (NTRS)

    Janaswamy, R.; Schaubert, D. H.; Pozar, D. M.

    1985-01-01

    The theoretical analysis of the radiation characteristics of the TEM mode Linearly Tapered Slot Antenna (LTSA) is presented. The theory presented is valid for antennas with air dielectric and forms the basis for analysis of the more popular dielectric-supported antennas. The method of analysis involves two steps. In the first step, the aperture distribution in the flared slot is determined. In the second step, the equivalent magnetic current in the slot is treated as radiating in the presence of a conducting half-plane and the far-field components are obtained. Detailed comparison with experiment is made and excellent agreement is obtained. Design curves for the variation of the 3 dB and 10 dB beamwidths as a function of the antenna length, with the flare angle as a parameter, are presented.

  1. Examination of subaerially altered basaltic glass with TEM and EELS

    SciTech Connect

    Luo, J.-S.

    1998-06-17

    We have examined the weathered surfaces of 720 year old Hawaiian basalt glasses that were recovered from a subaerial environment with high-resolution transmission electron microscopy (TEM) and energy filtered imaging and electron energy loss spectroscopy (EELS) techniques. Whereas the alteration products (palagonite) were physically detached from the underlying glass in most samples, a gel-like amorphous layer was observed adjacent to the glass in a few samples. To our knowledge, this is the first time a gel layer has been observed on weathered basalt. This is significant because analogous gel layers have been observed on nuclear waste glasses reacted in laboratory tests, and this demonstrates an important similarity in the mechanisms of the weathering of basalt and the corrosion of waste glasses.

  2. Localized ion milling of metallic and ceramic TEM specimens

    SciTech Connect

    Fisher, A.T.; Bentley, J.

    1986-01-01

    The utility of localized ion milling in the preparation of metallic and ceramic specimens for TEM and AEM is being evaluated from the standpoint of optimizing procedures and identifying limitations and milling characteristics. The equipment used was a Gatan model 645 precision ion milling system (PIMS). This device is a scanning ion beam instrument with which selected areas of a sample can be imaged by either secondary electron or secondary ion signals and selectively ion milled in a small region within the imaged area. The 1 to 10 keV ion beam can be focussed to a 2 ..mu..m spot. Specimens are thinned without removing them from the electron microscope specimen holder.

  3. TEM observations of hydrogen nanobubbles in implanted amorphous silicon

    SciTech Connect

    Jones, K.M.; Al-Jassim, M.M.; Williamson, D.L.; Acco, S.

    1996-12-31

    Over the last two decades extensive studies on the optical and electrical properties of hydrogenated amorphous Si (a-Si:H) have been reported. However, less attention was given to the structural characterization of this material partly due to the insensitivity to hydrogen of structural probes such as x-rays and electron diffraction. From a recent set of experiments, results on the solubility limit of hydrogen in a special type of a-Si:H and the characterization of hydrogen induced complexes or nanobubbles has been reported. In this study, we report TEM observations of the structural morphology of hydrogen related defects that support these recent measurements obtained by secondary ion mass spectrometry (SIMS) and small-angle x-ray scattering (SAXS).

  4. FIM/IAP/TEM studies of ion implanted nickel emitters

    SciTech Connect

    Walck, S.D.; Hren, J.J.

    1985-01-01

    Accurate depth profiling of implanted hydrogen and its isotopes in metals is extremely important. Field ion microscopy and atom-probe techniques provide the most accurate depth profiling analytical method of any available. In addition, they are extremely sensitive to hydrogen. This paper reports our early work on hydrogen trapping at defects in metals using the Field Ion Microscope/Imaging Atom Probe (FIM/IAP). Our results deal primarily with the control experiments required to overcome instrumental difficulties associated with in situ implantation and the influence of a high electric field. Transmission Electron Microscopy (TEM) has been used extensively to independently examine the influence of high electric fields on emitters. 11 references, 7 figures.

  5. Correlation Analysis of TEM Images of Nanocrystal Molecules

    SciTech Connect

    Micheel, Christine; Zanchet, Daniele; Alivisatos, A. Paul

    2008-05-21

    Quantitative characterizataion of images of naocrystals and nanostructures is a challenging but important task. The development and optimization of methods for the construction of complex nanostructures rely on imaging techniques. Computer programs were developed to quantify TEM images of nanocrystal/DNA nanostructures, and results are presented for heterodimers annd trimers of gold nanocrystals. The programs presented here have also been used to analyze more complex trimers and tetramers linked by branched DNA, as well as for structures made from attaching gold nanocrystals to CdSe/ZnS core-shell quantum dots. This work has the additional goal of enabling others to quickly and easily adapt the methods for their own use.

  6. Identification of cooked bone using TEM imaging of bone collagen.

    PubMed

    Koon, Hannah E C

    2012-01-01

    Mild heating (≤100° C, 1 h)-typical of cooking-does not lead to detectable changes in any biochemical parameter yet measured; consequently bones that have been cooked, but which have not reached a temperature that will induce charring go undetected. We have used a microscopy based approach to investigate changes in the organization of the bone protein, collagen, as it is heated, using bone from heating experiments, short term burials, and archaeological sites. The work has revealed that the presence of a mineral matrix stabilizes the collagen enabling the damage to accumulate, but preventing it from causing immediate gelatinization. Once the mineral is removed, the damage can be observed using appropriate visualization methods. This chapter describes the transmission electron microscopy (TEM) technique that has been used to detect cooked bone by visualizing minor heat-induced damage at the level of the collagen fibril. PMID:22907413

  7. Transmission Electron Microscopy (TEM) investigations of ancient Egyptian cosmetic powders

    NASA Astrophysics Data System (ADS)

    Deeb, C.; Walter, P.; Castaing, J.; Penhoud, P.; Veyssière, P.

    The processing technologies available during the time of ancient Egypt are of present concern to the field of Archaeology and Egyptology. Materials characterization is the best tool for establishing the processing history of archaeological objects. In this study, transmission electron microscopy (TEM) is used, in addition to other techniques, for phase identification and study of the microstructure and characteristic defect structures in ancient Egyptian cosmetic powders. These powders generally consist of a mix of Pb-containing mineral phases: galena (PbS), cerussite (PbCO3), and phosgenite (Pb2Cl2CO3), among others. Modern materials are fabricated according to recipes found in ancient texts to mimic the processing of ancient times and to compare with the archaeological specimens. In particular, a comparison between the dislocation structures of PbS crystals deformed in the laboratory and PbS from archaeological specimens from the collections of the Louvre Museum is presented .

  8. Enabling direct nanoscale observations of biological reactions with dynamic TEM

    PubMed Central

    Evans, James E.; Browning, Nigel D.

    2013-01-01

    Biological processes occur on a wide range of spatial and temporal scales: from femtoseconds to hours and from angstroms to meters. Many new biological insights can be expected from a better understanding of the processes that occur on these very fast and very small scales. In this regard, new instruments that use fast X-ray or electron pulses are expected to reveal novel mechanistic details for macromolecular protein dynamics. To ensure that any observed conformational change is physiologically relevant and not constrained by 3D crystal packing, it would be preferable for experiments to utilize small protein samples such as single particles or 2D crystals that mimic the target protein's native environment. These samples are not typically amenable to X-ray analysis, but transmission electron microscopy has imaged such sample geometries for over 40 years using both direct imaging and diffraction modes. While conventional transmission electron microscopes (TEM) have visualized biological samples with atomic resolution in an arrested or frozen state, the recent development of the dynamic TEM (DTEM) extends electron microscopy into a dynamic regime using pump-probe imaging. A new second-generation DTEM, which is currently being constructed, has the potential to observe live biological processes with unprecedented spatiotemporal resolution by using pulsed electron packets to probe the sample on micro- and nanosecond timescales. This article reviews the experimental parameters necessary for coupling DTEM with in situ liquid microscopy to enable direct imaging of protein conformational dynamics in a fully hydrated environment and visualize reactions propagating in real time. PMID:23315566

  9. An alternative to the TEM (Transformed Eulerian Mean) equations

    NASA Astrophysics Data System (ADS)

    Gaßmann, Almut

    2013-04-01

    The TEM equations constitute a powerful means to get access to the residual circulation. However, due to their foundation on the wave perspective, they deliver only a zonally averaged picture without access to the three-dimensional structure or the local origins of the residual circulation. Therefore it is worth to investigate whether there are alternatives. The pathway followed here is to perform a transformation of the momentum and the potential temperature equation before taking the zonal mean. This is done by removing the steady state ideal wind solution vid = ?×?B-(?±P) from the equations (? - potential temperature, B - Bernoulli function, P - Ertel's potential vorticity EPV, ?± - density). The advantage of that approach is that the total EPV-flux does no longer contain an explicitly visible 'do-nothing-flux'. This flux, ?? ×?B, does only vanish when averaging on isentropic surfaces, but not on other isosurfaces. Here we find the reason why the conventional zonal mean on isentropes delivers a direct overturning cell on each hemisphere, whereas on other isosurfaces we obtain the typical three-cell structure with Headley, Ferrel, and polar cells. It will be demonstrated and made visible through idealized climate experiments with the ICON-IAP model that the zonal averages of the nonideal wind components vnid = v - vid and wnid = w - wid constitute similar direct overturning cells on non-isentropic surfaces as obtained with the TEM-generated v* and w*. It is also interesting to inspect fields of local nonideal wind components, the very origin of the residual circulation.

  10. A Raman, IR and XRD analysis of the deterioration on historical monuments: case study from Mexico.

    PubMed

    Ostrooumov, Mikhail

    2009-08-01

    Raman, infrared and XRD analysis have been applied to the examination of deterioration on historical monuments (Morelia, Mexico). Forty-three samples pyroclastic volcanic rocks (ignimbrites) have been studied, all originating from two ex-convents San Francisco and San Agustin, which were the first architectonic complexes in the city of Morelia. Several new mineral neoformation such as sulfates, carbonates, halides, and phosphates were identified in these samples with spectrometric and XRD technique. The observed Raman and infrared spectra are reported and some mineral compound assignments in unaltered and deteriorated volcanic rocks have been made. This survey is the first Raman and infrared spectrometric examination of the environmental mineralogy in Mexico under conditions of urban weathering that are characterized mainly by one secondary alteration formations of low scale. PMID:19201254

  11. Combined synchrotron XRD/Raman measurements: in situ identification of polymorphic transitions during crystallization processes.

    PubMed

    Klimakow, Maria; Leiterer, Jork; Kneipp, Janina; Rössler, Ernst; Panne, Ulrich; Rademann, Klaus; Emmerling, Franziska

    2010-07-01

    A combination of two analytical methods, time-resolved X-ray diffraction (XRD) and Raman spectroscopy, is presented as a novel tool for crystallization studies. An acoustic levitator was employed as sample environment. This setup enables the acquisition of XRD and Raman data in situ simultaneously within a 20 s period and hence permits investigation of polymorphic phase transitions during the crystallization process in different solvents (methanol, ethanol, acetone, dichloromethane, acetonitrile). These real time measurements allow the determination of the phase content from the onset of the first crystalline molecular assemblies to the stable system. To evaluate the capability of this approach, the setup was applied to elucidate the crystallization process of the polymorphic compound nifedipine. The results indicate the existence of solvent-dependent transient phases during the crystallization process. The quality of the data allowed the assignment of the lattice constants of the hitherto unknown crystal structure of the beta-polymorph. PMID:20222693

  12. Applying high resolution SyXRD analysis on sulfate attacked concrete field samples

    SciTech Connect

    Stroh, J.; Schlegel, M.-C.; Irassar, E.F.; Meng, B.; Emmerling, F.

    2014-12-15

    High resolution synchrotron X-ray diffraction (SyXRD) was applied for a microstructural profile analysis of concrete deterioration after sulfate attack. The cement matrices consist of ordinary Portland cement and different amounts of supplementary cementitious materials, such as fly ash, natural pozzolana and granulated blast furnace slag. The changes of the phase composition were determined along the direction of sulfate ingress. This approach allows the identification of reaction fronts and zones of different phase compositions and conclusions about the mechanisms of sulfate attack. Two reaction fronts were localized in the initial 4 mm from the sample surface. The mechanism of deterioration caused by the exposition in the sulfate-bearing soil is discussed. SyXRD is shown to be a reliable method for investigation of cementitious materials with aggregates embedded in natural environments.

  13. Characterising palladium-silver and palladium-nickel alloy membranes using SEM, XRD and PIXE

    NASA Astrophysics Data System (ADS)

    Keuler, J. N.; Lorenzen, L.; Sanderson, R. D.; Prozesky, V.; Przybylowicz, W. J.

    1999-10-01

    Palladium alloy membranes were prepared by successive electroless plating steps on an alumina-zirconia support membrane. Palladium, silver and nickel were deposited in layers and then the metal films were heat treated for 5 h in a hydrogen atmosphere at 650°C. The topography of the metal coatings and cross-sections of the films (before and after heating) were characterised using scanning electron microscopy (SEM). XRD was used to determine the crystal phase of the alloy coatings. Both SEM and XRD provide only surface information and therfore micro-PIXE was used to extract depth information of the alloy coating. Concentration profiles across the thickness of the films were constructed to determine penetration of the coating into the support membrane pores during electroless plating and to investigate diffusion of coated layers during the heating step.

  14. TEM-EDS study of metals' partition at particle level after their sorption in soil

    NASA Astrophysics Data System (ADS)

    Sipos, Peter; Kovács Kis, Viktória; Németh, Tibor; Balázs, Réka

    2016-04-01

    Association of soil mineral particles could significantly modify the sorption capacity of the individual soil components. We studied this phenomena using single element and competitive batch Cd, Cu, Pb and Zn sorption experiments on six soil samples with contrasting characteristics. Their sorption properties were characterized by XRD and FTIRS analyses, as well as sorption curve evaluation. TEM-EDS analyses were used to characterize the soil mineral particle associations and their metal sorption capacities. Submicron sized smectite particles were found to be associated to tiny ferryhidrite and goethite patches in the acidic forest soil samples, whereas the alkaline meadow soils could be characterized by goethite and smectite particles attached to large carbonate grains. Point chemical analyses carried out on such associations showed that significant metal separation may occur at particle level within the mineral associations observed. This is primarily obvious for Cu and Pb, which are preferentially sorbed by iron oxides over clay mineral particles. This phenomenon is more pronounced in competitive situation. Highest affinity to clay minerals was found for Zn and it may be also characteristic for Cd in acid conditions. However, decrease in available sorption sites and increase in pH may result in enhanced precipitation for the studied metals. Our results suggest that estimation of the role of soil components in metals' sorption can not be adequate enough when the sorption properties of a set of bulk soils are studied exclusively. Direct observation of metals' partition at particle level may result in a deeper insight into soil-metal interaction. This study was financially supported by the Hungarian Scientific Research Fund (OTKA K105009).

  15. Lattice Expansion of LSCF-6428 Cathodes Measured by In-situ XRD during SOFC Operation

    SciTech Connect

    Hardy, John S.; Templeton, Jared W.; Edwards, Danny J.; Lu, Zigui; Stevenson, Jeffry W.

    2012-01-03

    A new capability has been developed for analyzing solid oxide fuel cells (SOFCs). This paper describes the initial results of in-situ x-ray diffraction (XRD) of the cathode on an operating anode-supported solid oxide fuel cell. It has been demonstrated that XRD measurements of the cathode can be performed simultaneously with electrochemical measurements of cell performance or electrochemical impedance spectroscopy (EIS). While improvements to the technique are still to be made, the XRD pattern of a lanthanum strontium cobalt ferrite (LSCF) cathode with the composition La0.6Sr0.4Co0.2Fe0.8O3-δ (LSCF-6428) was found to continually but gradually change over the course of more than 60 hours of operation in air under typical SOFC operating conditions. It was determined that the most significant change was a gradual increase in the cubic lattice parameters of the LSCF from 3.92502 Å (as determined from the integration of the first 20 hours of XRD patterns) to 3.92650 Å (from the integration of the last 20 hours). This analysis also revealed that there were several peaks from unidentified minor phases that increased in intensity over this timeframe. After a temporary loss of airflow early in the test, the cell generated between 225 and 250 mW/cm2 for the remainder of the test. A large low frequency arc in the impedance spectra suggests the cell performance was gas diffusion limited and that there is room for improvement in air delivery to the cell.

  16. Phase analysis of aluminium modified GeSbTe bulk prepared from XRD of samples

    NASA Astrophysics Data System (ADS)

    Sandhu, Sharanjit; Singh, D.; Kumar, S.; Thangaraj, R.

    2016-05-01

    Various compositions of Aluminium modified GST as Alx(Ge2Sb2Te5)1-x x= 0, 0.15, 0.20, 0.25, 0.30 are prepared to study as a phase change material. Bulk prepared is studied with XRD scans for various phases formed. Phases other than Ge2Sb2Te5 do come in but dominated one is Ge2Sb2Te5 hexagonal phase.

  17. Effect of detrital muscovite on illite crystallinity measurement by x-ray diffraction (XRD)

    SciTech Connect

    Gundy, L.

    1987-08-01

    Illite crystallinity measurement by XRD can determine shale geothermometry and be used to map anchimetamorphic or diagenetic zones. A problem occurs in accuracy of XRD peak measurement because detrital muscovite from higher temperature source rocks constitutes a small percentage in many shales. The (001) XRD peaks coincide for diagenetic illite and detrital muscovite. The muscovite peak is very sharp, whereas the illite peak becomes sharper with increasing diagenetic grade. Thermal history, detrital muscovite, and sample preparation techniques will affect illite crystallinity measurements. Natural and artificially mixed samples can be used to show this effect quantitatively. Pegmatitic muscovite ground to clay size simulates this detrital component. When mixed with clay fractions from illitic shales, the induced error becomes insignificant for shales with a high-temperature history. Small detrital muscovite fractions adversely affect determination of lower diagenetic grades. Separation techniques that presume the coarser detrital fraction can be removed are not effective for siliceous shales, which must be ground. Calcareous and organic-rich shales may require disaggregation by chemical treatment, which may alter illite peak sharpness. Shales with 1 to 7% detrital muscovite showed higher illite crystallinity on x-ray diffractograms if the coarser fraction was not removed. At trace amounts of muscovite, the difference was negligible . By accurately estimating detrital percentages, a decision may be made to abandon tedious separation procedures. A correction factor may also be applied to crystallinity measurements to allow for the amount of detrital muscovite.

  18. XRD investigation of the strain/stress state of ion-irradiated crystals

    NASA Astrophysics Data System (ADS)

    Debelle, Aurélien; Declémy, Alain

    2010-05-01

    In this work, it is demonstrated that XRD is a powerful technique for the study of ion-irradiated materials. For this purpose, XRD experiments have been performed under different configurations on a <1 0 0>-oriented yttria-stabilized zirconia single crystal implanted with 300 keV caesium-ions at 3 × 10 14 cm -2. Initially, it is demonstrated that the depth strain profile can be determined from the refinement of a symmetric θ-2 θ scan. Moreover, in order to explore the whole XRD data, a model that describes the strain/stress state of the damaged layer is proposed. This model takes into account the elastic response of the bulk material (substrate) underneath the irradiated layer. The measured elastic strain is then the sum of a free strain due to the formation of radiation-induced defects and of an additional strain arising from the substrate elastic reaction. Application of this model allowed the calculation of the different strain contributions and the stress experienced by the irradiated layer. It is shown that these parameters may reach large values (respectively 0.7% and -1.9 GPa) despite the low radiation damage level.

  19. Validation of enhanced stabilization of municipal solid waste under controlled leachate recirculation using FTIR and XRD.

    PubMed

    Sethi, Sapna; Kothiyal, N C; Nema, Arvind K

    2012-07-01

    Leachate recirculation at neutral PH accompanied with buffer/nutrients addition has been used successfully in earlier stabilization of municipal solid waste in bioreactor landfills. In the present study, efforts were made to enhance the stabilization rate of municipal solid waste (MSW) and organic solid waste (OSW) in simulated landfill bioreactors by controlling the pH of recirculated leachate towards slightly alkaline side in absence of additional buffer and nutrients addition. Enhanced stabilization in waste samples was monitored with the help of analytical tools like Fourier Transform Infrared Spectroscopy (FTIR) and X-Ray Diffraction (XRD). Predominance of bands assigned to inorganic compounds and comparatively lower intensities of bands for organic compounds in the FTIR spectra of waste samples degraded with leachate recirculation under controlled pH confirmed higher rate of biodegradation and mineralization of waste than the samples degraded without controlled leachate recirculation. XRD spectra also confirmed to a greater extent of mineralization in the waste samples degraded under leachate recirculation with controlled pH. Comparison of XRD spectra of two types of wastes pointed out higher degree of mineralization in organic solid waste as compared to municipal solid waste. PMID:24749191

  20. Synchronizing flash-melting in a diamond cell with synchrotron X ray diffraction (XRD)

    NASA Astrophysics Data System (ADS)

    Karandikar, Amol; Boehler, Reinhard; Meng, Yue; Rod, Eric; Shen, Guoyin

    2013-06-01

    The major challenges in measuring melting temperatures in laser heated diamond cells are sample instability, thermal runaway and chemical reactions. To circumvent these problems, we developed a ``flash heating'' method using a modulated CW fiber laser and fast X ray detection capability at APS (Pilatus 1M detector). As an example, Pt spheres of 5 micron diameter were loaded in a single crystal sapphire encapsulation in the diamond cell at 65 GPa and heated in a single flash heating event for 20 ms to reach a desired temperature. A CCD spectrometer and the Pilatus were synchronized to measure the temperature and the XRD signal, respectively, when the sample reached the thermal steady state. Each successive flash heating was done at a higher temperature. The integrated XRD pattern, collected during and after (300 K) each heating, showed no chemical reaction up to 3639 K, the highest temperature reached in the experiment. Pt111 and 200 peak intensity variation showed gradual recrystalization and complete diminishing at about 3600 K, indicating melting. Thus, synchronized flash heating with novel sample encapsulation circumvents previous notorious problems and enables accurate melting temperature measurement in the diamond cell using synchrotron XRD probe. Affiliation 2: Geowissenschaeften, Goethe-Universitaet, Altenhoeferallee 1, D-60438 Frankfurt a.M., Germany.

  1. Effects and efficiency of consolidation treatments on Palaeolithic reindeer antler. Multi-analytical study by means of XRD, FT-IR microspectroscopy, SEM, TEM and μ-PIXE/PIGE analyses

    NASA Astrophysics Data System (ADS)

    Chadefaux, C.; Vignaud, C.; Menu, M.; Reiche, I.

    2008-07-01

    Bone materials record information on palaeodiets and palaeoenvironment, contained in their chemical and isotopic composition. Therefore, it is very important, while preserving these objects, to keep an open access to this information. In the present paper, we characterise the effects of consolidation treatments on the structure and chemical composition of archaeological reindeer antler at different hierarchical scales. X-ray diffraction, infra-red spectroscopy and microscopy, scanning and transmission electron microscopy coupled with an X-ray analysing system and proton-induced X-ray and γ-ray emission were used to reveal the state of preservation of reindeer antler and to evaluate the effectiveness of their consolidation treatments. These treatments are shown not to affect the chemical composition, but the crystallinity of the solid phase, as far as Palaeolithic material is concerned. In terms of penetration, the most efficient treatment, among those tested, seems to be the Rhodopas 15% single-bath treatment.

  2. TEM characterization of microstructure and chemistry in magnesium diboride superconductor

    NASA Astrophysics Data System (ADS)

    Zhu, Ye

    MgB2 is a superconductor with promising properties, but to meet application requirements, the properties of MgB2 have to be improved through microstructure modifications: chemical doping, introduction of precipitates, and atomic-scale control of defects. The small length scale of these modifications means that structure and chemistry characterization using the transmission electron microscope (TEM) are required to better understand the correlation between MgB2's superconducting properties and its microstructure. We have used TEM-based techniques to characterize microstructures of pure MgB2 bulks, SiC-doped MgB2 tapes, pure and C-doped MgB2 thin films prepared by hybrid physical-chemical vapor deposition (HPCVD) method with different carbon precursors, degraded pure HPCVD thin films, and O-doped MgB2 thin films prepared by molecular beam epitaxy. Characterization results and effects of microstructure on superconducting properties are discussed for each material. We have found that in pure MgB2 the main contaminating current-blocking phases are MgO grains and amorphous MgO + boron + BxO y phases. Both second phase nano-segregations and grain boundaries are effective pinning defects in MgB2, which can enhance Jc(H) at high fields. However, second phases also act as current-blocking phases that reduce the measured Jc, which suggests that MgB2 samples with small grain size and without any boundary second phases are desirable to achieve higher Jc. Extensive studies have been made to understand the Hc 2 enhancement mechanisms in MgB2. Both carbon dopant and grain boundaries in MgB2 can cause more electron scattering that increases Hc2. Degradation in MgB 2 leads to the formation of the amorphous boundary phase which also enhances Hc2 by introducing electron scattering. The over 60 T Hc2 ||ab obtained in C-doped HPCVD MgB 2 films is caused by the two-band nature and strong pi-band scattering of MgB2. We believe that the strain fields generated from c-axis tilt boundaries

  3. Aquifer characterisation in East Timor, with ground TEM

    NASA Astrophysics Data System (ADS)

    Ley-Cooper, A.

    2011-12-01

    An assessment of Climate Change Impacts on Groundwater Resources in East Timor led by Geosciences Australia is aimed at assisting East Timor's government to better understand and manage their groundwater resources. Form the current known information most aquifers in Timor-Leste are recharged by rainfall during the wet season. There is a concern that without a regular recharge, the stored groundwater capacity will decrease. Timor's population increase has caused a higher demand for groundwater which is currently been met by regulated pumping bores which are taped into deep aquifers, plus the sprouting of unregulated spear point bores in the shallow aquifers . Both groundwater recharge and the aquifers morphology need to be better understood in order to ensure supply and so groundwater can be managed for the future. Current weather patterns are expected to change and this could cause longer periods of drought or more intense rainfall, which in turn, would affect the availability and quality of groundwater. Salt water intrusions pose a threat on the low-lying aquifers as sea level rises. Australia's CSIRO has undertaken a series hydrogeophysical investigations employing ground TEM to assist in the characterisation of three aquifers near Dili, Timor Leste's capital. Interpreting ground water chemistry and dating; jointly with EM data has enhanced the understanding of the aquifers architecture, groundwater quality and helped identify potential risks of seawater intrusions.

  4. TEM in situ lithiation of tin nanoneedles for battery applications

    DOE PAGESBeta

    Janish, Matthew T.; Mackay, David T.; Liu, Yang; Jungjohann, Katherine L.; Carter, C. Barry; Norton, M. Grant

    2015-08-12

    Materials such as tin (Sn) and silicon that alloy with lithium (Li) have attracted renewed interest as anode materials in Li-ion batteries. Although their superior capacity to graphite and other intercalation materials has been known for decades, their mechanical instability due to extreme volume changes during cycling has traditionally limited their commercial viability. This limitation is changing as processes emerge that produce nanostructured electrodes. The nanostructures can accommodate the repeated expansion and contraction as Li is inserted and removed without failing mechanically. Recently, one such nano-manufacturing process, which is capable of depositing coatings of Sn “nanoneedles” at low temperature withmore » no template and at industrial scales, has been described. The present work is concerned with observations of the lithiation and delithiation behavior of these Sn nanoneedles during in situ experiments in the transmission electron microscope, along with a brief review of how in situ TEM experiments have been used to study the lithiation of Li-alloying materials. Individual needles are successfully lithiated and delithiated in solid-state half-cells against a Li-metal counter-electrode. Furthermore the microstructural evolution of the needles is discussed, including the transformation of one needle from single-crystal Sn to polycrystalline Sn–Li and back to single-crystal Sn.« less

  5. Transmission electron microscopy (TEM) study of minerals in coal

    SciTech Connect

    Hsieh, Kuang-Chien

    1982-01-01

    Minerals in eight coals from different mines were characterized in the micron-size range by using analytical transmission electron microscopy. Specimens were thinned by ion-milling wafers cut from these coals; a cold stage cooled by liquid nitrogen was used to reduce thermal degradation of the minerals by the ion-beam. Different mineral compounds were observed in different coals. The major minerals are clays, sulfides, oxides, carbonates and some minor-element-bearing phosphates. Clays (kaolinite, illite and others) have been most commonly found as either flat sheets or round globules. Iron sulfide was mostly found in the No. 5 and No. 6 coals from Illinois, distributed as massive polycrystals, as clusters of single crystals (framboids) or as isolated single crystals with size range down to some 0.25 microns. Other sulfides and some oxides were found in other coals with particle size as small as some 200 angstroms. Quartz, titanium oxides and many other carbonates and phosphate compounds were also characterized. Brief TEM work in the organic mass of coal was also introduced to study the nature of the coal macerals.

  6. TEM in situ lithiation of tin nanoneedles for battery applications

    SciTech Connect

    Janish, Matthew T.; Mackay, David T.; Liu, Yang; Jungjohann, Katherine L.; Carter, C. Barry; Norton, M. Grant

    2015-08-12

    Materials such as tin (Sn) and silicon that alloy with lithium (Li) have attracted renewed interest as anode materials in Li-ion batteries. Although their superior capacity to graphite and other intercalation materials has been known for decades, their mechanical instability due to extreme volume changes during cycling has traditionally limited their commercial viability. This limitation is changing as processes emerge that produce nanostructured electrodes. The nanostructures can accommodate the repeated expansion and contraction as Li is inserted and removed without failing mechanically. Recently, one such nano-manufacturing process, which is capable of depositing coatings of Sn “nanoneedles” at low temperature with no template and at industrial scales, has been described. The present work is concerned with observations of the lithiation and delithiation behavior of these Sn nanoneedles during in situ experiments in the transmission electron microscope, along with a brief review of how in situ TEM experiments have been used to study the lithiation of Li-alloying materials. Individual needles are successfully lithiated and delithiated in solid-state half-cells against a Li-metal counter-electrode. Furthermore the microstructural evolution of the needles is discussed, including the transformation of one needle from single-crystal Sn to polycrystalline Sn–Li and back to single-crystal Sn.

  7. TEM study of impurity segregations in beryllium pebbles

    NASA Astrophysics Data System (ADS)

    Klimenkov, M.; Chakin, V.; Moeslang, A.; Rolli, R.

    2014-12-01

    Beryllium is planned to be used as a neutron multiplier in the Helium-cooled Pebble Bed European concept of a breeding blanket of demonstration power reactor DEMO. In order to evaluate the irradiation performance, individual pebbles and constrained pebble beds were neutron-irradiated at temperatures typical of fusion blankets. Beryllium pebbles 1 mm in diameter produced by the rotating electrode method were subjected to a TEM study before and after irradiation at High Flux Reactor, Petten, Netherlands at 861 K. The grain size varied in a wide range from sub-micron size up to several tens of micrometers, which indicated formation bimodal grain size distribution. Based on the application of combined electron energy loss spectroscopy and energy dispersive X-ray spectroscopy methods, we suggest that impurity precipitates play an important role in controlling the mechanical properties of beryllium. The impurity elements were present in beryllium at a sub-percent concentration form beryllide particles of a complex (Fe/Al/Mn/Cr)B composition. These particles are often ordered along dislocations lines, forming several micron-long chains. It can be suggested that fracture surfaces often extended along these chains in irradiated material.

  8. Determination of phosphorus speciation in dairy manure using XRD and XANES spectroscopy.

    PubMed

    Güngör, Kerem; Jürgensen, Astrid; Karthikeyan, K G

    2007-01-01

    Intensive manure application is an important source of diffuse phosphorus (P) pollution. Phosphorus availability from animal manure is influenced by its chemical speciation. The major objective of this study was to investigate the P speciation in raw and anaerobically digested dairy manure with an emphasis on the calcium (Ca) and magnesium (Mg) phosphate phases. Influent and effluent from an on-farm digester in Wisconsin were sampled and sieved, and the 25 to 53 microm size fraction was dried for X-ray powder diffraction (XRD) and P K-edge X-ray absorption near edge structure (XANES) analyses. Struvite (MgNH4PO4.6H2O) was identified in both the raw (influent) and anaerobically digested (effluent) manure using XRD. Qualitative analysis of P K-edge XANES spectra indicated that the Ca orthophosphate phases, except dicalcium phosphate anhydrous (DCPA) or monetite (CaHPO4), were not abundant in dairy manure. Linear combination fitting (LCF) of the P standard compounds showed that 57.0 and 43.0% of P was associated with DCPA and struvite, respectively, in the raw manure. In the anaerobically digested sample, 78.2% of P was present as struvite and 21.8% of P was associated with hydroxylapatite (HAp). The P speciation shifted toward Mg orthophosphates and least soluble Ca orthophosphates following anaerobic digestion. Similarity between the aqueous orthophosphate (aq-PO4), newberyite (MgHPO4.3H2O), and struvite spectra can cause inaccurate P speciation determination when dairy manure is analyzed solely using P K-edge XANES spectroscopy; however, XANES can be used in conjunction with XRD to quantify the distribution of inorganic P species in animal manure. PMID:17965388

  9. [Analysis of XRD spectral characteristics of soil clay mineral in two typical cultivated soils].

    PubMed

    Zhang, Zhi-Dan; Luo, Xiang-Li; Jiang, Hai-Chao; Li, Qiao; Shen, Cong-Ying; Liu, Hang; Zhou, Ya-Juan; Zhao, Lan-Po; Wang, Ji-Hong

    2014-07-01

    The present paper took black soil and chernozem, the typical cultivated soil in major grain producing area of Northeast, as the study object, and determinated the soil particle composition characteristics of two cultivated soils under the same climate and location. Then XRD was used to study the composition and difference of clay mineral in two kinds of soil and the evolutionary mechanism was explored. The results showed that the two kinds of soil particles were composed mainly of the sand, followed by clay and silt. When the particle accumulation rate reached 50%, the central particle size was in the 15-130 microm interval. Except for black soil profile of Shengli Xiang, the content of clay showed converse sequence to the central particle in two soils. Clay accumulated under upper layer (18.82%) in black soil profile while under caliche layer (17.41%) in chernozem profile. Clay content was the least in parent material horizon except in black profile of Quanyanling. Analysis of clay XRD atlas showed that the difference lied in not only the strength of diffraction peak, but also in the mineral composition. The main contents of black soil and chernozem were both 2 : 1 clay, the composition of black soil was smectite/illite mixed layer-illite-vermiculite and that of chernozem was S/I mixture-illite-montmorillonite, and both of them contained little kaolinite, chlorite, quartz and other primary mineral. This paper used XRD to determine the characteristics of clay minerals comprehensively, and analyzed two kinds of typical cultivated soil comparatively, and it was a new perspective of soil minerals study. PMID:25269317

  10. XRD, lead equivalent and UV-VIS properties study of Ce and Pr lead silicate glasses

    SciTech Connect

    Alias, Nor Hayati Abdullah, Wan Shafie Wan Isa, Norriza Mohd Isa, Muhammad Jamal Md Zali, Nurazila Mat; Abdullah, Nuhaslinda Ee; Muhammad, Azali

    2014-02-12

    In this work, Cerium (Ce) and Praseodymium (Pr) containing lead silicate glasses were produced with 2 different molar ratios low (0.2 wt%) and high (0.4wt%). These types of glasses can satisfy the characteristics required for radiation shielding glasses and minimize the lead composition in glass. The radiation shielding properties of the synthesized glasses is explained in the form of lead equivalent study. The XRD diffraction and UV-VIS analysis were performed to observe the structural changes of the synthesis glasses at 1.5 Gy gamma radiation exposures.

  11. Characterization of Mo/C catalysts by XRD, XPS, and TOF-SIMS

    SciTech Connect

    Rondon, S.; Wilkinson, W.R.; Proctor, A.; Houalla, M.; Hercules, D.M.

    1995-11-09

    The objective of this work is to undertake a detailed study of the Mo/C system. This will include (a) study of the adsorption of Mo oxyanions from aqueous solutions of ammonium heptamolybdate onto activated carbon and (b) characterization of a series of Mo/C catalysts obtained by the equilibrium absorption method, using X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and time-of-flight secondary ion mass spectroscopy. The structural information thus obtained will be used to evaluate the Mo speciation proposed earlier. 35 refs., 6 figs., 2 tabs.

  12. The XRD Amorphous Component in John Klein Drill Fines at Yellowknife Bay, Gale Crater, Mars

    NASA Technical Reports Server (NTRS)

    Morris, Richard V.; Ming,, Douglas W.; Blake, David; Vaniman, David; Bish, David L; Chipera, Steve; Downs, Robert; Morrison, Shaunna; Gellert, Ralf; Campbell, Iain; Treiman, Alan H.; Achilles, Cherie; Bristow, Thomas; Crisp, Joy A.; McAdam, Amy; Archer, Paul Douglas; Sutter, Brad; Rampe, Elizabeth B.

    2013-01-01

    Drill fines of mudstone (targets John Klein and Cumberland) from the Sheepbed unit at Yel-lowknife Bay were analyzed by MSL payload elements including the Chemistry and Mineralogy (CheMin), APXS (Alpha Particle X-Ray Spectrometer), and Sample Analysis at Mars (SAM) instruments. CheMin XRD results show a variety of crystalline phases including feldspar, pyroxene, olivine, oxides, oxyhydroxides, sulfates, sulfides, a tri-octahedral smectite, and XRD amorphous material. The drill fines are distinctly different from corresponding analyses of the global soil (target Rocknest) in that the mudstone samples contained detectable phyllosilicate. Here we focus on John Klein and combine CheMin and APXS data to calculate the chemical composition and concentration of the amorphous component. The chemical composition of the amorphous plus smectite component for John Klein was calculated by subtracting the abundance-weighted chemical composition of the individual XRD crystalline components from the bulk composition of John Kline as measured by APXS. The chemical composition of individual crystalline components was determined either by stoichiometry (e.g., hematite and magnetite) or from their unit cell parameters (e.g., feldspar, olivine, and pyroxene). The chemical composition of the amorphous + smectite component (approx 71 wt.% of bulk sample) and bulk chemical composition are similar. In order to calculate the chemical composition of the amorphous component, a chemical composition for the tri-octahedral smectite must be assumed. We selected two tri-octahedral smectites with very different MgO/(FeO + Fe2O3) ratios (34 and 1.3 for SapCa1 and Griffithite, respectively). Relative to bulk sample, the concentration of amorphous and smectite components are 40 and 29 wt.% for SapCa1 and 33 and 36 wt.% for Griffithite. The amount of smectite was calculated by requiring the MgO concentration to be approx 0 wt.% in the amorphous component. Griffithite is the preferred smectite because

  13. IN-SITU XRD OF OPERATING LSFC CATHODES: DEVELOPMENT OF A NEW ANALYTICAL CAPABILITY

    SciTech Connect

    Hardy, John S.; Templeton, Jared W.; Stevenson, Jeffry W.

    2012-11-19

    A solid oxide fuel cell (SOFC) research capability has been developed that facilitates measuring the electrochemical performance of an operating SOFC while simultaneously performing x-ray diffraction on its cathode. The evolution of this research tool’s development is discussed together with a description of the instrumentation used for in-situ x-ray diffraction (XRD) measurements of operating SOFC cathodes. The challenges that were overcome in the process of developing this capability, which included seals and cathode current collectors, are described together with the solutions that are presently being applied to mitigate them.

  14. A mathematical method for XRD pattern interpretation in clay containing nano composites

    NASA Astrophysics Data System (ADS)

    Khederlou, Kh.; Bagheri, R.; Shojaei, A.

    2014-11-01

    X-ray diffraction and rheological measurements were used to characterize nanoparticle dispersion in LDPE/LLDPE/nanoclay hybrid nanocomposites. XRD patterns were interpreted with a novel distribution formula and rheological measurements were used to confirm the results. Results of these two methods indicated that increasing clay in all the prepared nanocomposites exhibited a significant improvement in filler-matrix interaction because of increasing the probability of polymer diffusion but further exfoliation need more compatibilizing situations. It seems that this mathematical method could be used for predicting the overall change in clay gallery d-spacing and the extent of intercalation-exfoliation of nanoclay in these systems.

  15. The XRD Amorphous Component in John Klein Drill Fines at Yellowknife Bay, Gale Crater, Mars

    NASA Astrophysics Data System (ADS)

    Morris, R. V.; Ming, D. W.; Blake, D.; Vaniman, D.; Bish, D. L.; Chipera, S.; Downs, R.; Morrison, S.; Gellert, R.; Campbell, I.; Treiman, A. H.; Achilles, C.; Bristow, T.; Crisp, J. A.; McAdam, A.; Archer, P. D.; Sutter, B.; Rampe, E. B.; Team, M.

    2013-12-01

    Drill fines of mudstone (targets John Klein and Cumberland) from the Sheepbed unit at Yel-lowknife Bay were analyzed by MSL payload elements including the Chemistry and Mineralogy (CheMin), APXS (Alpha Particle X-Ray Spectrometer), and Sample Analysis at Mars (SAM) instruments. CheMin XRD results show a variety of crystalline phases including feldspar, pyrox-ene, olivine, oxides, oxyhydroxides, sulfates, sulfides, a tri-octahedral smectite, and XRD amorphous material. The drill fines are distinctly different from corresponding analyses of the global soil (target Rocknest) in that the mudstone samples contained detectable phyllosilicate. Here we focus on John Klein and combine CheMin and APXS data to calculate the chemical composition and concentration of the amorphous component. The chemical composition of the amorphous plus smectite component for John Klein was cal-culated by subtracting the abundance-weighted chemical composition of the individual XRD crystalline components from the bulk composition of John Kline as measured by APXS. The chemical composition of individual crystalline components was determined either by stoichiome-try (e.g., hematite and magnetite) or from their unit cell parameters (e.g., feldspar, olivine, and pyroxene). The chemical composition of the amorphous + smectite component (~71 wt.% of bulk sample) and bulk chemical compositon are similar. In order to calculate the chemical composition of the amorphous component, a chemical composition for the tri-octahedral smectite must be assumed. We selected two tri-octahedral smectites with very different MgO/(FeO + Fe2O3) ratios (34 and 1.3 for SapCa1 and Griffithite, respectively). Relative to bulk sample, the concentration of amorphous and smectite components are 40 and 29 wt.% for SapCa1 and 33 and 36 wt.% for Griffithite. The amount of smectite was calculated by requiring the MgO concentration to be~0 wt.% in the amporphous component. Griffithite is the preferred smectite because the position

  16. Analytical electron microscopy of Mg-SiO smokes - A comparison with infrared and XRD studies

    NASA Technical Reports Server (NTRS)

    Rietmeijer, F. J. M.; Nuth, J. A.; Mackinnon, I. D. R.

    1986-01-01

    Analytical electron microscopy conducted for Mg-SiO smokes (experimentally obtained from samples previously characterized by IR spectroscopy) indicates that the microcrystallinity content of unannealed smokes increases with increased annealing for up to 30 hr. The growth of forsterite microcrystallites in the initially nonstoichiometric smokes may give rise to the contemporaneous growth of the SiO polymorph tridymite and MgO; after 4 hr of annealing, these react to form enstatite. It is suggested that XRD analysis and IR spectroscopy should be conducted in conjunction with detailed analytical electron microscopy for the detection of emerging crystallinity in vapor-phase condensates.

  17. Study of dislocations in copper by weak beam, stereo, and in situ straining TEM

    SciTech Connect

    McCabe, R. J.; Misra, A.; Mitchell, T. E.

    2002-01-01

    Conventional transmission electron microscopy (TEM) has been an invaluable tool for verifjhg and developing dislocation theories since the first direct observations of dislocations were made using a TEM in the 1950s. Several useful techniques and technological advancements have been made since, helping fbrther the advancement of dislocation knowledge. The present paper concerns two studies of dislocations in copper made by coupling several of these techniques, specifically weak beam, in situ straining, and stereo TEM. Stereo-TEM coupled with in situ straining TEM was used for tracking 3D dislocation motion and interactions in low dislocation density copper foils. A mechanism by which dislocations in a pileup bypass a dislocation node is observed and discussed. Weak beam TEM is used in conjunction with stereo-TEM to analyze the dislocation content of a dense dislocation wall (DDW).

  18. Three Dimensional TEM Forward Modeling Using FDTD Accelerated by GPU

    NASA Astrophysics Data System (ADS)

    Li, Z.; Huang, Q.

    2015-12-01

    Three dimensional inversion of transient electromagnetic (TEM) data is still challenging. The inversion speed mostly depends on the forward modeling. Finite-difference time-domain (FDTD) method is one of the popular forward modeling scheme. In an explicit type, which is based on the Du Fort-Frankel scheme, the time step is under the constraint of quasi-static approximation. Often an upward-continuation boundary condition (UCBC) is applied on the earth-air surface to avoid time stepping in the model air. However, UCBC is not suitable for models with topography and has a low parallel efficiency. Modeling without UCBC may cause a much smaller time step because of the resistive attribute of the air and the quasi-static constraint, which may also low the efficiency greatly. Our recent research shows that the time step in the model air is not needed to be constrained by the quasi-static approximation, which can let the time step without UCBC much closer to that with UCBC. The parallel performance of FDTD is then largely released. On a computer with a 4-core CPU, this newly developed method is obviously faster than the method using UCBC. Besides, without UCBC, this method can be easily accelerated by Graphics Processing Unit (GPU). On a computer with a CPU of 4790k@4.4GHz and a GPU of GTX 970, the speed accelerated by CUDA is almost 10 times of that using CPU only. For a model with a grid size of 140×140×130, if the conductivity of the model earth is 0.02S/m, and the minimal space interval is 15m, it takes only 80 seconds to evolve the field from excitation to 0.032s.

  19. In-situ TEM characterization of Copper Growth

    NASA Astrophysics Data System (ADS)

    Shelberg, Daniel T.

    In-situ liquid experiments in the transmission electron microscope (TEM) allow dynamic phenomena to be imaged at the nanoscale. This opens the opportunity to view electrochemical depositions at the nano scale in real time. However, there are a number of issues regarding in situ imaging that prevent a straightforward approach. This thesis addresses two issues regarding in-situ experiments; the fabrication of electron transparent windows and the nucleation of a metal from an electrolyte as a result of beam damage. Silicon chips that were 2.6mm x 2.6mm with 50mum x 50mum windows consisting of 50nm S3N 4 were fabricated with the goal of minimizing fabrication complexity at a cost significantly below commercial prices. These silicon nitride windows were used to sandwich a small volume of CuSO4 solution and observe copper nucleation as a result of the radiolysis damage of water due to the electron beam. Scanning transmission electron microscopy (STEM) was used to image growth, and reducing species are shown to diffuse on the order of hundreds of nanometers in solution. Copper nanoparticle growth was compared to Oswald ripening, and diffusion limited growth was observed at high electron dose rates. The diffusion limited growth was suppressed and led to a slower growth rate, with a calculated diffusion coefficient for Cu 2+ of 2 x 10--10 m2/s. Low electron dose rates corresponding to low magnifications in STEM yielded kinetic limited or mixed growth and yielded faceted nanoparticles. Atomic resolution was achieved in copper film deposited at low magnifications, and lattice fringes corresponding to the copper <111> were observed.

  20. Trace elemental analysis of Indian natural moonstone gems by PIXE and XRD techniques.

    PubMed

    Venkateswara Rao, R; Venkateswarulu, P; Kasipathi, C; Sivajyothi, S

    2013-12-01

    A selected number of Indian Eastern Ghats natural moonstone gems were studied with a powerful nuclear analytical and non-destructive Proton Induced X-ray Emission (PIXE) technique. Thirteen elements, including V, Co, Ni, Zn, Ga, Ba and Pb, were identified in these moonstones and may be useful in interpreting the various geochemical conditions and the probable cause of their inceptions in the moonstone gemstone matrix. Furthermore, preliminary XRD studies of different moonstone patterns were performed. The PIXE technique is a powerful method for quickly determining the elemental concentration of a substance. A 3MeV proton beam was employed to excite the samples. The chemical constituents of moonstones from parts of the Eastern Ghats geological formations of Andhra Pradesh, India were determined, and gemological studies were performed on those gems. The crystal structure and the lattice parameters of the moonstones were estimated using X-Ray Diffraction studies, trace and minor elements were determined using the PIXE technique, and major compositional elements were confirmed by XRD. In the present work, the usefulness and versatility of the PIXE technique for research in geo-scientific methodology is established. PMID:24055999

  1. The use of micro-XRD for the study of glaze color decorations

    NASA Astrophysics Data System (ADS)

    Pradell, T.; Molina, G.; Molera, J.; Pla, J.; Labrador, A.

    2013-04-01

    The compounds responsible for the colors and decorations in glass and glazed ceramics include: coloring agents (transition-metal ions), pigments (micro- and nanoprecipitates of compounds that either do not dissolve or recrystallize in the glassy matrix) and opacifiers (microcrystalline compounds with high light scattering capability). Their composition, structure and range of stability are highly dependent not only on the composition but also on the procedures followed to obtain them. Chemical composition of the colorants and crystallites may be obtained by means of SEM-EDX and WDX. Synchrotron radiation micro-X-ray diffraction (SR-micro-XRD) has a small beam size adequate (10 to 50 microns footprint size) to obtain the structural information of crystalline compounds and high brilliance, optimal for determining the crystallites even when present in low amounts. In addition, in glass decorations the crystallites often appear forming thin layers (from 10 to 100 micrometers thick) and they show a depth-dependent composition and crystal structure. Their nature and distribution across the glass/glaze decorations gives direct information on the technology of production and stability and may be related to the color and appearance. A selection of glass and glaze coloring agents and decorations are studied by means of SR-micro-XRD and SEM-EDX including: manganese brown, antimony yellow, red copper lusters and cobalt blue. The selection includes Medieval (Islamic, and Hispano Moresque) and Renaissance tin-glazed ceramics from the 10th to the 17th century AD.

  2. XRD characterisation of composite Ni-based coatings prepared by electrodeposition

    NASA Astrophysics Data System (ADS)

    Tarkowski, L.; Indyka, P.; Bełtowska-Lehman, E.

    2012-08-01

    The present work is aimed at XRD investigation of structural parameters that influence the functional properties of Ni-W/Al2O3 electrodeposit coatings. The relationship between electrodeposition parameters and structural properties of the coatings deposited on steel substrates has been determined. XRD investigations were performed on a Bruker D8 Discover diffractometer equipped with a position-sensitive linear detector. The modified sin2ψ X-ray diffraction method was used to determine the macroscopic residual stresses of deposits. The crystallite size and lattice strain of the coatings were evaluated by analysis of X-ray diffraction patterns (Rietveld analysis). The crystallographic texture was analysed using the orientation distribution function (ODF) calculated from the incomplete pole figures. It was shown that the structural properties of the deposits were strongly correlated with chemical composition. X-ray diffraction patterns of all Ni-W coatings exhibit mainly the fcc phase structure of the Ni-W solid solution with a lattice parameter intermediate between those of Ni and W, which rises when the tungsten content increases. At the same time the crystallite dimension (the size of the coherent domains) was gradually reduced. It was found that Ni-W coatings containing about 40 wt.% W revealed the tensile residual stresses (2300-1200 MPa), depending on deposition conditions.

  3. XRD and AFM characterization of epitaxial Nb films before and after hydrogen exposure

    NASA Astrophysics Data System (ADS)

    Allain, Monica; Heuser, Brent; Durfee, Curtis

    2001-03-01

    Epitaxial Nb films have been characterized with x-ray diffraction (XRD) and atomic force microscopy (AFM) before and after hydrogenation at 100 C and 760 Torr. Two 1000 Angstrom epitaxial Nb films were grown on a-plane sapphire with two different miscut angles, 0.08 and 1.4 degrees. Both Nb films were capped with a 100 Angstrom thick Pd layer to facilitate molecular hydrogen dissociation. While the as-grow film mosaic did not depend on miscut angle, the surface morphology was significantly different. In particular, the high miscut film exhibited a fingered topography that was absent in the low miscut film. Hydrogen absorption under the conditions stated above induce a complete conversion of Nb to the alpha prime hydride phase. The Nb hydride phase transformation process is known to create dislocations as incoherent phase boundaries pass through the lattice. The surface morphology and lattice mosaic from post-hydrogen AFM and XRD measurements, respectively, show the extreme effect of the phase transformation process. Discussion will focus on the lattice mosaic broadening, residual strain, and surface features after hydrogen exposure.

  4. Structural investigations in helium implanted cubic zirconia using grazing incidence XRD and EXAFS spectroscopy

    NASA Astrophysics Data System (ADS)

    Kuri, G.; Degueldre, C.; Bertsch, J.; Döbeli, M.

    2010-06-01

    The crystal structure and local atom arrangements surrounding Zr atoms were determined for a helium implanted cubic stabilized zirconia (CSZ) using X-ray diffraction (XRD) and extended X-ray absorption fine structure (EXAFS) spectroscopy, respectively, measured at glancing angles. The implanted specimen was prepared at a helium fluence of 2 × 10 16 cm -2 using He + beams at two energies (2.54 and 2.74 MeV) passing through a 8.0 μm Al absorber foil. XRD results identified the formation of a new rhombohedral phase in the helium embedded layer, attributed to internal stress as a result of expansion of the CSZ-lattice. Zr K-edge EXAFS data suggested loss of crystallinity in the implanted lattice and disorder of the Zr atoms environment. EXAFS Fourier transforms analysis showed that the average first-shell radius of the Zr sbnd O pair in the implanted sample was slightly larger than that of the CSZ standard. Common general disorder features were explained by rhombohedral type short-range ordered clusters. The average structural parameters estimated from the EXAFS data of unimplanted and implanted CSZ are compared and discussed. Potential of EXAFS as a local probe of atomic-scale structural modifications induced by helium implantation in CSZ is demonstrated.

  5. XRD studies of beta-chitin from squid pen with calcium solvent.

    PubMed

    Nagahama, H; Higuchi, T; Jayakumar, R; Furuike, T; Tamura, H

    2008-05-01

    The crystalline structure of beta-chitin from squid pen was investigated by X-ray diffraction (XRD). The purified beta-chitin was prepared from bigfin reefsquid pen. beta-Chitin was treated with saturated calcium chloride dihydrate/alchohol (CaCl(2).2H(2)O/MeOH) solvent system at different conditions for XRD studies. The change of crystallinity of beta-chitin from squid pen was studied by using the fiber photographs on imaging plates. The results showed that the diffraction peak (010) was shifted. It means that the lattice plane (010) interplanarilly spreaded to 3.4A, when the squid pen was washed with water after treatment of Ca solvent. Furthermore, when the squid pen was dried after treatment of Ca solvent and washing with water, interplanar spacing of (010) inversely shrank to 1.1A. These results suggested that Ca solvent especially influences the plane (010) of beta-chitin structure. PMID:18036656

  6. XRD and FTIR structural investigation of gadolinium-zinc-borate glass ceramics

    SciTech Connect

    Borodi, G.; Pascuta, P.; Dan, V.; Pop, V.; Stefan, R.; Radulescu, D.

    2013-11-13

    X-ray diffraction (XRD) and Fourier transform infrared (FTIR) spectroscopy measurements have been employed to investigate the (Gd{sub 2}O{sub 3}){sub x}⋅(B{sub 2}O{sub 3}){sub (60−x)}⋅(ZnO){sub 40} glass ceramics system, with 0 ≤ x ≤ 15 mol%. After heat treatment applied at 860 °C for 2 h, some structural changes were observed and new crystalline phases appeared in the structure of the samples. In these glass ceramics four crystalline phases were identified using powder diffraction files (PDF 2), namely ZnB{sub 4}O{sub 7}, Zn{sub 4}O(B{sub 6}O{sub 12}), Zn{sub 3}(BO{sub 3}){sub 2} and GdBO{sub 3}. From the XRD data, the average unit-cell parameter and the quantitative ratio of the crystallographic phases in the studied samples were evaluated. FTIR data revealed that the BO{sub 3}, BO{sub 4} and ZnO{sub 4} are the main structural units of these glass ceramics network. The compositional dependence of the different structural units which appear in the studied samples was followed.

  7. An Integrated XRF/XRD Instrument for Mars Exobiology and Geology Experiments

    NASA Technical Reports Server (NTRS)

    Koppel, L. N.; Franco, E. D.; Kerner, J. A.; Fonda, M. L.; Schwartz, D. E.; Marshall, J. R.

    1993-01-01

    By employing an integrated x-ray instrument on a future Mars mission, data obtained will greatly augment those returned by Viking; details characterizing the past and present environment on Mars and those relevant to the possibility of the origin and evolution of life will be acquired. A combined x-ray fluorescence/x-ray diffraction (XRF/XRD) instrument was breadboarded and demonstrated to accommodate important exobiology and geology experiment objectives outlined for MESUR and future Mars missions. Among others, primary objectives for the exploration of Mars include the intense study of local areas on Mars to establish the chemical, mineralogical, and petrological character of different components of the surface material; to determine the distribution, abundance, and sources and sinks of volatile materials, including an assessment of the biologic potential, now and during past epoches; and to establish the global chemical and physical characteristics of the Martian surface. The XRF/XRD breadboard instrument identifies and quantifies soil surface elemental, mineralogical, and petrological characteristics and acquires data necessary to address questions on volatile abundance and distribution. Additionally, the breadboard is able to characterize the biogenic element constituents of soil samples providing information on the biologic potential of the Mars environment. Preliminary breadboard experiments confirmed the fundamental instrument design approach and measurement performance.

  8. XRD and FTIR structural investigation of gadolinium-zinc-borate glass ceramics

    NASA Astrophysics Data System (ADS)

    Borodi, G.; Pascuta, P.; Stefan, R.; Dan, V.; Pop, V.; Radulescu, D.

    2013-11-01

    X-ray diffraction (XRD) and Fourier transform infrared (FTIR) spectroscopy measurements have been employed to investigate the (Gd2O3)xṡ(B2O3)(60-x)ṡ(ZnO)40 glass ceramics system, with 0 ≤ x ≤ 15 mol%. After heat treatment applied at 860 °C for 2 h, some structural changes were observed and new crystalline phases appeared in the structure of the samples. In these glass ceramics four crystalline phases were identified using powder diffraction files (PDF 2), namely ZnB4O7, Zn4O(B6O12), Zn3(BO3)2 and GdBO3. From the XRD data, the average unit-cell parameter and the quantitative ratio of the crystallographic phases in the studied samples were evaluated. FTIR data revealed that the BO3, BO4 and ZnO4 are the main structural units of these glass ceramics network. The compositional dependence of the different structural units which appear in the studied samples was followed.

  9. Microstructure analysis of melt-spun Al{sub 3}Ti intermetallics by XRD and EXAFS

    SciTech Connect

    Chen, J.; Barrera, E.V.; Frazier, W.E.

    1997-12-31

    In an effort to expand the composition range over which Al{sub 3}Ti is stable, various amounts of niobium were substituted for titanium and processed by melt-spinning. Several samples were annealed both at 600 C and 1,000 C for 24 hours. The effects of processing parameters such as wheel speed, the amount of niobium, and annealing temperatures on the structure were investigated by XRD and EXAFS. XRD showed that for all the samples the only structure present was DO{sub 22}. The DO{sub 22} structure was stable even after the high temperature heat treatments. By means of EXAFS, niobium atoms were observed to occupy titanium sites in the DO{sub 22} structure. Furthermore, in the unannealed samples, increasing wheel speed of the melt spinning process or the niobium concentration tended to distort the crystal structure. It was observed that Ti EXAFS had different results from the Nb EXAFS beyond their occupying similar sites, which suggested there may exist some composition zones, i.e., rich Nb zone or rich Ti zones, although the structures present were still DO{sub 22}. The samples were found to experience different distortions as a function of annealing temperatures.

  10. [FTIR and XRD analysis of hydroxyapatite from fossil human and animal teeth in Jinsha Relict, Chengdu].

    PubMed

    Huang, Cheng-min; Zhang, Qing; Bai, Song; Wang, Cheng-shan

    2007-12-01

    Diagenetic effect during burial on the hydroxyapatite in enamel and dentin from fossil human and animal teeth was examined, using X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR). For the enamel and dentin of all fossil teeth, XRD patterns exhibit bulge line and overlap between major reflections of hydroxyapatite, and the crystallinity of hydroxyapatite is low. For each infrared spectrum, H2O and OH(-) have distinct peaks of absorbance, and PO4(3-) and CO3(2-) ions have intensive infrared vibration modes at the fundamental wave numbers. The component of hydroxyapatite of all fossil teeth is similar to the modern biological hydroxyapatite. Furthermore, the index (PCI) which reflects the hydroxyapatite crystallinity of each sample ranges from 2.4 to 4.0 while the index (BPI) reflecting the amount of type B carbonate to phosphate indicates that the values of CO3(2-) content in hydroxyapatite are rather high, accordingly the crystallinity of all fossil hydroxyapatites are poor. It could be concluded that little alteration of hydroxyapatites from fossil human and animal teeth occurred in the process of diagenesis in Jinsha Relict, Chengdu, China. PMID:18330282

  11. Development of 89Zr-Ontuxizumab for in vivo TEM-1/endosialin PET applications

    PubMed Central

    Lange, Sara E.S.; Zheleznyak, Alex; Studer, Matthew; O'Shannessy, Daniel J.; Lapi, Suzanne E.; Van Tine, Brian A.

    2016-01-01

    Purpose The complexity of sarcoma has led to the need for patient selection via in vivo biomarkers. Tumor endothelial marker-1 (TEM-1) is a cell surface marker expressed by the tumor microenvironment. Currently MORAb-004 (Ontuxizumab), an anti-TEM-1 humanized monoclonal antibody, is in sarcoma clinical trials. Development of positron emission tomography (PET) for in vivo TEM-1 expression may allow for stratification of patients, potentially enhancing clinical outcomes seen with Ontuxizumab. Results Characterization of cell lines revealed clear differences in TEM-1 expression. One high expressing (RD-ES) and one low expressing (LUPI) cell line were xenografted, and mice were injected with 89Zr-Ontuxizumab. PET imaging post-injection revealed that TEM-1 was highly expressed and readily detectable in vivo only in RD-ES. In vivo biodistribution studies confirmed high radiopharmaceutical uptake in tumor relative to normal organs. Experimental Design Sarcoma cell lines were characterized for TEM-1 expression. Ontuxizumab was labeled with 89Zr and evaluated for immunoreactivity preservation. 89Zr-Ontuxizumab was injected into mice with high or null expressing TEM-1 xenografts. In vivo PET imaging experiments were performed. Conclusion 89Zr-Ontuxizumab can be used in vivo to determine high versus low TEM-1 expression. Reliable PET imaging of TEM-1 in sarcoma patients may allow for identification of patients that will attain the greatest benefit from anti-TEM-1 therapy. PMID:26909615

  12. Seismicity triggered by the olivine-spinel transition: new insights from combined XRD and acoustic emission monitoring during deformation experiments in Mg2GeO4

    NASA Astrophysics Data System (ADS)

    Schubnel, A.; Hilairet, N.; Brunet, F.; Gasc, J.; Cordier, P.; Wang, Y.; Green, H. W.

    2012-04-01

    Polycrystalline Mg2GeO4-olivine has been deformed (strain rates from 2.10-4/s to 10-5/s) in the deformation-DIA in 13-BM-D at GSECARS (Advanced Photon Source) at ca. 2 GPa confining pressure for temperatures between 973 and 1573 K (i.e., in the Mg2GeO4-ringwoodite field). Stress, advancement of transformation, and strain were measured in-situ using X-ray diffraction (XRD) and imaging, and acoustic emissions (AE) were recorded simultaneously. When differential stress is applied (ca. 1- to 2 GPa) and temperature is increased, the very beginning of the transformation to the ringwoodite structure (as evidenced by in situ XRD) is accompanied by AE bursts which locate within the sample. At high strain rates (>10-4/s) and low temperatures (800-900 degrees C), the number of AEs is comparable, if not larger, to that observed during the cold compression of quartz grains. The largest events always occur at a temperature slightly below that of appearance of the ringwoodite-structure phase on the XRD images patterns. This suggests that AEs are generated while the transition is still nucleation controlled (pseudo-martensitic stage). During stress-relaxation periods, the rate of AE triggering decreases, but does not completely vanish. Importantly, we still observed very large AEs at strain rates as low as approx. 10-5/ s, while at these early stages of the transformation, the samples did not show any macroscopic rheological weakening. Focal mechanism analysis of the largest AEs showed that they are all of shear type, some being even pure double couple. They radiate about the same amount of energy as typically recorded during fast crack propagation in amorphous glass material. Microstructural analysis (SEM, EBSD and TEM) highlights the presence of thin transformation bands, with plausible evidence of shear (grain distortion and grain size reduction). These bands are made of incoherent spinel and olivine nano-grains which run across germanium-olivine grain boundaries. These bands

  13. Seismicity triggered by the olivine-spinel transition: new insights from combined XRD and acoustic emission monitoring during deformation experiments in Mg2GeO4

    NASA Astrophysics Data System (ADS)

    Schubnel, A. J.; Hilairet, N.; Brunet, F.; Héripré, E.; Cordier, P.; Wang, Y.

    2011-12-01

    Polycrystalline Mg2GeO4-olivine has been deformed (strain rates from 2.10-4/s to 10-5/s) in the deformation-DIA in 13-BM-D at GSECARS (Advanced Photon Source) at ca. 2 GPa confining pressure for temperatures between 973 and 1573 K (i.e., in the Mg2GeO4-ringwoodite field). Stress, advancement of transformation, and strain were measured in-situ using X-ray diffraction (XRD) and imaging, and acoustic emissions (AE) were recorded simultaneously. When differential stress is applied (ca. 1- to 2 GPa) and temperature is increased, the very beginning of the transformation to the ringwoodite structure (as evidenced by in situ XRD) is accompanied by AE bursts which locate within the sample. At high strain rates (>10-4/s) and low temperatures (800-900 degrees C), the number of AEs is comparable, if not larger, to that observed during the cold compression of quartz grains. The largest events always occur at a temperature slightly below that of appearance of the ringwoodite-structure phase on the XRD images patterns. This suggests that AEs are generated while the transition is still nucleation controlled (pseudo-martensitic stage). During stress-relaxation periods, the rate of AE triggering decreases, but does not completely vanish. Importantly, we still observed very large AEs at strain rates as low as approx. 10-5/ s, while at these early stages of the transformation, the samples did not show any macroscopic rheological weakening. Focal mechanism analysis of the largest AEs showed that they are all of shear type, some being even pure double couple. They radiate about the same amount of energy as typically recorded during fast crack propagation in amorphous glass material. Microstructural analysis (SEM, EBSD and TEM) highlights the presence of thin transformation bands, with plausible evidence of shear (grain distortion and grain size reduction). These bands are made of incoherent spinel and olivine nano-grains which run across germanium-olivine grain boundaries. These bands

  14. Carbonate Mineral Assemblages as Inclusions in Yakutian Diamonds: TEM Verifications

    NASA Astrophysics Data System (ADS)

    Logvinova, A. M.; Wirth, R.; Sobolev, N. V.; Taylor, L. A.

    2014-12-01

    Carbonate mineral inclusions are quite rare in diamonds from the upper mantle, but are evidence for a carbonate abundance in the mantle. It is believed that such carbonatitic inclusions originated from high-density fluids (HDFs) that were enclosed in diamond during its growth. Using TEM and EPMA, several kinds of carbonate inclusions have been identified in Yakutian diamonds : aragonite, dolomite, magnesite, Ba-, Sr-, and Fe-rich carbonates. Most of them are represented by multi-phase inclusions of various chemically distinct carbonates, rich in Ca, Mg, and K and associated with minor amounts of silicate, oxide, saline, and volatile phases. Volatiles, leaving some porosity, played a significant role in the diamond growth. A single crystal of aragonite (60μm) is herein reported for the first time. This inclusion is located in the center of a diamond from the Komsomolskaya pipe. Careful CL imaging reveals the total absence of cracks around the aragonite inclusion - i.e., closed system. This inclusion has been identified by X-ray diffraction and microprobe analysis. At temperatures above 1000 0C, aragonite is only stable at high pressures of 5-6 GPa. Inside this aragonite, we observed nanocrystalline inclusions of titanite, Ni-rich sulfide, magnetite, water-bearing Mg-silicate, and fluid bubbles. Dolomite is common in carbonate multi-phase inclusions in diamonds from the Internatsionalnaya, Yubileinaya, and Udachnaya kimberlite pipes. Alluvial diamonds of the northeastern Siberian Platform are divided into two groups based on the composition of HDFs: 1) Mg-rich multi-phase inclusions (60% magnesite + dolomite + Fe-spinel + Ti-silicate + fluid bubbles); and 2) Ca-rich multi-phase inclusions (Ca,Ba-, Ca,Sr-, Ca,Fe-carbonates + Ti-silicate + Ba-apatite + fluid bubbles). High-density fluids also contain K. Volatiles in the fluid bubbles are represented by water, Cl, F, S, CO2, CH4, and heavy hydrocarbons. Origin of the second group of HDFs may be related to the non

  15. Evolution of the Mobile Information SysTem (MIST)

    NASA Technical Reports Server (NTRS)

    Litaker, Harry L., Jr.; Thompson, Shelby; Archer, Ronald D.

    2008-01-01

    The Mobile Information SysTem (MIST) had its origins in the need to determine whether commercial off the shelf (COTS) technologies could improve intervehicular activities (IVA) on International Space Station (ISS) crew maintenance productivity. It began with an exploration of head mounted displays (HMDs), but quickly evolved to include voice recognition, mobile personal computing, and data collection. The unique characteristic of the MIST lies within its mobility, in which a vest is worn that contains a mini-computer and supporting equipment, and a headband with attachments for a HMD, lipstick camera, and microphone. Data is then captured directly by the computer running Morae(TM) or similar software for analysis. To date, the MIST system has been tested in numerous environments such as two parabolic flights on NASA's C-9 microgravity aircraft and several mockup facilities ranging from ISS to the Altair Lunar Sortie Lander. Functional capabilities have included its lightweight and compact design, commonality across systems and environments, and usefulness in remote collaboration. Human Factors evaluations of the system have proven the MIST's ability to be worn for long durations of time (approximately four continuous hours) with no adverse physical deficits, moderate operator compensation, and low workload being reported as measured by Corlett Bishop Discomfort Scale, Cooper-Harper Ratings, and the NASA Total Workload Index (TLX), respectively. Additionally, through development of the system, it has spawned several new applications useful in research. For example, by only employing the lipstick camera, microphone, and a compact digital video recorder (DVR), we created a portable, lightweight data collection device. Video is recorded from the participants point of view (POV) through the use of the camera mounted on the side of the head. Both the video and audio is recorded directly into the DVR located on a belt around the waist. This data is then transferred to

  16. Evaluation of rock powdering methods to obtain fine-grained samples for CHEMIN, a combined XRD/XRF instrument

    SciTech Connect

    Chipera, S. J.; Vaniman, D. T.; Bish, D. L.; Sarrazin, P.; Feldman, S.; Blake, D.; Bearman, G. H.; Bar-Cohen, Yoseph

    2004-01-01

    A miniature XRD/XRD (X-ray diffraction/X-ray fluorescence) instrument, CHEMIN, is currently being developed for definite mineralogic analysis of soils and rocks on Mars. One of the technical issues that must be addressed to enable remote XRD analysis is how best to obtain a representative sample powder for analysis. For powder XRD analyses, it is beneficial to have a fine-grained sample to reduce preferred orientation effects and to provide a statistically significant number of crystallites to the X-ray beam. Although a two-dimensional detector as used in the CHEMIN instrument produces good results even with poorly prepared powder, the quality of the data improves and the time required for data collection is reduced if the sample is fine-grained and randomly oriented. A variety of methods have been proposed for XRD sample preparation. Chipera et al. presented grain size distributions and XRD reuslts from powders generated with an Ultrasonic/Sonic Driller/Corer (USDC) currently being developed at JPL. The USDC was shown to be an effective instrument for sampling rock to produce powder suitable for XRD. In this paper, they compare powder prepared using the USDC with powder obtained with a miniaturized rock crusher developed at JPL and with powder obtained with a rotary tungsten carbide bit to powders obtained from a laboratory bench-scale Retsch mill (provides benchmark mineralogical data). These comparisons will allow assessment of the suitability of these methods for analysis by an XRD/XRD instrument such as CHEMIN.

  17. SHI Induced Modifications in CdS/CuInSe{sub 2} Thin Film: XRD Analysis

    SciTech Connect

    Joshi, Rajesh A.; Taur, Vidya S.; Sharma, Ramphal; Ghule, Anil V.

    2011-07-15

    CuInSe{sub 2}(CIS nanostructured) thin films were prepared by ion exchange method at room temperature on ITO coated glass substrates in an alkaline medium. The as prepared thin films were irradiated by 120 MeV Au{sup 9+} swift heavy ion (SHI) at 5x10{sup 11} and 5x10{sup 12} ions/cm{sup 2} fluence respectively. To study the effect of irradiation, the pristine and irradiated nanostructured thin films were characterized by X ray Diffraction (XRD) and analyzed the improvement in crystalline quality and crystallite size. The observed structural modifications discussed considering the high electronic energy deposition by 120 MeV gold heavy (Au{sup 9+}) ions in CuInSe{sub 2} thin films.

  18. Laboratory Detection and Analysis of Organic Compounds in Rocks Using HPLC and XRD Methods

    NASA Technical Reports Server (NTRS)

    Dragoi, D.; Kanik, I.; Bar-Cohen, Y.; Sherrit, S.; Tsapin, A.; Kulleck, J.

    2004-01-01

    In this work we describe an analytical method for determining the presence of organic compounds in rocks, limestone, and other composite materials. Our preliminary laboratory experiments on different rocks/limestone show that the organic component in mineralogical matrices is a minor phase on order of hundreds of ppm and can be better detected using high precision liquid chromatography (HPLC). The matrix, which is the major phase, plays an important role in embedding and protecting the organic molecules from the harsh Martian environment. Some rocks bear significant amounts of amino acids therefore, it is possible to identify these phases using powder x-ray diffraction (XRD) by crystallizing the organic. The method of detection/analysis of organics, in particular amino acids, that have been associated with life will be shown in the next section.

  19. High temperature XRD of Cu{sub 2}GeSe{sub 3}

    SciTech Connect

    Premkumar, D. S.; Malar, P.; Chetty, Raju; Mallik, Ramesh Chandra

    2015-06-24

    The Cu{sub 2}GeSe{sub 3} is prepared by solid state synthesis method. The high temperature XRD has been done at different temperature from 30 °C to 450 °C. The reitveld refinement confirms Cu{sub 2}GeSe{sub 3} phase and orthorhombic crystal structure. The lattice constants are increasing with increase in the temperature and their rate of increase with respect to temperature are used for finding the thermal expansion coefficient. The calculation of the linear and volume coefficient of thermal expansion is done from 30 °C to 400 °C. Decrease in the values of linear expansion coefficients with temperature are observed along a and c axis. Since thermal expansion coefficient is the consequence of the distortion of atoms in the lattice; this can be further used to find the minimum lattice thermal conductivity at given temperature.

  20. Powder XRD and dielectric studies of gel grown calcium pyrophosphate crystals

    NASA Astrophysics Data System (ADS)

    Parekh, Bharat; Parikh, Ketan; Joshi, Mihir

    2013-06-01

    Formation of calcium pyrophosphate dihydrate (CPPD) crystals in soft tissues such as cartilage, meniscus and synovial tissue leads to CPPD deposition diseases. The appearance of these crystals in the synovial fluid can give rise to an acute arthritic attack with pain and inflammation of the joints, a condition called pseudo-gout. The growth of CPP crystals has been carried out, in the present study, using the single diffusion gel growth technique, which can broadly mimic in vitro the condition in soft tissues. The crystals were characterized by different techniques. The FTIR study revealed the presence of various functional groups. Powder XRD study was also carried out to verify the crystal structure. The dielectric study was carried out at room temperature by applying field of different frequency from 500 Hz to 1 MHz. The dielectric constant, dielectric loss and a.c. resistivity decreased as frequency increased, whereas the a.c. conductivity increased as frequency increased.

  1. Studying Cellulose Fiber Structure by SEM, XRD, NMR and Acid Hydrolysis

    SciTech Connect

    Zhao, Haibo; Kwak, Ja Hun; Zhang, Z. Conrad; Brown, Heather M.; Arey, Bruce W.; Holladay, John E.

    2007-03-21

    Cotton linters were partially hydrolyzed in dilute acid and the morphology of remaining macrofibrils studied with Scanning Electron Microscopy (SEM) under various magnifications. The crystal region (microfibril bundles) in the macrofibrils was not altered by hydrolysis, and only amorphous cellulose was hydrolyzed and leached out from the macrofibrils. The diameter of microfibril bundles was 20-30 nm after the amorphous cellulose was removed by hydrolysis. XRD experiments confirm the unaltered diameter of the microfibrils after hydrolysis. The strong stability of these microfibril bundles in hydrolysis limits both the total sugar monomer yield and the size of nano particles or rods produced in hydrolysis. The large surface potential on the remaining microfibril bundles drives the agglomeration of macrofibrils.

  2. A high-pressure study of PbCO3 by XRD and Raman spectroscopy

    NASA Astrophysics Data System (ADS)

    Zhang, Yu-Feng; Liu, Jing; Qin, Zhen-Xing; Lin, Chuan-Long; Xiong, Lun; Li, Rui; Bai, Li-Gang

    2013-03-01

    The pressure-induced phase transitions of PbCO3 are studied using synchrotron radiation in a diamond anvil cell at room temperature. The XRD measurement indicates that PbCO3 with an initial phase of aragonite-type structure undergoes two phase transitions at ~7.8 GPa and ~15.7 GPa, respectively. The higher-pressure phase appearing at ~15.7 GPa is stable up to 51.8 GPa. The two phase transitions are further confirmed by Raman scattering up to 23.3 GPa. During the decompression process, the high-pressure phases of PbCO3 are gradually recovered to the starting aragonite-type structure, but exhibit some hysteresis. The bulk modulus B0 of the aragonite-type structure is obtained to be 63±(3) GPa by fitting the volume-pressure data to the Birch—Murnaghan equation of states with B'0 fixed to 4.

  3. Thermal decomposition of dolomite under CO2: insights from TGA and in situ XRD analysis.

    PubMed

    Valverde, Jose Manuel; Perejon, Antonio; Medina, Santiago; Perez-Maqueda, Luis A

    2015-11-28

    Thermal decomposition of dolomite in the presence of CO2 in a calcination environment is investigated by means of in situ X-ray diffraction (XRD) and thermogravimetric analysis (TGA). The in situ XRD results suggest that dolomite decomposes directly at a temperature around 700 °C into MgO and CaO. Immediate carbonation of nascent CaO crystals leads to the formation of calcite as an intermediate product of decomposition. Subsequently, decarbonation of this poorly crystalline calcite occurs when the reaction is thermodynamically favorable and sufficiently fast at a temperature depending on the CO2 partial pressure in the calcination atmosphere. Decarbonation of this dolomitic calcite occurs at a lower temperature than limestone decarbonation due to the relatively low crystallinity of the former. Full decomposition of dolomite leads also to a relatively low crystalline CaO, which exhibits a high reactivity as compared to limestone derived CaO. Under CO2 capture conditions in the Calcium-Looping (CaL) process, MgO grains remain inert yet favor the carbonation reactivity of dolomitic CaO especially in the solid-state diffusion controlled phase. The fundamental mechanism that drives the crystallographic transformation of dolomite in the presence of CO2 is thus responsible for its fast calcination kinetics and the high carbonation reactivity of dolomitic CaO, which makes natural dolomite a potentially advantageous alternative to limestone for CO2 capture in the CaL technology as well as SO2in situ removal in oxy-combustion fluidized bed reactors. PMID:26506285

  4. XRD and EPR structural investigation of some zinc borate glasses doped with iron ions

    NASA Astrophysics Data System (ADS)

    Stefan, Razvan; Pascuta, Petru; Popa, Adriana; Raita, Oana; Indrea, Emil; Culea, Eugen

    2012-02-01

    Glasses in the system xFe2O3·(100-x) [45ZnO·55B2O3] (0≤x≤10 mol%) have been prepared by melting at 1200 °C and rapidly cooling at room temperature. The obtained samples were submitted to an additional thermal treatment at 570 °C for 12 h in order to relax the glass structure as well as to improve the local order. The as cast and heat treated samples were investigated using X-ray diffraction (XRD) and electron paramagnetic resonance (EPR) measurements. The XRD patterns of all the studied samples show their vitreous nature. Structural modifications occurring in the heat treated samples compared to the untreated ones have been pointed out. EPR spectra of untreated and heat treated samples revealed resonance absorptions centered at g≈2.0, g≈4.3 and g≈6.4. The compositional variation of the line intensity and linewidth of the absorptions from g≈4.3 and g≈2.0 have been interpreted in terms of the variation in the concentration of the Fe3+ ions and the interaction between the iron ions. The EPR spectra of the untreated samples containing 5 mol% Fe2O3 have been studied at different temperatures (110-290 K). The line intensity of the resonance signals decreases with increase in temperature whereas the linewidth is found to be independent of temperature. It was also found that the temperature variation of reciprocal line intensity obeys the Boltzmann law.

  5. Exploring the potential reservoirs of non specific TEM beta lactamase (blaTEM) gene in the Indo-Gangetic region: A risk assessment approach to predict health hazards.

    PubMed

    Singh, Gulshan; Vajpayee, Poornima; Rani, Neetika; Amoah, Isaac Dennis; Stenström, Thor Axel; Shanker, Rishi

    2016-08-15

    The emergence of antimicrobial resistant bacteria is an important public health and environmental contamination issue. Antimicrobials of β-lactam group accounts for approximately two thirds, by weight, of all antimicrobials administered to humans due to high clinical efficacy and low toxicity. This study explores β-lactam resistance determinant gene (blaTEM) as emerging contaminant in Indo-Gangetic region using qPCR in molecular beacon format. Quantitative Microbial Risk Assessment (QMRA) approach was adopted to predict risk to human health associated with consumption/exposure of surface water, potable water and street foods contaminated with bacteria having blaTEM gene. It was observed that surface water and sediments of the river Ganga and Gomti showed high numbers of blaTEM gene copies and varied significantly (p<0.05) among the sampling locations. The potable water collected from drinking water facility and clinical settings exhibit significant number of blaTEM gene copies (13±0.44-10200±316 gene copies/100mL). It was observed that E.crassipes among aquatic flora encountered in both the rivers had high load of blaTEM gene copies. The information on prevalence of environmental reservoirs of blaTEM gene containing bacteria in Indo-Gangetic region and risk associated will be useful for formulating strategies to protect public from menace of clinical risks linked with antimicrobial resistant bacteria. PMID:27111425

  6. Final Report - SRNL Agreement #AC51296V SEM, FIB, TEM Studies of CZT Samples

    SciTech Connect

    Bradley, J; Dai, Z R; Graham, G A; Teslich, N E

    2007-08-28

    The aims of this study are: (1) to characterize the surfaces of samples 3-7-8-3 and 4-1-3 using SEM, FIB and TEM techniques; (2) identify raised surface features; (3) prepare FIB-TEM lift-out sections from identified raised surfaces; and (4) perform detailed TEM characterization of FIB Sections. Focusing on the composition and crystallinity of the phases within the sections, including impurities.

  7. Retrofit implementation of Zernike phase plate imaging for cryo-TEM

    PubMed Central

    Marko, Michael; Leith, ArDean; Hsieh, Chyongere; Danev, Radostin

    2011-01-01

    In-focus phase-plate imaging is particularly beneficial for cryo-TEM because it offers a substantial overall increase in image contrast, without an electron dose penalty, and it simplifies image interpretation. We show how phase-plate cryo-TEM can be implemented with an appropriate existing TEM, and provide a basic practical introduction to use of thin-film (carbon) phase plates. We point out potential pitfalls of phase-plate operation, and discuss solutions. We provide information on evaluating a particular TEM for its suitability. PMID:21272647

  8. Modal Mineralogy of CV3 Chondrites by PSD-XRD: Mineralogic Insights into a Complex Evolutionary History

    NASA Astrophysics Data System (ADS)

    Howard, K. T.; Benedix, G. K.; Bland, P. A.; Cressey, G.

    2009-03-01

    CV3 chondrites Vigarano, Efremovka, Allende, Mokoia, Grosnaja and Kaba are amongst the most studied rocks in existence. By XRD we define the first quantitative modal mineralogy of these samples and explore implications of our data to petrogenesis.

  9. Spectral studies on a series of metal ion complexes derived from pyrimidine nucleus, TEM, biological and γ-irradiation effect

    NASA Astrophysics Data System (ADS)

    Al-Ashqer, Sawsan; Abou-Melha, Khlood S.; Al-Hazmi, G. A. A.; Saad, Fawaz A.; El-Metwaly, Nashwa M.

    2014-11-01

    A series of thiouracil complexes was prepared, all the prepared compounds are investigated by all possible tools. The ligand coordinates towards two central atoms as a neutral hexadentate mode. The octahedral structure was proposed with Ni(II), Pt(IV) and UO2(II) complexes. Square-pyramidal and square planar with VO(II) and Pd(II) complexes, respectively. VO(II) complex was irradiated by using Gamma radiation to through a light on the probability of geometry changes with the effect of radiation. The parameters calculated from ESR spectra before and after γ-irradiation reflect the rigidity of the complex towards the effect. Such may discuss the unaffected biological behavior before and after irradiation. XRD patterns were carried out to emphasis on the nature of the particles and the purity of products. The ligand, Pt(IV) and Pd(II) are found in nanometer range. TEM is a sensitive tool used to justify on the microstructure and surface morphology. All the investigated compounds are in nanorange. TG curves reflect a lower thermal stability of all investigated complexes due to the presence of water of crystallization. Finally, a toxic effect was observed with all investigated complexes towards Gram positive bacterium as well as a resistant behavior was observed with Gram negative bacteria.

  10. Application of Mythen detector: In-situ XRD study on the thermal expansion behavior of metal indium

    NASA Astrophysics Data System (ADS)

    Du, Rong; Chen, ZhongJun; Cai, Quan; Fu, JianLong; Gong, Yu; Wu, ZhongHua

    2016-07-01

    A Mythen detector has been equipped at the beamline 4B9A of Beijing Synchrotron Radiation Facility (BSRF), which is expected to enable BSRF to perform time-resolved measurement of X-ray diffraction (XRD) full-profiles. In this paper, the thermal expansion behavior of metal indium has been studied by using the in-situ XRD technique with the Mythen detector. The indium was heated from 303 to 433 K with a heating rate of 2 K/min. The in-situ XRD full-profiles were collected with a rate of one profile per 10 seconds. Rietveld refinement was used to extract the structural parameters. The results demonstrate that these collected quasi-real-time XRD profiles can be well used for structural analysis. The metal indium was found to have a nonlinear thermal expansion behavior from room temperature to the melting point (429.65 K). The a-axis of the tetragonal unit cell expands with a biquadratic dependency on temperature, while the c-axis contracts with a cubic dependency on temperature. By the time-resolved XRD measurements, it was observed that the [200] preferred orientation can maintain to about 403.15 K. While (110) is the last and detectable crystal plane just before melting of the polycrystalline indium foil. This study is not only beneficial to the application of metal indium, but also exhibits the capacity of in-situ time-resolved XRD measurements at the X-ray diffraction station of BSRF.

  11. The proposed icy mineralogy package (XRD/XRF) for TandEM

    NASA Astrophysics Data System (ADS)

    Fortes, Andrew Dominic; Wood, Ian G.; Dobson, David P.; Fewster, Paul F.; Coustenis, Athena; Lebreton, Jean-Pierre

    Introduction: Understanding the geology of Titan's crust, and its interaction with the atmosphere, requires determination of the chemistry and mineralogy of surface materials which can only be achieved unambiguously using a combination of X-ray fluorescence spectroscopy (XRF) and X-ray diffraction (XRD). Here we describe an icy mineralogy package (IMP) consisting of a miniaturised XRD/XRF instrument designed primarily with Titan (and the TandEM ESA Cosmic Vision proposal [1]) in mind; however, the instrument is not predicated upon an a priori knowledge of surface mineralogy and consequently is applicable with little modification to any solar system body (rocky or icy). The proposed instrument is well suited to integration with other analytical tools, such as IR and UV Raman spectrometers. Instrument design: Two design concepts are currently under study, which differ in the complexity of the sample handling system, and the range of Bragg angles which may be observed. Both are focusing cameras, one (IMP senior) working in transmission, and the other (IMP junior) working in back-reflection. IMP jnr is intended for deployment on a static surface probe with no sample acquisition capability, collecting a single diffraction pattern through a window in the probe's underside. IMP snr is intended for deployment on a balloon with a sample collection arm able to deliver scoops of surface material to a rotating specimen stage. The latter may therefore be used to analyse many samples at geographically dispersed points. In each case we will use X-rays generated by high specific-activity radioisotope sources, 55 Fe and 241 Am. Our paper will present the results of the following activities: (a) compilation of a crystallographic database of materials expected on Titan's surface; (b) simulation of single-phase and polyphase diffraction data to illustrate the ease with which substances may be distinguished (even in complex mixtures); (c) blind tests of peak-matching software against

  12. XRD Analysis of Cement Paste Samples Exposed to the Simulated Environment of a Deep Repository - 12239

    SciTech Connect

    Ferreira, Eduardo G.A.; Marumo, Julio T.; Vicente, Roberto; Gobbo, Luciano

    2012-07-01

    Portland cement materials are widely used as engineered barriers in repositories for radioactive waste. The capacity of such barriers to avoid the disposed of radionuclides to entering the biosphere in the long-term depends on the service life of those materials. Thus, the performance assessment of structural materials under a series of environmental conditions prevailing at the environs of repositories is a matter of interest. The durability of cement paste foreseen as backfill in a deep borehole for disposal of disused sealed radioactive sources is investigated in the development of the repository concept. Results are intended to be part of the body of evidence in the safety case of the proposed disposal technology. This paper presents the results of X-Ray Diffraction (XRD) Analysis of cement paste exposed to varying temperatures and simulated groundwater after samples received the radiation dose that the cement paste will accumulate until complete decay of the radioactive sources. The XRD analysis of cement paste samples realized in this work allowed observing some differences in the results of cement paste specimens that were submitted to different treatments. The cluster analysis of results was able to group tested samples according to the applied treatments. Mineralogical differences, however, are tenuous and, apart from ettringite, are hardly observed. The absence of ettringite in all the seven specimens that were kept in dry storage at high temperature had hardly occurred by natural variations in the composition of hydrated cement paste because ettringite is observed in all tested except the seven specimens. Therefore this absence is certainly the result of the treatments and could be explained by the decomposition of ettringite. Although the temperature of decomposition is about 110-120 deg. C, it may be initially decomposed to meta-ettringite, an amorphous compound, above 50 deg. C in the absence of water. Influence of irradiation on the mineralogical

  13. Modal mineralogy of CV3 chondrites by X-ray diffraction (PSD-XRD)

    NASA Astrophysics Data System (ADS)

    Howard, K. T.; Benedix, G. K.; Bland, P. A.; Cressey, G.

    2010-09-01

    Using position sensitive detector X-ray diffraction (PSD-XRD) we determine a complete modal mineralogy for all phases present in abundances greater than 1 wt% in Vigarano, Efremovka, Mokoia, Grosnaja, Kaba and Allende. Reduced CV3 samples are comprised of (vol%): olivine (83-85%); enstatite (6.5-8.1%); anorthite (1.1-1.2%); magnetite (1.4-1.8%); sulphide (2.4-5.1%); Fe, Ni metal (2-2.2%). The oxidized samples are comprised of: olivine (76.3-83.9%); enstatite (4.8-7.8%); anorthite (1.1-1.7%); magnetite (0.3-6.1%); sulphide (2.9-8.1%); Fe, Ni metal (0.2-1.1%); Fe-oxide (0-2.7%) and phyllosilicate (1.9-4.2%). When our modal data is used to calculate a bulk chemistry that is compared to literature data a near 1:1 correlation is observed. PSD-XRD data indicates that olivine compositions may span almost the entire Fe-Mg solid solution series in all CV samples and that these contain a component (4-13%) of fine-grained olivine that is more Fe-rich (>Fa 60) than is typically reported. Modal mineralogy shows that there are mineralogic differences between CV3 samples classified as oxidized and reduced but that these sub-classes are most clearly distinguished by the relative abundance of metal and Ni content of sulphide, rather than abundance of magnetite. The most significant difference in modal mineralogy observed is the relative absence of phyllosilicate in reduced CV that essentially escaped aqueous alteration. Fayalite, ferrous olivine and magnetite are typically considered secondary alteration products. The abundances of these minerals overlap in oxidized and reduced samples and correlate positively supporting common conditions of formation in a relatively oxidizing environment. The abundances of fayalite, ferrous olivine and magnetite show no relationship to petrographic type and if these abundances were used as a proxy for alteration, Allende would be the least altered CV - contrary to all previous data. The implication is that thermal metamorphism on the parent body

  14. XRD monitoring of α self-irradiation in uranium-americium mixed oxides.

    PubMed

    Horlait, Denis; Lebreton, Florent; Roussel, Pascal; Delahaye, Thibaud

    2013-12-16

    The structural evolution under (241)Am self-irradiation of U(1-x)Am(x)O(2±δ) transmutation fuels (with x ≤ 0.5) was studied by X-ray diffraction (XRD). Samples first underwent a preliminary heat treatment performed under a reducing atmosphere (Ar/H2(4%)) aiming to recover the previously accumulated structural defects. Over all measurements (carried out over up to a full year and for integrated doses up to 1.5 × 10(18) α-decay events·g(-1)), only fluorite U(1-x)Am(x)O(2±δ) solid solutions were observed. Within a few days after the end of the heat treatment, each of the five studied samples was slowly oxidized as a consequence of their move to air atmosphere, which is evidenced by XRD by an initial sharp decrease of the unit cell parameter. For the compounds with x ≤ 0.15, this oxidation occurred without any phase transitions, but for U0.6Am0.4O(2±δ) and U0.5Am0.5O(2±δ), this process is accompanied by a transition from a first fluorite solid solution to a second oxidized one, as the latter is thermodynamically stable in ambient conditions. In the meantime and after the oxidation process, (241)Am α self-irradiation caused a structural swelling up to ∼0.8 vol %, independently of the sample composition. The kinetic constants of swelling were also determined by regression of experimental data and are, as expected, dependent on x and thus on the dose rate. The normalization of these kinetic constants by sample α-activity, however, leads to very close swelling rates among the samples. Finally, evolutions of microstrain and crystallite size were also monitored, but for the considered dose rates and cumulated doses, α self-irradiation was found, within the limits of the diffractometer used, to have almost no impact on these characteristics. Microstrain was found to be influenced instead by the americium content in the materials (i.e., by the impurities associated with americium starting material and the increase of cationic charge heterogeneity with

  15. Spectroscopic and XRD characterisation of zeolite catalysts active for the oxidative methylation of benzene with methane

    NASA Astrophysics Data System (ADS)

    Adebajo, Moses O.; Long, Mervyn A.; Frost, Ray L.

    2004-03-01

    The benzene methylation with methane over zeolite catalysts was previously shown in our laboratory to require the presence of oxygen. Thus, a two-step mechanism involving the intermediate formation of methanol by partial oxidation of methane followed by the methylation of benzene with methanol in the second step, was postulated. This paper now reports the results of the characterisation of the zeolite catalysts used for the oxidative benzene methylation reaction in order to provide some information about their composition, structure, properties and their behaviour before and after the reaction. The catalysts were characterised by X-ray diffraction (XRD), inductively coupled plasma atomic emission spectroscopy (ICP-AES), X-ray fluorescence (XRF), FT-IR and solid state NMR. XRD results indicate that the crystalline structures of all the ZSM-5 and H-beta catalysts remained unchanged after batch reaction of benzene with methane over the catalysts in agreement with the observation that the catalysts recovered from the reactor could be reused without loss of activity. Elemental analyses and FT-IR data show that as the level of metal ion exchange increases, the Brönsted acid concentration decreases but this metal ion exchange does not totally remove Brönsted acidity. FT-IR results further show that only a small amount of acid sites is actually necessary for a catalyst to be active since used catalysts containing highly reduced Brönsted acidity are found to be reusable without any loss of their activity. 29Si and 27Al magic angle spinning (MAS) NMR together with FT-IR spectra also show that all the active zeolites catalysts contain some extra-framework octahedral aluminium in addition to the normal tetrahedral framework aluminium. The presence of this extra-lattice aluminium does not, however, have any adverse effect on the crystallinity of the catalysts both before and after oxidative benzene methylation reaction. There appears also to be no significant dealumination

  16. Data from the Mars Science Laboratory CheMin XRD/XRF Instrument

    NASA Technical Reports Server (NTRS)

    Vaniman, David; Blake, David; Bristow, Tom; DesMarais, David; Achilles, Cherie; Anderson, Robert; Crips, Joy; Morookian, John Michael; Spanovich, Nicole; Vasavada, Ashwin; Yen, Albert; Bish, David; Chipera, Steve; Downs, Robert; Morrison, Shaunna; Farmer, Jack; Grotzinger, John; Stolper, Edward; Ming, Douglas; Morris, Richard; Rampe, Elizabeth; Treiman, Allan; Sarrazin, Philippe

    2013-01-01

    The CheMin instrument on the Mars Science Laboratory (MSL) rover Curiosity uses a Co tube source and a CCD detector to acquire mineralogy from diffracted primary X-rays and chemical information from fluoresced X-rays. CheMin has been operating at the MSL Gale Crater field site since August 5, 2012 and has provided the first X-ray diffraction (XRD) analyses in situ on a body beyond Earth. Data from the first sample collected, the Rocknest eolian soil, identify a basaltic mineral suite, predominantly plagioclase (approx.An50), forsteritic olivine (approx.Fo58), augite and pigeonite, consistent with expectation that detrital grains on Mars would reflect widespread basaltic sources. Minor phases (each <2 wt% of the crystalline component) include sanidine, magnetite, quartz, anhydrite, hematite and ilmenite. Significantly, about a third of the sample is amorphous or poorly ordered in XRD. This amorphous component is attested to by a broad rise in background centered at approx.27deg 2(theta) (Co K(alpha)) and may include volcanic glass, impact glass, and poorly crystalline phases including iron oxyhydroxides; a rise at lower 2(theta) may indicate allophane or hisingerite. Constraints from phase chemistry of the crystalline components, compared with a Rocknest bulk composition from the APXS instrument on Curiosity, indicate that in sum the amorphous or poorly crystalline components are relatively Si, Al, Mg-poor and enriched in Ti, Cr, Fe, K, P, S, and Cl. All of the identified crystalline phases are volatile-free; H2O, SO2 and CO2 volatile releases from a split of this sample analyzed by the SAM instrument on Curiosity are associated with the amorphous or poorly ordered materials. The Rocknest eolian soil may be a mixture of local detritus, mostly crystalline, with a regional or global set of dominantly amorphous or poorly ordered components. The Rocknest sample was targeted by MSL for "first time analysis" to demonstrate that a loose deposit could be scooped, sieved to

  17. Multielemental analyses of isomorphous Indian garnet gemstones by XRD and external pixe techniques.

    PubMed

    Venkateswarulu, P; Srinivasa Rao, K; Kasipathi, C; Ramakrishna, Y

    2012-12-01

    Garnet gemstones were collected from parts of Eastern Ghats geological formations of Andhra Pradesh, India and their gemological studies were carried out. Their study of chemistry is not possible as they represent mixtures of isomorphism nature, and none of the individual specimens indicate independent chemistry. Hence, non-destructive instrumental methodology of external PIXE technique was employed to understand their chemistry and identity. A 3 MeV proton beam was employed to excite the samples. In the present study geochemical characteristics of garnet gemstones were studied by proton induced X-ray emission. Almandine variety of garnet is found to be abundant in the present study by means of their chemical contents. The crystal structure and the lattice parameters were estimated using X-Ray Diffraction studies. The trace and minor elements are estimated using PIXE technique and major compositional elements are confirmed by XRD studies. The technique is found very useful in characterizing the garnet gemstones. The present work, thus establishes usefulness and versatility of the PIXE technique with external beam for research in Geo-scientific methodology. PMID:23041780

  18. A 4-(o-chlorophenyl)-2-aminothiazole: Microwave assisted synthesis, spectral, thermal, XRD and biological studies

    NASA Astrophysics Data System (ADS)

    Rajmane, S. V.; Ubale, V. P.; Lawand, A. S.; Nalawade, A. M.; Karale, N. N.; More, P. G.

    2013-11-01

    A 4-(o-chlorophenyl)-2-aminothiazole (CPAT) has been synthesized by reacting o-chloroacetophenone, iodine and thiourea under microwave irradiation as a green chemistry approach. The reactions proceed selectively and within a couple of minutes giving high yields of the products. The compound was characterized by elemental, spectral (UV-visible, IR, NMR and GC-MS), XRD and thermal analyses. The TG curve of the compound was analyzed to calculate various kinetic parameters (n, E, Z, ΔS and ΔG) by using Coats-Redfern (C.R.), MacCallum-Tanner (M.T.) and Horowitz-Metzger (H.M.) method. The compound was tested for the evaluation of antibacterial activity against B. subtilis and E. coli and antifungal activity against A. niger and C. albicans. The compound was evaluated for their in vitro nematicidal activity on plant parasitic nematode Meloidogyne javanica and molluscicidal activity on fresh water helminthiasis vector snail Lymnea auricularia. The compound is biologically active in very low concentration. X-ray diffraction study suggests a triclinic crystal system for the compound.

  19. XRD and XAS structural study of CuAlO2 under high pressure.

    PubMed

    Pellicer-Porres, J; Segura, A; Ferrer-Roca, Ch; Polian, A; Munsch, P; Kim, D

    2013-03-20

    We present the results of x-ray diffraction and x-ray absorption spectroscopy experiments in CuAlO(2) under high pressure. We discuss the polarization dependence of the x-ray absorption near-edge structure at the Cu K-edge. XRD under high pressure evidences anisotropic compression, the a-axis being more compressible than the c-axis. EXAFS yields the copper-oxygen bond length, from which the only internal parameter of the delafossite structure is deduced. The combination of anisotropic compression and the internal parameter decrease results in a regularization of the AlO(6) octahedra. The anisotropic compression is related to the chemical trends observed in the lattice parameters when Al is substituted by other trivalent cations. Both experiments evidence the existence of an irreversible phase transition that clearly manifests at 35 ± 2 GPa. The structure of the high-pressure polymorph could not be determined, but it implies a change of the Cu environment, which remains anisotropic. Precursor effects are observed from the lowest pressures, which are possibly related to crystal breaking at a submicroscopic scale with partial reorientation of the crystallites. PMID:23423689

  20. Modeling the PbI2 formation in perovskite solar cells using XRD/XPS patterns

    NASA Astrophysics Data System (ADS)

    Sohrabpoor, Hamed; Elyasi, Majid; Aldosari, Marouf; Gorji, Nima E.

    2016-09-01

    The impact of prolonged irradiation and air humidity on the stability of perovskite solar cells is modeled using X-ray diffraction and X-ray photoelectron spectroscopy patterns reported in the literature. Light or air-moisture causes the formation of a thin PbI2 or oxide defective layers (in nanoscale) at the interface of perovskite/hole-transport-layer or at the junction with metallic back contact. This thin layer blocks the carrier transport/passivation at the interfaces and cause degradation of device parameters. Variation in thickness of defective layers, changes the XRD and XPS peaks. This allows detection and estimation of the type, crystallinity and thickness of the defective layer. A simple model is developed here to extract the thickness of such thin defective layers formed in nanometer scale at the back region of several perovskite devices. Based on this information, corrected energy band diagram of every device before and after degradation/aging is drawn and discussed in order to obtain insight into the carrier transport and charge collection at the barrier region. In addition, graphene contacted perovskite devices are investigated showing that honey-comb network of graphene contact reduces the effect of aging leading to formation of a thinner defective layer at the perovskite surface compared to perovskite devices with conventional inorganic contacts i.e. Au, Al.

  1. Mechanical Properties of Polycrystalline Titanium Nitride Films Measured by XRD Tensile Testing

    NASA Astrophysics Data System (ADS)

    Namazu, Takahiro; Inoue, Shozo; Takemoto, Hideki; Koterazawa, Keiji

    This paper describes measurement of mechanical properties of micron-thin polycrystalline titanium nitride (TiN) films. We developed a novel tensile test technique that can directly measure lateral elastic strain of a microscale single/poly-crystalline specimen by means of X-ray diffraction (XRD), which enables evaluation of not only Young's modulus but also Poisson's ratio of TiN films. TiN films having thicknesses of 0.5 μm to 1.6 μm are deposited onto the top and bottom surfaces of a microscale single crystal silicon (Si) specimen. The deposition is carried out by r.f. reactive magnetron sputtering under Ar partial pressure ranging from 0.7 Pa to 1.0 Pa. Average values of Young's modulus and Poisson's ratio for the Si monolayer specimen are found to be 169 GPa and 0.35, respectively, which are in close agreement with analytical values. TiN films deposited under an Ar partial pressure of 0.7 Pa have average Young's modulus of 290 GPa and Poisson's ratio of 0.36. These values gradually decrease with increasing Ar partial pressure, but are independent of TiN film thickness. Fracture strength of a TiN/Si/TiN composite specimen shows dependence on film thickness, regardless of Ar partial pressure.

  2. XRD Technique: A way to disseminate structural changes in iron-based amorphous materials

    SciTech Connect

    Saw, C K; Lian, T; Day, D; Farmer, J

    2007-05-24

    Prevention of corrosion is a vital goal for the Department of Defense when billions of dollars are spent every year. Corrosion resistant materials have applications in all sort of military vehicles, and more importantly in naval vessels and submarines which come in contact with the seawater. It is known that corrosion resistance property can be improved by the used of structurally designed materials in the amorphous state where the atoms are arranged in a non-periodic fashion and specific atoms, tailored to the required properties can be interjected into the matrix for specific application. The XRD techniques reported here is to demonstrate the optimal conditions for characterization of these materials. The samples, which normally contain different compositions of Fe, Cr, B, Mo, Y, Mn, Si and W, are in the form of powders, ribbons and coatings. These results will be compared for the different forms of the sample which appears to correlate to the cooling rate during sample processing. In most cases, the materials are amorphous or amorphous with very small amount of crystallinity. In the ribbon samples for different compositions we observed that the materials are essentially amorphous. In most cases, starting from an amorphous powder sample, the coatings are also observed to be amorphous with a small amount of iron oxide on the surface, probably due to exposure to air.

  3. Radiometric, SEM and XRD investigation of the Chituc black sands, southern Danube Delta, Romania.

    PubMed

    Margineanu, R M; Blebea-Apostu, Ana-Maria; Celarel, Aurelia; Gomoiu, Claudia-Mariana; Costea, C; Dumitras, Delia; Ion, Adriana; Duliu, O G

    2014-12-01

    The black sand of the Chituc marine sand bank, northern of the city of Navodari (Romania), presents anomalous high radioactivity. Field measurements recorded in some places dose rate up to 200 nSv/h, significantly overpassing the average value of 44 ± 20 nSv/h along the entire Southern sector of Romanian Black Sea shore. Gamma ray spectrometry performed on both Slanic-Prahova Underground Low Background Laboratory and Geological Institute of Romania Radiometric Facilities showed with clarity the dominance of (228)Ac radioisotope in the 50 microns fraction together with the (226)Ra and traces of (40)K. No significant amount of anthropogenic (137)Cs was identified. Based on radiometric as well as on SEM-EDAX and XRD determinations we come to the conclusion that the evidenced radioactivity could be attributed to both uranium and thorium series in the zircon and monazite fractions and to a lesser extent to potassium in the feldspars. PMID:25181034

  4. Correlative Characterization of Li-S Batteries Using In situ TXM and XRD

    NASA Astrophysics Data System (ADS)

    Nelson, Johanna; Misra, Sumohan; Yang, Yuan; Jackson, Ariel; Cui, Yi; Andrews, Joy; Toney, Michael

    2011-11-01

    Sulfur is an attractive Li-ion battery cathode material candidate because of its high specific energy (2600 Wh/kg); however, it is well known that Li-S batteries suffer from capacity loss or fading. It is generally accepted that this is due to the loss of active material and the formation of nonconducting Li2S as a thin film coating the electrode. Both phenomena stem from the dissolution of active sulfur particles in the non-aqueous electrolyte as soluble long chain polysulfides form during the early stages of cell discharge. Using in situ, high resolution transmission X-ray microscopy (TXM) at SSRL beam line 6-2 and in situ X-ray diffraction (XRD) at beam line 11-3, we have explored initial discharge and charge cycle of Li-S batteries in real time. By combining these complementary methods, we can characterize the morphological changes of the active material as well as changes in crystallinity and crystal structure. We can then correlate these changes and the electrochemistry to better understand the reduction of elemental sulfur and various adaptations employed to retain battery capacity over many cycles.

  5. FTIR spectroscopic, thermal and XRD characterization of hydroxyapatite from new natural sources.

    PubMed

    Shaltout, Abdallah A; Allam, Moussa A; Moharram, Mohamed A

    2011-12-01

    The inorganic constituents of 5 different plants (leaves and stalks) were investigated by using Fourier transformer infrared spectroscopy (FTIR), X-ray diffraction (XRD) and thermal analysis including thermal gravimetric analysis (TGA), derivative thermogravimetry (DTG) and differential scanning calorimetry (DSC). These plants are Catha edulis (Khat), basil, mint, green tea and trifolium. The absorption bands of carbonate ions CO(3)(2-) was exhibited at 1446 cm(-1), and the phosphate ions PO(4)(3-) was assigned at 1105 and 1035 cm(-1). At high temperatures (600, 700 and 600°C) further absorption bands of the phosphate ions PO(4)(3-) was assigned at the frequencies 572, 617, 962, 1043 and 1110 cm(-1) and the vibrational absorption band of the carbonate ions CO(3)(2-) was assigned at 871, 1416 and 1461 cm(-1). X-ray diffraction and thermal analysis confirm the obtained results of FITR. Results showed that the main inorganic constituents of C. edulis and basil leaves are hydroxyapatite whereas the hydroxyapatite content in the other plant samples is less than that in case of C. edulis and basil plant leaves. PMID:21903453

  6. Synchrotron Radiation XRD Analysis of Indialite in Y-82094 Ungrouped Carbonaceous Chondrite

    NASA Technical Reports Server (NTRS)

    Mikouchi, T.; Hagiya, K.; Sawa, N.; Kimura, M.; Ohsumi, K.; Komatsu, M.; Zolensky, M.

    2016-01-01

    Y-82094 is an ungrouped type 3.2 carbonaceous chondrite, with abundant chondrules making 78 vol.% of the rock. Among these chondrules, an unusual porphyritic Al-rich magnesian chondrule is reported that consists of a cordierite-like phase, Al-rich orthopyroxene, cristobalite, and spinel surrounded by an anorthitic mesostasis. The reported chemical formula of the cordierite-like phase is Na(0.19)Mg(1.95)Fe(0.02)Al(3.66)Si(5.19)O18, which is close to stoichiometric cordierite (Mg2Al3[AlSi5O18]). Although cordierite can be present in Al-rich chondrules, it has a high temperature polymorph (indialite) and it is therefore necessary to determine whether it is cordierite or indialite in order to better constrain its formation conditions. In this abstract we report on our synchrotron radiation X-ray diffraction (SR-XRD) study of the cordierite-like phase in Y-82094.

  7. Material Characterization of Electrodeposited Copper-Nickel Nanolaminated Alloy by SEM, EDS, and XRD

    NASA Astrophysics Data System (ADS)

    Wang, Irene Cheryl

    Electrodeposited nanolaminated copper-nickel alloys (Cu-Ni) exhibit excellent mechanical properties due to their modulated structure and nanocrystalline microstructure. X-ray diffraction, scanning electron microscopy, and energy dispersive X-ray spectroscopy were used to characterize the composition, grain size, phases, and laminate structure of a nanolaminated deposit to explore structure-process-property relationships. The processing method of interest was pulse current electrodeposition of Cu-Ni a rotating disk electrode (RDE) with increased rotation speed during deposition of Cu-rich layers. Although copper content was enhanced in this way, it also caused macroscopic swirls in the deposit's surface, which were reflected microstructurally as Cu-rich streaks, non-planar layers, and other inhomogeneous morphology in the nanolaminate coating. Bulk composition of the nanolaminate was calculated from XRD spectra as being over 67wt%Ni overall, with over 91wt% Ni in Ni-rich layers and over 43wt% Ni in Cu-rich layers. EDS data of the same deposit differed significantly from these values, suggesting an overall composition closer to 55 wt% Ni, with a Ni-rich layer composition of 81 wt% Ni and 8.4 wt% Ni in the Cu-rich layers. Grain sizes of 15.8--22.3 nm were calculated for the nanolaminated deposit compared to 13--19 nm grains in a monolithic Ni-rich deposit of Cu-Ni.

  8. XRD, Electron Microscopy and Vibrational Spectroscopy Characterization of Simulated SB6 HLW Glasses - 13028

    SciTech Connect

    Stefanovsky, S.V.; Nikonov, B.S.; Omelianenko, B.I.; Choi, A.; Marra, J.C.

    2013-07-01

    Sample glasses have been made using SB6 high level waste (HLW) simulant (high in both Al and Fe) with 12 different frit compositions at a constant waste loading of 36 wt.%. As follows from X-ray diffraction (XRD) and optical and scanning electron microscopy (SEM) data, all the samples are composed of primarily glass and minor concentration of spinel phases which form both isometric grains and fine cubic (∼1 μm) crystals. Infrared spectroscopy (IR) spectra of all the glasses within the range of 400-1600 cm{sup -1} consist of the bands due to stretching and bending modes in silicon-oxygen, boron-oxygen, aluminum-oxygen and iron-oxygen structural groups. Raman spectra showed that for the spectra of all the glasses within the range of 850-1200 cm{sup -1} the best fit is achieved by suggestion of overlapping of three major components with maxima at 911-936 cm{sup -1}, 988-996 cm{sup -1} and 1020-1045 cm{sup -1}. The structural network is primarily composed of metasilicate chains and rings with embedded AlO{sub 4} and FeO{sub 4} tetrahedra. Major BO{sub 4} tetrahedra and BO{sub 3} triangles form complex borate units and are present as separate constituents. (authors)

  9. FTIR spectroscopic, thermal and XRD characterization of hydroxyapatite from new natural sources

    NASA Astrophysics Data System (ADS)

    Shaltout, Abdallah A.; Allam, Moussa A.; Moharram, Mohamed A.

    2011-12-01

    The inorganic constituents of 5 different plants (leaves and stalks) were investigated by using Fourier transformer infrared spectroscopy (FTIR), X-ray diffraction (XRD) and thermal analysis including thermal gravimetric analysis (TGA), derivative thermogravimetry (DTG) and differential scanning calorimetry (DSC). These plants are Catha edulis (Khat), basil, mint, green tea and trifolium. The absorption bands of carbonate ions CO 32- was exhibited at 1446 cm -1, and the phosphate ions PO 43- was assigned at 1105 and 1035 cm -1. At high temperatures (600, 700 and 600 °C) further absorption bands of the phosphate ions PO 43- was assigned at the frequencies 572, 617, 962, 1043 and 1110 cm -1 and the vibrational absorption band of the carbonate ions CO 32- was assigned at 871, 1416 and 1461 cm -1. X-ray diffraction and thermal analysis confirm the obtained results of FITR. Results showed that the main inorganic constituents of C. edulis and basil leaves are hydroxyapatite whereas the hydroxyapatite content in the other plant samples is less than that in case of C. edulis and basil plant leaves.

  10. μ-XRF/μ-RS vs. SR μ-XRD for pigment identification in illuminated manuscripts

    NASA Astrophysics Data System (ADS)

    van der Snickt, G.; de Nolf, W.; Vekemans, B.; Janssens, K.

    2008-07-01

    For the non-destructive identification of pigments and colorants in works of art, in archaeological and in forensic materials, a wide range of analytical techniques can be used. Bearing in mind that every method holds particular limitations, two complementary spectroscopic techniques, namely confocal μ-Raman spectroscopy (μ-RS) and μ-X-ray fluorescence spectroscopy (μ-XRF), were joined in one instrument. The combined μ-XRF and μ-RS device, called PRAXIS unites both complementary techniques in one mobile setup, which allows μ- and in situ analysis. μ-XRF allows one to collect elemental and spatially-resolved information in a non-destructive way on major and minor constituents of a variety of materials. However, the main disadvantages of μ-XRF are the penetration depth of the X-rays and the fact that only elements and not specific molecular combinations of elements can be detected. As a result μ-XRF is often not specific enough to identify the pigments within complex mixtures. Confocal Raman microscopy (μ-RS) can offer a surplus as molecular information can be obtained from single pigment grains. However, in some cases the presence of a strong fluorescence background limits the applicability. In this paper, the concrete analytical possibilities of the combined PRAXIS device are evaluated by comparing the results on an illuminated sheet of parchment with the analytical information supplied by synchrotron radiation μ-X-ray diffraction (SR μ-XRD), a highly specific technique.

  11. High pressure study of group-IV clathrate by XRD and Raman scattering

    NASA Astrophysics Data System (ADS)

    Kume, Tetsuji; Sasaki, Shigeo

    2013-06-01

    Group-IV clathrates, which are open-structured Si, Ge, and Sn cage-like compounds, have attracted increasing attention because of their potential applications for thermoelectric devices due to the behavior of phonon-glass and electron-crystal. One of the keys for the intriguing properties is so called rattling vibrations of guests. The direct observation of the rattling is important for understanding of the clathrate properties. Furthermore, the systematic observations of the rattling vibrations as a function of the cage size controlled by pressure are very significant to investigate the guest-host interaction. The pressurization also throws light on the structural stability of the clathrate, which is improved by the guest atoms. The clathrate structure with sp3 network is preserved up to very high pressure. Instead of the structural change, the doped Si clathrates undergo an isostructural phase transition. This paper is concerned with the structural stabilities under high pressure and the rattling vibrations of the guest as a function of the cage size, investigated for various semiconductor clathrates (Sr8Ga16Ge30, Eu8Ga16Ge30 and so on) by means of Raman and XRD experiments. On the basis of the recent data, the guest-host interaction is discussed.

  12. Evaluation of Rock Powdering Methods to Obtain Fine-grained Samples for CHEMIN, a Combined XRD/XRF Instrument

    NASA Technical Reports Server (NTRS)

    Chipera, S. J.; Vaniman, D. T.; Bish, D. L.; Sarrazin, P.; Feldman, S.; Blake, D. F.; Bearman, G.; Bar-Cohen, Y.

    2004-01-01

    A miniature XRD/XRF (X-ray diffraction / X-ray fluorescence) instrument, CHEMIN, is currently being developed for definitive mineralogic analysis of soils and rocks on Mars. One of the technical issues that must be addressed to enable remote XRD analysis is how best to obtain a representative sample powder for analysis. For powder XRD analyses, it is beneficial to have a fine-grained sample to reduce preferred orientation effects and to provide a statistically significant number of crystallites to the X-ray beam. Although a two-dimensional detector as used in the CHEMIN instrument will produce good results even with poorly prepared powder, the quality of the data will improve and the time required for data collection will be reduced if the sample is fine-grained and randomly oriented. A variety of methods have been proposed for XRD sample preparation. Chipera et al. presented grain size distributions and XRD results from powders generated with an Ultrasonic/Sonic Driller/Corer (USDC) currently being developed at JPL. The USDC was shown to be an effective instrument for sampling rock to produce powder suitable for XRD. In this paper, we compare powder prepared using the USDC with powder obtained with a miniaturized rock crusher developed at JPL and with powder obtained with a rotary tungsten carbide bit to powders obtained from a laboratory bench-scale Retsch mill (provides benchmark mineralogical data). These comparisons will allow assessment of the suitability of these methods for analysis by an XRD/XRF instrument such as CHEMIN.

  13. Chemical bioimaging for the subcellular localization of trace elements by high contrast TEM, TEM/X-EDS, and NanoSIMS.

    PubMed

    Penen, Florent; Malherbe, Julien; Isaure, Marie-Pierre; Dobritzsch, Dirk; Bertalan, Ivo; Gontier, Etienne; Le Coustumer, Philippe; Schaumlöffel, Dirk

    2016-09-01

    Chemical bioimaging offers an important contribution to the investigation of biochemical functions, biosorption and bioaccumulation processes of trace elements via their localization at the cellular and even at the subcellular level. This paper describes the combined use of high contrast transmission electron microscopy (HC-TEM), energy dispersive X-ray spectroscopy (X-EDS), and nano secondary ion mass spectrometry (NanoSIMS) applied to a model organism, the unicellular green algae Chlamydomonas reinhardtii. HC-TEM providing a lateral resolution of 1nm was used for imaging the ultrastructure of algae cells which have diameters of 5-10μm. TEM coupled to X-EDS (TEM/X-EDS) combined textural (morphology and size) analysis with detection of Ca, P, K, Mg, Fe, and Zn in selected subcellular granules using an X-EDS probe size of approx. 1μm. However, instrumental sensitivity was at the limit for trace element detection. NanoSIMS allowed chemical imaging of macro and trace elements with subcellular resolution (element mapping). Ca, Mg, and P as well as the trace elements Fe, Cu, and Zn present at basal levels were detected in pyrenoids, contractile vacuoles, and granules. Some metals were even localized in small vesicles of about 200nm size. Sensitive subcellular localization of trace metals was possible by the application of a recently developed RF plasma oxygen primary ion source on NanoSIMS which has shown good improvements in terms of lateral resolution (below 50nm), sensitivity, and stability. Furthermore correlative single cell imaging was developed combining the advantages of TEM and NanoSIMS. An advanced sample preparation protocol provided adjacent ultramicrotome sections for parallel TEM and NanoSIMS analyses of the same cell. Thus, the C. reinhardtii cellular ultrastructure could be directly related to the spatial distribution of metals in different cell organelles such as vacuoles and chloroplast. PMID:27288221

  14. Transient Measurements Under Simulated Mantle Conditions - Simultaneous DTF-Ultrasonic Interferometry, X-Radiography, XRD

    NASA Astrophysics Data System (ADS)

    Mueller, H. J.; Schilling, F. R.; Lathe, C.; Wunder, B.

    2004-12-01

    The interpretation of seismic data from the Earth's deep interior requires measurements of the physical properties of Earth materials under experimental simulated mantle conditions. Elastic wave velocity measurement by ultrasonic interferometry is an important tool for the determination of the elastic properties in multi-anvil devices. Whereas the classical sweep method is very time-consuming, the ultrasonic data transfer function technique (DTF), simultaneously generating all the frequencies used in the experiment, first described by Li et al. (2002), requires just few seconds to save the response of the system. The success of the technique substantially depends on the excitation function and the resolution used for saving the DTF (Mueller et al., 2004a). Background discussion as well as high pressure AƒA_A,A¿A,A 1/2 high temperature results demonstrate how to optimize the technique. All Ultrasonic interferometry allows highly precise travel time measurement at a sample enclosed in a high-pressure multi-anvil device. But under high pressure conditions the influence of sample deformation on the frequencies for destructive and constructive interference used for the evaluation of the elastic properties might be stronger than that from the shift of the elastic moduli. Consequently ultrasonic interferometry requires the exact sample length measurement under in situ conditions. X-ray imaging using brillant synchrotron radiation, called X-radiography, produces grey-scale images of the sample under in situ conditions by converting the X-ray image to an optical one by a CE-YAG-crystal. Saving the optical image by a CCD-camera after redirection by a mirrow, also requires few seconds. To derive the sample length, the different brightness of sample, buffer rod and reflector at the electronic image is evaluated (Mueller et al., 2004b). Contrary to XRD measurements, imaging the sample by X-rays requires a beam diameter larger than the sample length. Therefore the fixed

  15. Quantitative shock stage assessment in olivine and pyroxene bearing meteorites via in situ micro-XRD

    NASA Astrophysics Data System (ADS)

    McCausland, P. J.; Flemming, R. L.; Izawa, M. R.

    2010-12-01

    Shock metamorphism is observed in most meteorites and impact structures [1]. Qualitative petrographic observations underpin a shock classification system [1-3] based on the deformation features in common silicates and on textural relations such as the development of maskelynite from feldspars, mobility of sulphides and metal in veins and local Fe-reduction in silicates. Shock deformation of minerals produces streaks (mosaicity) rather than discrete spots in 2D X-ray diffraction patterns, representing the progressive disruption of the crystal lattice into a mosaic of rotated domains [4,5]. Here we use in situ micro-XRD [5,6] to measure the mosaicity of olivine and pyroxene in ordinary chondrites of increasing shock stages S1 to S5 and then apply the method to achondrites with qualitatively low to high shock. X-ray diffraction data were collected in situ on polished thin sections and slab cut surfaces using a Bruker D8 Discover micro X-ray diffractometer [5], operated using CuKα radiation generated at 40 kV and 40 mA with a beam diameter of 500 μm. Diffracted X-rays were recorded with a 2D detector, giving images with information in both the 2-theta and chi dimensions, in which each lattice plane (hkl) will have a diffraction spot or streak lying along an arc in chi of radius 2-theta (hkl). Individual reflections can be indexed and then integrated as a function of chi angle, allowing examination of the peak shape and quantitative analysis of the mosaic peak FWHM along chi. We find that both forsterite and enstatite exhibit greater mosaicity in chi with increasing shock stage: Forsterite chi ranges from <1° for S1 to >6° for S5. Enstatite chi values from the same meteorites show a more subdued growth of streak length with shock state, from ~1° to ~4°. A slab of the olivine shergottite DaG 476 exhibits forsterite mosaicity of 6.9°+/-1.1°, indicating that it has experienced shock stage S5, with shock pressures 30-45 GPa [1,4], consistent with the 40-45 GPa shock

  16. Annealing dynamics of WO{sub 3} by in situ XRD

    SciTech Connect

    Righettoni, Marco; Pratsinis, Sotiris E.

    2014-11-15

    Highlights: • Flame-made WO{sub 3} nanoparticles with closely controlled crystal and grain size. • Dynamic phase transition of annealing of pure and Si-doped WO{sub 3} by in situ XRD. • Irreversible evolution of WO{sub 3} crystallinity by heating/cooling during its annealing. • Si-doping alters the WO{sub 3} crystallinity dynamics and stabilizes nanosized WO{sub 3}. • Flame-made nano-WO{sub 3} can sense NO at the ppb level. - Abstract: Tungsten trioxide is a semiconductor with distinct applications in gas sensors, catalysis, batteries and pigments. As such the transition between its different crystal structures during its annealing are of interest, especially for sensor applications. Here, WO{sub 3} nanoparticles with closely controlled crystal and grain size (9–15 nm) and phase composition are made by flame spray pyrolysis and the formation of different WO{sub 3} phases during annealing is investigated. Most notably, the dynamic phase transition and crystal size evolution of WO{sub 3} during heating and cooling is monitored by in situ X-ray diffraction revealing how metastable WO{sub 3} phases can be captured stably. The effect of Si-doping is studied since it is used in practise to control crystal growth and phase transition during metal oxide synthesis and processing. Finally the influence of annealing on the WO{sub 3} sensing performance of NO, a lung inflammation tracer in the human breath, is explored at the ppb-level.

  17. Geoelectrical characterization by joint inversion of VES/TEM in Paraná basin, Brazil

    NASA Astrophysics Data System (ADS)

    Bortolozo, C. A.; Couto, M. A.; Almeida, E. R.; Porsani, J. L.; Santos, F. M.

    2012-12-01

    For many years electrical (DC) and transient electromagnetic (TEM) soundings have been used in a great number of environmental, hydrological and mining exploration studies. The data of both methods are interpreted usually by individual 1D models resulting in many cases in ambiguous models. This can be explained by how the two different methodologies sample the subsurface. The vertical electrical sounding (VES) is good on marking very resistive structures, while the transient electromagnetic sounding (TEM) is very sensitive to map conductive structures. Another characteristic is that VES is more sensitive to shallow structures, while TEM soundings can reach deeper structures. A Matlab program for joint inversion of VES and TEM soundings, by using CRS algorithm was developed aiming explore the best of the both methods. Initially, the algorithm was tested with synthetic data and after it was used to invert experimental data from Paraná sedimentary basin. We present the results of a re-interpretation of 46 VES/TEM soundings data set acquired in Bebedouro region in São Paulo State - Brazil. The previous interpretation was based in geoelectrical models obtained by single inversion of the VES and TEM soundings. In this work we present the results with single inversion of VES and TEM sounding inverted by the Curupira Program and a new interpretation based in the joint inversion of both methodologies. The goal is increase the accuracy in determining the underground structures. As a result a new geoelectrical model of the region is obtained.

  18. Elucidation of reaction mechanism involved in the formation of LaNiO3 from XRD and TG analysis

    NASA Astrophysics Data System (ADS)

    Dharmadhikari, Dipti V.; Athawale, Anjali A.

    2013-06-01

    The present work is focused on the synthesis and elucidation of reaction mechanism involved in the formation of LaNiO3 with the help of X-ray diffraction (XRD) and thermogravimetric (TG) analysis. LaNiO3 was synthesized by hydrothermal method by heating at 160°C under autogenous pressure for 6h. Pure phase product was obtained after calcining the hydrothermally activated product for 6h at 700°C. The various phases of the product obtained after hydrothermal treatment and calcination followed by the formation of pure phase nanocrystalline lanthanum nickel oxide could be determined from XRD analysis of the samples. The reaction mechanism and phase formation temperature has been interpreted by thermogravimetric analysis of the hydrothermally synthesized product and XRD analysis.

  19. Thermal Analysis of SRF Cavity Couplers Using Parallel Multiphysics Tool TEM3P

    SciTech Connect

    Akcelik, V; Lee, L.-Q.; Li, Z.; Ng, C.-K.; Ko, K.; Cheng, G.; Rimmer, R.; Wang, H.; /Jefferson Lab

    2009-05-20

    SLAC has developed a multi-physics simulation code TEM3P for simulating integrated effects of electromagnetic, thermal and structural loads. TEM3P shares the same software infrastructure with SLAC's parallel finite element electromagnetic codes, thus enabling all physics simulations within a single framework. The finite-element approach allows high-fidelity, high-accuracy simulations and the parallel implementation facilitates large-scale computation with fast turnaround times. In this paper, TEM3P is used to analyze thermal loading at coupler end of the JLAB SRF cavity.

  20. Thermal Analysis of SRF Cavity Couplers Using Parallel Multiphysics Tool TEM3P

    SciTech Connect

    Akcelik, V, Lee, L.-Q., Li, Z., Ng, C.-K., Ko, K.,Cheng, G., Rimmer, R., Wang, H.

    2009-05-01

    SLAC has developed a multi-physics simulation code TEM3P for simulating integrated effects of electromagnetic, thermal and structural loads. TEM3P shares the same software infrastructure with SLAC’s paralell finite element electromagnetic codes, thus enabling all physics simulations within a single framework. The finite-element approach allows high fidelity, high-accuracy simulations and the parallel implementation facilitates large-scale computation with fast turnaround times. In this paper, TEM3P is used to analyze thermal loading at coupler end of the JLAB SRF cavity.

  1. ESR and XRD investigation of effects induced by gamma radiation on PVA-TiO2 membranes

    NASA Astrophysics Data System (ADS)

    Todica, Mihai; Stefan, Traian; Trandafir, Diana; Simon, Simion

    2013-07-01

    The effects of gamma radiation on the local structure of PVA membranes containing TiO2 were investigated by ESR and XRD methods. An intense ESR signal is observed after irradiation at 16 KGy dose. This signal appears only for irradiated samples and it is associated with the breaking of the polymeric chain, followed by local reorganization of the polymeric segments and the apparition of the unpaired electrons and free radicals. The intensity of the signal decreases with the concentration of TiO2, indicating a shielding effect of the dopand. That the modification of local order of the polymeric chains has been modified after irradiation is confirmed by XRD method.

  2. XRD and XPS analysis of the degradation of the polymer electrolyte in H 2-O 2 fuel cell

    NASA Astrophysics Data System (ADS)

    Huang, Chengde; Seng Tan, Kim; Lin, Jianyi; Lee Tan, Kuang

    2003-03-01

    Nafion ® is frequently used as electrolyte membrane in polymer electrolyte fuel cells (PEFC). In this Letter the degradation of the Nafion ® polymer electrolyte was investigated using X-ray powder diffraction (XRD) and X-ray photoelectron spectroscopy (XPS). XRD showed that the electrode potential and low gas humidification temperature could decrease the crystallinity of Nafion ®. XPS analysis indicated that the Nafion ® was decomposed in the hydrogen potential region of the fuel cell, through the interaction of the hydrophobic (CF 2) n groups of the membrane with H or/and C atoms.

  3. Interaction of selenite with reduced Fe and/or S species: An XRD and XAS study

    NASA Astrophysics Data System (ADS)

    Finck, Nicolas; Dardenne, Kathy

    2016-05-01

    In this study, we investigated the interaction between selenite and either Fe(II)aq or S(- II)aq in solution, and the results were used to investigate the interaction between Se(IV)aq and FeS in suspension. The reaction products were characterized by a combination of methods (SEM, XRD and XAS) and the reaction mechanisms were identified. In a first experiment, Se(IV)aq was reduced to Se(0) by interaction with Fe(II)aq which was oxidized to Fe(III), but the reaction was only partial. Subsequently, some Fe(III) produced akaganeite (β-FeOOH) and the release of proton during that reaction decreased the pH. The pH decrease changed the Se speciation in solution which hindered further Se(IV) reduction by Fe(II)aq. In a second experiment, Se(IV)aq was quantitatively reduced to Se(0) by S(- II)aq and the reaction was fast. Two sulfide species were needed to reduce one Se(IV), and the observed pH increase was due to a proton consumption. For both experiments, experimental results are consistent with expectations based on the oxidation reduction potential of the various species. Upon interaction with FeS, Se(IV)aq was reduced to Se(0) and minute amounts of pyrite were detected, a consequence of partial mackinawite oxidation at surface sulfur sites. These results are of prime importance with respect to safe deep disposal of nuclear waste which contains the long-lived radionuclide 79Se. This study shows that after release of 79Se(IV) upon nuclear waste matrix corrosion, selenite can be reduced in the near field to low soluble Se(0) by interaction with Fe(II)aq and/or S(- II)aq species. Because the solubility of Se(0) species is significantly lower than that of Se(IV), selenium will become much less (bio)available and its migration out of deep HLW repositories may be drastically hindered.

  4. Interaction of selenite with reduced Fe and/or S species: An XRD and XAS study.

    PubMed

    Finck, Nicolas; Dardenne, Kathy

    2016-05-01

    In this study, we investigated the interaction between selenite and either Fe((II))aq or S((-II))aq in solution, and the results were used to investigate the interaction between Se((IV))aq and FeS in suspension. The reaction products were characterized by a combination of methods (SEM, XRD and XAS) and the reaction mechanisms were identified. In a first experiment, Se((IV))aq was reduced to Se((0)) by interaction with Fe((II))aq which was oxidized to Fe((III)), but the reaction was only partial. Subsequently, some Fe((III)) produced akaganeite (β-FeOOH) and the release of proton during that reaction decreased the pH. The pH decrease changed the Se speciation in solution which hindered further Se((IV)) reduction by Fe((II))aq. In a second experiment, Se((IV))aq was quantitatively reduced to Se((0)) by S((-II))aq and the reaction was fast. Two sulfide species were needed to reduce one Se((IV)), and the observed pH increase was due to a proton consumption. For both experiments, experimental results are consistent with expectations based on the oxidation reduction potential of the various species. Upon interaction with FeS, Se((IV))aq was reduced to Se((0)) and minute amounts of pyrite were detected, a consequence of partial mackinawite oxidation at surface sulfur sites. These results are of prime importance with respect to safe deep disposal of nuclear waste which contains the long-lived radionuclide (79)Se. This study shows that after release of (79)Se((IV)) upon nuclear waste matrix corrosion, selenite can be reduced in the near field to low soluble Se((0)) by interaction with Fe((II))aq and/or S((-II))aq species. Because the solubility of Se((0)) species is significantly lower than that of Se((IV)), selenium will become much less (bio)available and its migration out of deep HLW repositories may be drastically hindered. PMID:27010738

  5. Phase-locking of oscillating images using laser-induced spin-polarized pulse TEM.

    PubMed

    Kuwahara, Makoto; Nambo, Yoshito; Kusunoki, Soichiro; Jin, Xiuguang; Saitoh, Koh; Asano, Hidefumi; Ujihara, Toru; Takeda, Yoshikazu; Nakanishi, Tsutomu; Tanaka, Nobuo

    2013-12-01

    Pulse-mode operation was realized in spin-polarized transmission electron microscopy (SP-TEM) using a laser-driven electron gun with a GaAs-GaAsP strained-layer-superlattice photocathode. TEM images were acquired with a pulsed electron beam with a 5-μs pulse duration. Phase locking of wobbling TEM images was demonstrated using a pulsed beam with a 1-kHz repetition frequency, which matched the image wobbling frequency. It was found that in composite images formed by superimposing 2 × 10(4) separate single-pulse exposures, the amount of image blurring due to wobbling was a linear function of the pulse duration. These results suggest the possibility of pump-probe measurements in SP-TEM using the pulsed electron beam as a probe, allowing nanometer-scale time-resolved spin mapping. PMID:23797969

  6. TEM00 mode Nd:YAG solar laser by side-pumping a grooved rod

    NASA Astrophysics Data System (ADS)

    Vistas, Cláudia R.; Liang, Dawei; Almeida, Joana; Guillot, Emmanuel

    2016-05-01

    A simple TEM00 mode solar laser system with a grooved Nd:YAG rod pumped through a heliostat-parabolic mirror system is reported here. The radiation coupling capacity of a fused silica tube lens was combined with the multipass pumping ability of a 2 V-shaped cavity to provide efficient side-pumping along a 4.0 mm diameter grooved Nd:YAG single-crystal rod. TEM00 mode solar laser power of 3.4 W was measured by adopting an asymmetric large-mode laser resonant cavity. Record TEM00 mode solar laser collection efficiency of 3.4 W/m2and slope efficiency of 1.9% was achieved, which corresponds to 1.8 and 2.4 times more than the previous TEM00 mode Nd:YAG solar laser using the PROMES-CNRS heliostat-parabolic mirror system, respectively.

  7. METHOD FOR CALCULATING ELECTRIC AND MAGNETIC FIELDS IN TEM CELLS AT ELF (JOURNAL VERSION)

    EPA Science Inventory

    A method is presented whereby the electric and magnetic field distributions within rectangular strip transmission lines (TEM cells) can be calculated. Quasi-static approximations are employed, thereby restricting the validity of the results to operational frequencies well below t...

  8. Jet thinning of germanium for TEM using automatic termination of polishing

    SciTech Connect

    Kestel, B.J.

    1993-01-01

    This report describes an automated jet electropolishing technique, using modified commercial equipment, for the production of germanium TEM specimens. This technique allows rapid and reliable thinning of large areas and results in clean surfaces.

  9. A comparison of TEM and DLS methods to characterize size distribution of ceramic nanoparticles

    NASA Astrophysics Data System (ADS)

    Souza, T. G. F.; Ciminelli, V. S. T.; Mohallem, N. D. S.

    2016-07-01

    The accuracy of dynamic light scattering (DLS) measurements are compared with transmission electron microscopy (TEM) studies for characterization of size distributions of ceramic nanoparticles. It was found that measurements by DLS using number distribution presented accurate results when compared to TEM. The presence of dispersants and the enlargement of size distributions induce errors to DLS particle sizing measurements and shifts its results to higher values.

  10. In situ TEM tensile testing of carbon-linked graphene oxide nanosheets using a MEMS device

    NASA Astrophysics Data System (ADS)

    Cao, Changhong; Howe, Jane Y.; Perovic, Doug; Filleter, Tobin; Sun, Yu

    2016-07-01

    This paper reports in situ transmission electron microscopy (TEM) tensile testing of carbon-linked graphene oxide nanosheets using a monolithic TEM compatible microelectromechanical system device. The set-up allows direct on-chip nanosheet thickness mapping, high resolution electron beam linking of a pre-fractured nanosheet, and mechanical tensile testing of the nanosheet. This technique enables simultaneous mechanical and high energy electron beam characterization of 2D nanomaterials.

  11. In situ TEM tensile testing of carbon-linked graphene oxide nanosheets using a MEMS device.

    PubMed

    Cao, Changhong; Howe, Jane Y; Perovic, Doug; Filleter, Tobin; Sun, Yu

    2016-07-15

    This paper reports in situ transmission electron microscopy (TEM) tensile testing of carbon-linked graphene oxide nanosheets using a monolithic TEM compatible microelectromechanical system device. The set-up allows direct on-chip nanosheet thickness mapping, high resolution electron beam linking of a pre-fractured nanosheet, and mechanical tensile testing of the nanosheet. This technique enables simultaneous mechanical and high energy electron beam characterization of 2D nanomaterials. PMID:27256541

  12. Novel freestanding nanotube devices for combining TEM and electron diffraction with Raman and Transport

    SciTech Connect

    Meyer, Jannik C.; Obergfell, Dirk; Roth, Siegmar; Paillet, Matthieu; Sauvajol, Jean-Louis; Neumann, Anita; Duesberg, Georg

    2005-09-27

    A versatile procedure for combining high-resolution transmission electron microscopy (TEM) and electron diffraction with Raman spectroscopy and transport measurements on the very same nanotube is presented. For this we prepare free-standing structures on the corner of a substrate by electron beam lithography and an etching process. Further, this procedure makes possible a TEM quality control of nanotubes grown directly on the substrate.

  13. Kinetic Study of the Effect of Histidines 240 and 164 on TEM-149 Enzyme Probed by β-Lactam Inhibitors

    PubMed Central

    Mancini, Alisia; Celenza, Giuseppe; Bottoni, Carlo; Bellio, Pierangelo; Sabatini, Alessia; Di Pietro, Letizia; Brisdelli, Fabrizia; Segatore, Bernardetta; Amicosante, Gianfranco

    2014-01-01

    In the present study, we performed a detailed kinetic analysis of the enzymes TEM-149, TEM-149H240, and TEM-149H164-H240 versus a large panel of inhibitors/inactivators, including penicillins, penems, carbapenems, monobactams, cephamycin, and carbacephem. These compounds behaved as poor substrates versus TEM-149, TEM-149H240, and TEM-149H164-H240 β-lactamases, and the Ki (inhibition constant), K (dissociation constant of the Henri-Michaelis complex), k+2 and k+3 (first-order acylation and deacylation constants, respectively), and k+2/K values were calculated. PMID:25092695

  14. Benchmarking of a novel contactless characterisation method for micro thermoelectric modules (μTEMs)

    NASA Astrophysics Data System (ADS)

    Hickey, S.; Punch, J.; Jeffers, N.

    2014-07-01

    Significant challenges exist in the thermal control of Photonics Integrated Circuits (PICs) for use in optical communications. Increasing component density coupled with greater functionality is leading to higher device-level heat fluxes, stretching the capabilities of conventional cooling methods using thermoelectric modules (TEMs). A tailored thermal control solution incorporating micro thermoelectric modules (μTEMs) to individually address hotspots within PICs could provide an energy efficient alternative to existing control methods. Performance characterisation is required to establish the suitability of commercially-available μTEMs for the operating conditions in current and next generation PICs. The objective of this paper is to outline a novel method for the characterisation of thermoelectric modules (TEMs), which utilises infra-red (IR) heat transfer and temperature measurement to obviate the need for mechanical stress on the upper surface of low compression tolerance (~0.5N) μTEMs. The method is benchmarked using a commercially-available macro scale TEM, comparing experimental data to the manufacturer's performance data sheet.

  15. Correlation between full width at half maximum (FWHM) of XRD peak with residual stress on ground surfaces

    NASA Astrophysics Data System (ADS)

    Vashista, M.; Paul, S.

    2012-11-01

    The full width at half maximum (FWHM) of XRD profiles is used to characterize different material properties and surface integrity features. However, there is no literature available that discusses the nature of the correlation between the FWHM of XRD peaks with induced surface residual stress upon grinding with simultaneous occurrence of plastic deformation, formation of white layer, grain elongation, change in microhardness, etc. AISI 1060 steel samples were ground under different grinding domains, i.e. conventional abusive grinding, conventional grinding, cBN grinding and high speed grinding with moderately deep cut. Induction of tensile and compressive residual stress, microstructural changes, white layer formation, grain refinement, plastic deformation, grain elongation and change in microhardness were observed upon grinding AISI 1060 steel. A correlation was established between the FWHM of XRD peaks and surface residual stress when simultaneous changes in microhardness and microstructure, grain elongation, plastic deformation and formation of white layer take place due to grinding. The correlation between FWHM of XRD peak and residual stress appears to be nonlinear due to simultaneous change in other aspects of surface integrity.

  16. Structure and Output Characteristics of a TEM Array Fitted to a Fin Heat Exchanger

    NASA Astrophysics Data System (ADS)

    Zhang, Z.; Chen, L. N.; Chen, Z. J.; Xiao, G. Q.; Liu, Z. J.

    2015-06-01

    In the design of a thermoelectric generator, both the heat transfer area and the number of thermoelectric modules (TEMs) should be increased accordingly as the generator power increases; crucially, both aspects need to be coordinated. A kilowatt thermoelectric generator with a fin heat exchanger is proposed for use in a constant-speed diesel generator unit. Interior fins enhance convective heat transfer, whereas an exterior fin segment increases the heat transfer area. The heat transfer surface is double that of a plane heat exchanger, and the temperature field over the exterior fins is constrained to a one-dimensional distribution. Between adjoining exterior fins, there is a cooling water channel with trapezoid cross-section, enabling compact TEMs and cooling them. Hence, more TEMs are built as a series-parallel array of TEMs with lower resistance and more stable output current. Under nonuniform conditions, to prevent circulation and energy loss, bypass diodes and antidiodes are added. Experiments and numerical calculations show that, with matching and optimization of the heat exchanger and TEM array, a stable maximum output power is obtainable from the interior of the thermoelectric generator system, which can be connected to an external maximum power point tracking system.

  17. Developing of an environmental cell TEM holder for dynamic in situ observation

    NASA Astrophysics Data System (ADS)

    Bataineh, Khaled M.

    2016-02-01

    This paper deals with the subject of "in situ" development of environmental-transmission electron microscope (E-TEM) holder assemblies. In E-TEM, the sample is continuously subjected to gases as opposed to conventional TEM where the sample is under high vacuum. E-TEM offers the possibility of achieving a new level of material analysis. E-TEM allows obtaining information about chemical information during the reaction at atomic level. Rarefied gas dynamics analysis is used to assess the proposed design. The analysis is focused on determining the molecular distribution inside the vacuum chamber and calculating the impingement rate on the target surface of the specimen. Simulations are performed to predict the molecular interaction with the specimen at given pressures to determine the proper position of a specimen within a vacuum chamber to optimize and predict reaction characteristics. Results of direct simulation Monte Carlo show that the two sides of the sample operate at different temperatures due to the gas flow and experience different molecular distributions.

  18. As-rigid-as-possible mosaicking and serial section registration of large ssTEM datasets

    PubMed Central

    Saalfeld, Stephan; Cardona, Albert; Hartenstein, Volker; Tomančák, Pavel

    2010-01-01

    Motivation: Tiled serial section Transmission Electron Microscopy (ssTEM) is increasingly used to describe high-resolution anatomy of large biological specimens. In particular in neurobiology, TEM is indispensable for analysis of synaptic connectivity in the brain. Registration of ssTEM image mosaics has to recover the 3D continuity and geometrical properties of the specimen in presence of various distortions that are applied to the tissue during sectioning, staining and imaging. These include staining artifacts, mechanical deformation, missing sections and the fact that structures may appear dissimilar in consecutive sections. Results: We developed a fully automatic, non-rigid but as-rigid-as-possible registration method for large tiled serial section microscopy stacks. We use the Scale Invariant Feature Transform (SIFT) to identify corresponding landmarks within and across sections and globally optimize the pose of all tiles in terms of least square displacement of these landmark correspondences. We evaluate the precision of the approach using an artificially generated dataset designed to mimic the properties of TEM data. We demonstrate the performance of our method by registering an ssTEM dataset of the first instar larval brain of Drosophila melanogaster consisting of 6885 images. Availability: This method is implemented as part of the open source software TrakEM2 (http://www.ini.uzh.ch/∼acardona/trakem2.html) and distributed through the Fiji project (http://pacific.mpi-cbg.de). Contact: tomancak@mpi-cbg.de PMID:20529937

  19. Developing of an environmental cell TEM holder for dynamic in situ observation.

    PubMed

    Bataineh, Khaled M

    2016-02-01

    This paper deals with the subject of "in situ" development of environmental-transmission electron microscope (E-TEM) holder assemblies. In E-TEM, the sample is continuously subjected to gases as opposed to conventional TEM where the sample is under high vacuum. E-TEM offers the possibility of achieving a new level of material analysis. E-TEM allows obtaining information about chemical information during the reaction at atomic level. Rarefied gas dynamics analysis is used to assess the proposed design. The analysis is focused on determining the molecular distribution inside the vacuum chamber and calculating the impingement rate on the target surface of the specimen. Simulations are performed to predict the molecular interaction with the specimen at given pressures to determine the proper position of a specimen within a vacuum chamber to optimize and predict reaction characteristics. Results of direct simulation Monte Carlo show that the two sides of the sample operate at different temperatures due to the gas flow and experience different molecular distributions. PMID:26931858

  20. Characterization of pre-Hispanic pottery from Teotihuacan, Mexico, by a combined PIXE-RBS and XRD analysis

    NASA Astrophysics Data System (ADS)

    Ruvalcaba-Sil, J. L.; Ontalba Salamanca, M. A.; Manzanilla, L.; Miranda, J.; Cañetas Ortega, J.; López, C.

    1999-04-01

    A combined analysis of IBA techniques (Proton Induced X-ray Emission (PIXE) and Rutherford Backscattering Spectroscopy (RBS)) and a complementary study by X-ray Diffraction (XRD) were performed to characterize pottery corresponding to the Epiclassic period (A.D. 700-900) from Teotihuacan, Mexico. Elemental compositions of pottery samples were measured by simultaneous PIXE and RBS using 2.6 MeV protons. Red, white and brown pottery pigments were studied by non-vacuum PIXE and a proton beam of 3 MeV. The various mineralogical phases of the pottery were identified by XRD. From pottery elemental compositions and its mineralogical phases, some differences among the pottery samples and groups were established.

  1. Non-destructive and in situ identification of rice paper, seals and pigments by FT-IR and XRD spectroscopy.

    PubMed

    Na, Na; Ouyang, Qi-Ming; Ma, Hui; Ouyang, Jin; Li, Yanping

    2004-11-15

    This paper studied the chemical characteristics of rice paper, pigments and seals on Chinese calligraphies and traditional Chinese paintings. The techniques used here were Fourier transform infrared (FT-IR) spectroscopy and X-ray diffraction (XRD). FT-IR allows good identification of the substances present in pigments and inkpads and differentiates each era of rice paper. This can be the base of estimating the age of rice paper. Different crystalline phases can be identified by XRD, which is further evidence to separate different kinds of pigments or inkpads. Both of these methods were non-destructive in situ analysis and can be used in the identification in calligraphies and traditional Chinese paintings. These results confirmed that the applied techniques are relatively quicker and more reliable than traditional approaches authenticated by years of experience. PMID:18969703

  2. Preparation and XRD analyses of Na-doped ZnO nanorod arrays based on experiment and theory

    NASA Astrophysics Data System (ADS)

    Yang, X. P.; Lu, J. G.; Zhang, H. H.; Chen, Y.; Kan, B. T.; Zhang, J.; Huang, J.; Lu, B.; Zhang, Y. Z.; Ye, Z. Z.

    2012-03-01

    ZnO nanorod arrays (NRAs) with different Na contents were prepared by thermal evaporation. Sodium pyrophosphate was adopted as the Na source. The Na contents in NRAs were determined by X-ray photoelectron spectra to be 0, 6.1, and 9.4 at.%. X-ray diffraction (XRD) analyses of Na-doped ZnO NRAs were performed in experiment and by first-principle calculation with the assumption of Na substitutions. A couple of typical changes were found in XRD patterns of Na-doped ZnO. The simulation results well agreed with the experimental data, which revealed that Na mainly located at the substitutional sites in Na-doped ZnO NRAs.

  3. Leonardo da Vinci's drapery studies: characterization of lead white pigments by µ-XRD and 2D scanning XRF

    NASA Astrophysics Data System (ADS)

    Gonzalez, Victor; Calligaro, Thomas; Pichon, Laurent; Wallez, Gilles; Mottin, Bruno

    2015-11-01

    This work focuses on the composition and microstructure of the lead white pigment employed in a set of paintworks, using a combination of µ-XRD and 2D scanning XRF, directly applied on five drapery studies attributed to Leonardo da Vinci (1452-1519) and conserved in the Département des Arts Graphiques, Musée du Louvre and in the Musée des Beaux- Arts de Rennes. Trace elements present in the composition as well as in the lead white highlights were imaged by 2D scanning XRF. Mineral phases were determined in a fully noninvasive way using a special µ-XRD diffractometer. Phase proportions were estimated by Rietveld refinement. The analytical results obtained will contribute to differentiate lead white qualities and to highlight the artist's technique.

  4. An exploratory method to detect tephras from quantitative XRD scans: Examples from Iceland and east Greenland marine sediments

    USGS Publications Warehouse

    Andrews, John T.; Eberl, D.D.; Kristjansdottir, G.B.

    2006-01-01

    Tephras, mainly from Iceland, are becoming increasingly important in interpreting leads and lags in the Holocene climate system across NW Europe. Here we demonstrate that Quantitative Phase Analysis of x-ray diffractograms of the 150 um fraction and identify these same peaks in XRD scans - two of these correlate geochemically and chronologically with Hekla 1104 and 3. At a distal site to the WNW of Iceland, on the East Greenland margin (core MD99-2317), the weight% of volcanic glass reaches values of 11% at about the time of the Saksunarvatn tephra. The XRD method identifies the presence of volcanic glass but not its elemental composition; hence it will assist in focusing attention on specific sections of sediment cores for subsequent geochemical fingerprinting of tephras. ?? 2006 SAGE Publications.

  5. On the Development of Thermally Stable Semi-IPNs of PVA and PAN using IR, DSC and XRD Studies

    NASA Astrophysics Data System (ADS)

    Deshpande, Deepti S.; Bajpai, R.; Bajpai, A. K.

    2011-07-01

    A novel biopolymer based Semi-IPN of polyvinyl alcohol (PVA) and polycrylonitrile (PAN) were synthesized in various proportions by redox polymerization and analyzed thermally by differential scanning calorimetry (DSC). DSC thermograms shows good thermal stability, as a result of incorporation of acrylonitrile as the second network. The structural and morphological study of these semi-IPNs by FTIR and XRD technique, respectively, were correlated. The approach seems to be beneficial for various biomedical applications.

  6. In-Situ Study of Gaseous Reduction of Magnetite Doped with Alumina Using High-Temperature XRD Analysis

    NASA Astrophysics Data System (ADS)

    Kapelyushin, Yury; Sasaki, Yasushi; Zhang, Jianqiang; Jeong, Sunkwang; Ostrovski, Oleg

    2015-12-01

    The reduction of magnetite of technical grade and magnetite doped with 3 mass pct Al2O3 was studied in situ using high-temperature XRD (HT-XRD) analysis. Magnetite was reduced by CO-CO2 gas (80 vol pct CO) at 1023 K (750 °C). Reduction of magnetite doped with alumina occurred from the Fe3O4-FeAl2O4 solid solution which has a miscibility gap with critical temperature of 1133 K (860 °C). The degree of reduction of magnetite was derived using Rietveld refinement of the HT-XRD spectra; the compositions of the Fe3O4-FeAl2O4 solid solution and the concentrations of carbon in γ-iron were determined from the lattice constants of the solutions. The reduction of magnetite progressed topochemically with the formation of a dense iron shell. The reduction of alumina-containing magnetite started along certain lattice planes with the formation of a network-like structure. Reduction of alumina-containing magnetite was faster than that of un-doped magnetite; this difference was attributed to the formation of the network-like structure. Hercynite content in the Fe3O4-FeAl2O4 solid solution in the process of reduction of magnetite doped with 3 mass pct Al2O3 increased from 5.11 to 20 mass pct, which is close to the miscibility gap at 1023 K (750 °C). The concentration of carbon in γ-Fe (0.76 mass pct) formed in the reduced sample of magnetite doped with 3 mass pct Al2O3 was close to the equilibrium value with 80 vol pct CO to 20 vol pct CO2 gas used in the HT-XRD experiments.

  7. Generation of entangled TEM01 modes with periodically poled KTiOPO4 crystal

    NASA Astrophysics Data System (ADS)

    Rong-Guo, Yang; Jing-jing, Wang; Jing, Zhang; Heng-Xin, Sun

    2016-07-01

    Spatial quantum optics based on the high-order transverse mode is important for the super-resolution measurement and quantum image beyond the shot noise level. Quantum entanglement of the transverse plane Hermite–Gauss TEM01 mode has been demonstrated experimentally in this paper. Two squeezed TEM01 modes, which are generated by a pair of degenerate optical parametric amplifiers (DOPA) with the nonlinear crystals of periodically poled KTiOPO4, have been combined to produce TEM01 mode entanglement using a beam splitter. The 1.5 dB for the sum of amplitude and 1.2 dB for the difference of phase below shot-noise level is achieved with the measurement system of a Bell state detection. Project supported by the National Natural Science Foundation of China (Grant Nos. 11504218 and 61108003) and the Natural Science Foundation of Shanxi Province, China (Grant No. 2013021005-2).

  8. High-power TEM00 and Laguerre-Gaussian mode generation in double resonator configuration

    NASA Astrophysics Data System (ADS)

    Kim, D. J.; Kim, J. W.

    2015-12-01

    A simple method for controlling the spatial gain distribution in an end-pumped solid-state laser to allow the selective excitation of the fundamental Gaussian (TEM00) and the first-order Laguerre-Gaussian doughnut (LG01) modes is reported. This approach has been applied to a Nd:YAG laser yielding 2.21 W of the TEM00 mode output and 1.62 W of the LG01 mode output at 1064 nm for 7.36 W of incident pump power at 808 nm. The corresponding slope efficiencies with respect to incident pump power were 40 and 32 % for the TEM00 and LG01 modes, respectively. The underlying mechanism and the prospects for further improvement in laser performance are discussed.

  9. Theoretical Study the Error Caused by Dipole Hypothesis of Large-loop TEM Response

    NASA Astrophysics Data System (ADS)

    Yan, S.; Xue, G.; Zhou, N.

    2010-12-01

    Transient electromagnetic method (Transient Electromagnetic Field is TEM for short) is an time domain artificial sources of electromagnetic detection method based on the principle of electromagnetic induction. This method has higher sensitivity for the anomalous body of low resistivity , a stimulating can cover the required frequency bands and greatly improve the work efficiency by using a rich spectrum component pulse waveform . Also because send magnetic moment is relatively large, so the loop source system TEM has been very widely used in geological exploration, engineering, geothermal and environmental exploration which belong to medium depth ( less than 2000m) exploration [1], especially the central-loop system TEM has become the preferred method in Coalfield Hydrogeology Exploration and metal ore exploration . In order to obtain greater depth of exploration, the launch frame side of loop system commonly use large-scale form , Now the imported equipments with a large number of applications are large-loop system which shall be accounted for about 80% of the share of middle-depth exploration on the ground , sush as V-5, V8, GDP-32, PROTEM, SIROTEM, PEM, etc. If only one point be observed in the frame center to move the whole system when the side of loop system reach to hundreds of meters, the work efficiency of TEM will be greatly reduced. In order to increase the production efficiency, we will observe the points from center of loop to 0ne third of loop in the actual production, which is to think that the field in this region is approximately homogeneous. So, we can derive large-loop center-model TEM system which is different from the center-loop TEM system in the conventional sense as well as large-loop source TEM system. Fixed loop source TEM sysetm has been built based on the theory of dipole infinitesimal, which can not show more correct character in near-field area, even though this kind of theory has played more important guide in TEM study. There exist

  10. Two-in-one sample preparation for plan-view TEM.

    PubMed

    Sáfrán, György; Szász, Noémi; Sáfrán, Eszter

    2015-07-01

    Transmission electron microscopy (TEM) sample preparation requires special skills, it is time consuming and costly, hence, an increase of the efficiency is of primary importance. This article describes a method that duplicates the yield of the conventional mechanical and ion beam preparation of plan-view TEM samples. As a modification of the usual procedures, instead of one two different samples are comprised in a single specimen. The two pre-cut slabs, one from each samples, are embedded side by side in the window of a 3 mm dia Ti disk and the specimen is thinned mechanically and by ion milling until perforation that occurs at the interface of the two different slabs. That, with proper implementation, provides acceptable size thin area for the TEM study of both samples. The suitability of the two-in-one method has been confirmed through examples. PMID:25989619

  11. Combined AES, LEED, SEM and TEM characterizations of CuSi(100) interfaces

    NASA Astrophysics Data System (ADS)

    Hanbücken, M.; Métois, J. J.; Mathiez, P.; Salvan, F.

    1985-10-01

    CuSi(100) interfaces prepared under UHV at different substrate temperatures ( TS) have been characterized using in-situ Auger electron spectroscopy (AES) and low energy electron diffraction (LEED) as well as ex-situ scanning and transmission electron microscopy (SEM, TEM). At room temperature (RT), the film grows in a layer by layer like mode. With increasing TS, the intensity of the Cu M 2,3VV (61 eV) Auger transition decreases and at TS = 500°C no Cu Auger signal could be measured below θ ˜ 100. Yet SEM and TEM observations of these deposits show islands in epitaxial relation with the substrate. It can be determined from TEM images that these islands are covered with a Si skin ( ˜ 50 Å; thick) and that they are deeply implanted in the Si substrate. This explains the AES measurements.

  12. TEM CHARACTERIZATION OF IRRADIATED U3SI2/AL DISPERSION FUEL

    SciTech Connect

    J. Gan; B. Miller; D. Keiser; A. Robinson; P. Medvedev; D. Wachs

    2010-10-01

    The silicide dispersion fuel of U3Si2/Al has been recognized as a reasonably good performance fuel for nuclear research and test reactors except that it requires the use of high enrichment uranium. An irradiated U3Si2/Al dispersion fuel (~75% enrichment) from the high flux side of a RERTR-8 (U0R040) plate was characterized using transmission electron microscopy (TEM). The fuel plate was irradiated in the advanced test reactor (ATR) for 105 days. The average irradiation temperature and fission density of the fuel particles for the TEM sample are estimated to be approximately ~110 degrees C and 5.4 x 10-21 f/cm3. The characterization was performed using a 200KV TEM with a LaB6 filament. Detailed microstructural information along with composition analysis is obtained. The results and their implication on the performance of this silicide fuel are discussed.

  13. XRD (x-ray diffraction) and HREM (high resolution electron microscopy) studies of nanocrystalline Cu and Pd

    SciTech Connect

    Nieman, G.W.; Weertman, J.R. . Dept. of Materials Science and Engineering); Siegel, R.W. )

    1990-12-01

    Consolidated powders of nanocrystalline Cu and Pd have been studied by x-ray diffraction (XRD) and high resolution electron microscopy (HREM) as part of an investigation of the mechanical behavior of nanocrystalline pure metals. XRD line broadening measurements were made to estimate grain size, qualitative grain size distribution and average long range strains in a number of samples. Mean grain sizes range from 4--60 nm and have qualitatively narrow grain size distributions. Long range lattice strains are of the order of 0.2--3% in consolidated samples. These strains apparently persist and even increase in Cu samples after annealing at 0.35 Tm (498K) for 2h, accompanied by an apparent increase in grain size of {ge}2x. Grain size, grain size distribution width and internal strains vary somewhat among samples produced under apparently identical processing conditions. HREM studies show that twins, stacking faults and low-index facets are abundant in as-consolidated nanocrystalline Cu samples. Methodology, results, and analysis of XRD and HREM experiments are presented. 17 refs., 2 figs., 2 tabs.

  14. 2.5D Modeling of TEM Data Applied to Hidrogeological Studies in PARANÁ Basin, Brazil

    NASA Astrophysics Data System (ADS)

    Bortolozo, C. A.; Porsani, J. L.; Santos, F. M.

    2013-12-01

    The transient electromagnetic method (TEM) is used all over the world and has shown great potential in hydrological, hazardous waste site characterization, mineral exploration, general geological mapping, and geophysical reconnaissance. However, the behavior of TEM fields are very complex and is not yet fully understood. Forward modeling is one of the most common and effective methods to understand the physical behavior and significance of the electromagnetics responses of a TEM sounding. Until now, there are a limited number of solutions for the 2D forward problem for TEM. More rare are the descriptions of a three-component response of a 3D source over 2D earth, which is the so-called 2.5D. The 2.5D approach is more realistic than the conventional 2D source previous used, once normally the source cannot be realistic represented for a 2D approximation (normally source are square loops). At present the 2.5D model represents the only way of interpreting TEM data in terms of a complex earth, due to the prohibitive amount of computer time and storage required for a full 3D model. In this work we developed a TEM modeling program for understanding the different responses and how the magnetic and electric fields, produced by loop sources at air-earth interface, behave in different geoelectrical distributions. The models used in the examples are proposed focusing hydrogeological studies, once the main objective of this work is for detecting different kinds of aquifers in Paraná sedimentary basin, in São Paulo State - Brazil. The program was developed in MATLAB, a widespread language very common in the scientific community.

  15. TEM and SHV Genes in Klebsiella pneumoniae Isolated from Cockroaches and Their Antimicrobial Resistance Pattern

    PubMed Central

    Doosti, Abbas; Pourabbas, Mohammad; Arshi, Asghar; Chehelgerdi, Mohammad; Kabiri, Hamidreza

    2014-01-01

    Objectives Klebsiella pneumoniae is a gram-negative rod bacterium, a known cause of community-acquired bacterial pneumonia and is an important hospital-acquired pathogen that causes severe morbidity and mortality. The aim of this study was to identify the TEM and SHV genes in K. pneumoniae isolated from cockroaches obtained from hospitals. Methods In this study, 250 cockroaches were collected from different hospitals in the province of Chaharmahal Va Bakhtiari, which is located in southwest Iran. The samples were examined for the presence of K. pneumoniae by plating onto a combination of culture media, and the antimicrobial susceptibility patterns of isolated K. pneumoniae from samples were evaluated using the disk diffusion test. In addition, from the culture, genomic bacterial DNA was extracted, and sequence-specific targets (TEM and SHV genes) were amplified using the polymerase chain reaction (PCR) method. Results Out of 250 cockroach samples collected from various hospitals, 179 samples (71.60%) were positive for K. pneumoniae. PCR reaction was performed using specific oligonucleotide primers (TEM-F, TEM-R and SHV-F, SHV-R) for the amplification of each gene, and amplified products were visualized on 1% agarose gel electrophoresis. Of all the specimens amplified by PCR in this research, 32 samples (17.87%) were positive for TEM and 15 samples (8.37%) were positive for SHV. Conclusion Detection of TEM and SHV genes using molecular methods and their pattern of antimicrobial resistance can provide useful information about the epidemiology of and risk factors associated with K. pneumoniae infection. PMID:25737824

  16. TEM and Moessbauer Study of Nano Sized Fe{sub 2}MnAl Flakes

    SciTech Connect

    Vinesh, A.; Sudheesh, V. D.; Lakshmi, N.; Venugopalan, K.

    2011-07-15

    Magnetic and structural properties of L21 ordered Fe{sub 2}MnAl Heusler alloy have been studied by X-ray diffraction, Transmission electron microscopy (TEM), Moessbauer spectroscopy and DC magnetization. Structural texturing induced by ball milling is destroyed on heating while Moessbauer and DC magnetization studies show magnetic texturing persists after thermal treatment. TEM shows large distribution in particle size with an average size of 27 nm. Thermal annealing of ball milled sample results L2{sub 1} ordering and the needle shaped particle contributes spin texturing.

  17. SANS and TEM studies of carbide precipitation and creep damage in type 304 stainless steel

    SciTech Connect

    Yoo, M.H.; Ogle, J.C.; Schneibel, J.H.; Swindeman, R.W.

    1984-01-01

    Small-angle neutron scattering (SANS) and transmission electron microscopy (TEM) studies were performed to characterize the carbide (M/sub 23/C/sub 6/) precipitation and creep damage induced in type 304 stainless steel in the primary creep stage. The size distribution of matrix carbides evaluated from SANS analyses was consistent with TEM data, and the expected accelerated kinetics of precipitation under applied stress was confirmed. Additional SANS measurements after the postcreep solution annealing were made in order to differentiate cavities from the carbides. Potential advantages and difficulties associated with characterization of creep-induced cavitation by the SANS techniques are discussed.

  18. Immuno-PET imaging of tumor endothelial marker 8 (TEM8).

    PubMed

    Kuo, Frank; Histed, Stephanie; Xu, Biying; Bhadrasetty, Veerendra; Szajek, Lawrence P; Williams, Mark R; Wong, Karen; Wu, Haitao; Lane, Kelly; Coble, Vincent; Vasalatiy, Olga; Griffiths, Gary L; Paik, Chang H; Elbuluk, Osama; Szot, Christopher; Chaudhary, Amit; St Croix, Brad; Choyke, Peter; Jagoda, Elaine M

    2014-11-01

    Tumor endothelial marker 8 (TEM8) is a cell surface receptor that is highly expressed in a variety of human tumors and promotes tumor angiogenesis and cell growth. Antibodies targeting TEM8 block tumor angiogenesis in a manner distinct from the VEGF receptor pathway. Development of a TEM8 imaging agent could aid in patient selection for specific antiangiogenic therapies and for response monitoring. In these studies, L2, a therapeutic anti-TEM8 monoclonal IgG antibody (L2mAb), was labeled with (89)Zr and evaluated in vitro and in vivo in TEM8 expressing cells and mouse xenografts (NCI-H460, DLD-1) as a potential TEM8 immuno-PET imaging agent. (89)Zr-df-L2mAb was synthesized using a desferioxamine-L2mAb conjugate (df-L2mAb); (125)I-L2mAb was labeled directly. In vitro binding studies were performed using human derived cell lines with high, moderate, and low/undetectable TEM8 expression. (89)Zr-df-L2mAb in vitro autoradiography studies and CD31 IHC staining were performed with cryosections from human tumor xenografts (NCI-H460, DLD-1, MKN-45, U87-MG, T-47D, and A-431). Confirmatory TEM8 Western blots were performed with the same tumor types and cells. (89)Zr-df-L2mAb biodistribution and PET imaging studies were performed in NCI-H460 and DLD-1 xenografts in nude mice. (125)I-L2mAb and (89)Zr-df-L2mAb exhibited specific and high affinity binding to TEM8 that was consistent with TEM8 expression levels. In NCI-H460 and DLD-1 mouse xenografts nontarget tissue uptake of (89)Zr-df-L2mAb was similar; the liver and spleen exhibited the highest uptake at all time points. (89)Zr-L2mAb was highly retained in NCI-H460 tumors with <10% losses from day 1 to day 3 with the highest tumor to muscle ratios (T:M) occurring at day 3. DLD-1 tumors exhibited similar pharmacokinetics, but tumor uptake and T:M ratios were reduced ∼2-fold in comparison to NCI-H460 at all time points. NCI-H460 and DLD-1 tumors were easily visualized in PET imaging studies despite low in vitro TEM8 expression

  19. Effectiveness of Shield Termination Techniques Tested with TEM Cell and Bulk Current Injection

    NASA Technical Reports Server (NTRS)

    Bradley, Arthur T.; Hare, Richard J.

    2009-01-01

    This paper presents experimental results of the effectiveness of various shield termination techniques. Each termination technique is evaluated by two independent noise injection methods; transverse electromagnetic (TEM) cell operated from 3 MHz 400 MHz, and bulk current injection (BCI) operated from 50 kHz 400 MHz. Both single carrier and broadband injection tests were investigated. Recommendations as to how to achieve the best shield transfer impedance (i.e. reduced coupled noise) are made based on the empirical data. Finally, the noise injection techniques themselves are indirectly evaluated by comparing the results obtained from the TEM Cell to those from BCI.

  20. Immuno-PET Imaging of Tumor Endothelial Marker 8 (TEM8)

    PubMed Central

    2015-01-01

    Tumor endothelial marker 8 (TEM8) is a cell surface receptor that is highly expressed in a variety of human tumors and promotes tumor angiogenesis and cell growth. Antibodies targeting TEM8 block tumor angiogenesis in a manner distinct from the VEGF receptor pathway. Development of a TEM8 imaging agent could aid in patient selection for specific antiangiogenic therapies and for response monitoring. In these studies, L2, a therapeutic anti-TEM8 monoclonal IgG antibody (L2mAb), was labeled with 89Zr and evaluated in vitro and in vivo in TEM8 expressing cells and mouse xenografts (NCI-H460, DLD-1) as a potential TEM8 immuno-PET imaging agent. 89Zr-df–L2mAb was synthesized using a desferioxamine–L2mAb conjugate (df–L2mAb); 125I-L2mAb was labeled directly. In vitro binding studies were performed using human derived cell lines with high, moderate, and low/undetectable TEM8 expression. 89Zr-df–L2mAb in vitro autoradiography studies and CD31 IHC staining were performed with cryosections from human tumor xenografts (NCI-H460, DLD-1, MKN-45, U87-MG, T-47D, and A-431). Confirmatory TEM8 Western blots were performed with the same tumor types and cells. 89Zr-df–L2mAb biodistribution and PET imaging studies were performed in NCI-H460 and DLD-1 xenografts in nude mice. 125I-L2mAb and 89Zr-df–L2mAb exhibited specific and high affinity binding to TEM8 that was consistent with TEM8 expression levels. In NCI-H460 and DLD-1 mouse xenografts nontarget tissue uptake of 89Zr-df–L2mAb was similar; the liver and spleen exhibited the highest uptake at all time points. 89Zr-L2mAb was highly retained in NCI-H460 tumors with <10% losses from day 1 to day 3 with the highest tumor to muscle ratios (T:M) occurring at day 3. DLD-1 tumors exhibited similar pharmacokinetics, but tumor uptake and T:M ratios were reduced ∼2-fold in comparison to NCI-H460 at all time points. NCI-H460 and DLD-1 tumors were easily visualized in PET imaging studies despite low in vitro TEM8 expression in

  1. High-Resolution Imaging and Spectroscopy at High Pressure: A Novel Liquid Cell for the TEM

    PubMed Central

    Tanase, Mihaela; Winterstein, Jonathan; Sharma, Renu; Aksyuk, Vladimir; Holland, Glenn; Liddle, J. Alexander

    2016-01-01

    We demonstrate quantitative core-loss electron energy-loss spectroscopy of iron oxide nanoparticles and imaging resolution of Ag nanoparticles in liquid down to 0.24 nm, in both transmission and scanning-transmission modes, in a novel, monolithic liquid cell developed for the transmission electron microscope (TEM). At typical SiN membrane thicknesses of 50 nm the liquid layer thickness has a maximum change of only 30 nm for the entire TEM viewing area of 200 μm × 200 μm. PMID:26650072

  2. On the structural affinity of macromolecules with different biological properties: molecular dynamics simulations of a series of TEM-1 mutants.

    PubMed

    Giampaolo, Alessia Di; Mazza, Fernando; Daidone, Isabella; Amicosante, Gianfranco; Perilli, Mariagrazia; Aschi, Massimiliano

    2013-07-12

    Molecular Dynamics simulations have been carried out in order to provide a molecular rationalization of the biological and thermodynamic differences observed for a class of TEM β-lactamases. In particular we have considered the TEM-1(wt), the single point mutants TEM-40 and TEM-19 representative of IRT and ESBL classes respectively, and TEM-1 mutant M182T, TEM-32 and TEM-20 which differ from the first three for the additional of M182T mutation. Results indicate that most of the thermodynamic, and probably biological behaviour of these systems arise from subtle effects which, starting from the alterations of the local interactions, produce drastic modifications of the conformational space spanned by the enzymes. The present study suggests that systems showing essentially the same secondary and tertiary structure may differentiate their chemical-biological activity essentially (and probably exclusively) on the basis of the thermal fluctuations occurring in their physiological environment. PMID:23770365

  3. Transmission X-ray Diffraction (XRD) Patterns Relevant to the MSL Chemin Amorphous Component: Sulfates And Silicates

    NASA Technical Reports Server (NTRS)

    Morris, R. V.; Rampe, E. B.; Graff, T. G.; Archer, P. D., Jr.; Le, L.; Ming, D. W.; Sutter, B.

    2015-01-01

    The Mars Science Laboratory (MSL) CheMin instrument on the Curiosity rover is a transmission X-ray diffractometer (Co-Kalpha radiation source and a approx.5deg to approx.52deg 2theta range) where the analyzed powder samples are constrained to have discrete particle diameters <150 microns by a sieve. To date, diffraction patterns have been obtained for one basaltic soil (Rocknest (RN)) and four drill fines of coherent rock (John Klein (JK), Cumberland (CB), Windjana (WJ), and Confidence Hills (CH)). The CheMin instrument has detected and quantified the abundance of both primary igneous (e.g., feldspar, olivine, and pyroxene) and secondary (e.g., Ca-sulfates, hematite, akaganeite, and Fe-saponite) minerals. The diffraction patterns of all CheMin samples are also characterized by a broad diffraction band centered near 30deg 2theta and by increasing diffraction intensity (scattering continuum) from approx.15deg to approx.5deg, the 2theta minimum. Both the broad band and the scattering continuum are attributed to the presence of an XRD amorphous component. Estimates of amorphous component abundance, based on the XRD data itself and on mass-balance calculations using APXS data crystalline component chemistry derived from XRD data, martian meteorites, and/or stoichiometry [e.g., 6-9], range from approx.20 wt.% to approx.50 wt.% of bulk sample. The APXSbased calculations show that the amorphous component is rich in volatile elements (esp. SO3) and is not simply primary basaltic glass, which was used as a surrogate to model the broad band in the RN CheMin pattern. For RN, the entire volatile inventory (except minor anhydrite) is assigned to the amorphous component because no volatile-bearing crystalline phases were reported within detection limits [2]. For JK and CB, Fesaponite, basanite, and akaganeite are volatile-bearing crystalline components. Here we report transmission XRD patterns for sulfate and silicate phases relevant to interpretation of MSL-CheMin XRD amorphous

  4. Characterizing the Phyllosilicates and Amorphous Phases Found by MSL Using Laboratory XRD and EGA Measurements of Natural and Synthetic Materials

    NASA Technical Reports Server (NTRS)

    Rampe, Elizabeth B.; Morris, Richard V.; Chipera, Steve; Bish, David L.; Bristow, Thomas; Archer, Paul Douglas; Blake, David; Achilles, Cherie; Ming, Douglas W.; Vaniman, David; Crisp, Joy A.; DesMarais, David J.; Downs, Robert; Farmer, Jack D.; Morookian, John Michael; Morrison, Shaunna; Sarrazin, Philippe; Spanovich, Nicole; Treiman, Allan H.; Yen, Albert S.

    2013-01-01

    The Curiosity Rover landed on the Peace Vallis alluvial fan in Gale crater on August 5, 2012. A primary mission science objective is to search for past habitable environments, and, in particular, to assess the role of past water. Identifying the minerals and mineraloids that result from aqueous alteration at Gale crater is essential for understanding past aqueous processes at the MSL landing site and hence for interpreting the site's potential habitability. X-ray diffraction (XRD) data from the CheMin instrument and evolved gas analyses (EGA) from the SAM instrument have helped the MSL science team identify phases that resulted from aqueous processes: phyllosilicates and amorphous phases were measure in two drill samples (John Klein and Cumberland) obtained from the Sheepbed Member, Yellowknife Bay Fm., which is believed to represent a fluvial-lacustrine environment. A third set of analyses was obtained from scoop samples from the Rocknest sand shadow. Chemical data from the APXS instrument have helped constrain the chemical compositions of these secondary phases and suggest that the phyllosilicate component is Mg-enriched and the amorphous component is Fe-enriched, relatively Si-poor, and S- and H-bearing. To refine the phyllosilicate and amorphous components in the samples measured by MSL, we measured XRD and EGA data for a variety of relevant natural terrestrial phyllosilicates and synthetic mineraloids in laboratory testbeds of the CheMin and SAM instruments. Specifically, Mg-saturated smectites and vermiculites were measured with XRD at low relative humidity to understand the behavior of the 001 reflections under Mars-like conditions. Our laboratory XRD measurements suggest that interlayer cation composition affects the hydration state of swelling clays at low RH and, thus, the 001 peak positions. XRD patterns of synthetic amorphous materials, including allophane, ferrihydrite, and hisingerite were used in full-pattern fitting (FULLPAT) models to help

  5. Time-frequency Analysis on low-resistivity Shielding Layer in TEM Soundings

    NASA Astrophysics Data System (ADS)

    Shi, Xianxin; Wu, Kai

    The transient electromagnetic (TEM) method will be influenced by shielding effect of the low-resistivity overburden layer. By adopting the smooth pseudo Wigner-Ville distribution (SPWD), the responses simulated with a finite-difference time-domain method (FDTD) of D- and G-type models by a 2D line source and H-, A-, K- and Q-type models by a loop source are transformed to the time-frequency (T-F) plane. It is indicated that in low-resistivity, the TEM wave aggregates and will consume more energy, it transmits faster in high-resistivity layers but slower in low-resistivity ones. For A-type models widely in distribution of the North China type coalfield of our country, energy of the TEM field has been almost depleted when arriving at the bottom interface (interfaces of Ordovician limestone and coal series) during the TEM exploration in this area, influence of the low resistive shielding layer shall be taken into full consideration, and relatively longer observing time window shall be selected to ensure the detection depth and high-power instruments shall be adopted to increase the signal-noise ratio during construction design.

  6. Occurrence of Siliceous Impact Melt in Netschaëvo IIE? A FIB-TEM Study

    NASA Astrophysics Data System (ADS)

    Hamann, C.; Van Roosbroek, N.; Greshake, A.; Pittarello, L.; Hecht, L.; Debaille, V.; Wirth, R.; Claeys, Ph.

    2015-07-01

    A silicate inclusion in a sample of the Netschaëvo IIE iron meteorite was studied with FIB-TEM. We present petrographic features indicating that this inclusion is quenched impact melt and suggest that Netschaëvo is an impact melt breccia.

  7. Mistranslation drives the evolution of robustness in TEM-1 β-lactamase

    PubMed Central

    Bratulic, Sinisa; Gerber, Florian; Wagner, Andreas

    2015-01-01

    How biological systems such as proteins achieve robustness to ubiquitous perturbations is a fundamental biological question. Such perturbations include errors that introduce phenotypic mutations into nascent proteins during the translation of mRNA. These errors are remarkably frequent. They are also costly, because they reduce protein stability and help create toxic misfolded proteins. Adaptive evolution might reduce these costs of protein mistranslation by two principal mechanisms. The first increases the accuracy of translation via synonymous “high fidelity” codons at especially sensitive sites. The second increases the robustness of proteins to phenotypic errors via amino acids that increase protein stability. To study how these mechanisms are exploited by populations evolving in the laboratory, we evolved the antibiotic resistance gene TEM-1 in Escherichia coli hosts with either normal or high rates of mistranslation. We analyzed TEM-1 populations that evolved under relaxed and stringent selection for antibiotic resistance by single molecule real-time sequencing. Under relaxed selection, mistranslating populations reduce mistranslation costs by reducing TEM-1 expression. Under stringent selection, they efficiently purge destabilizing amino acid changes. More importantly, they accumulate stabilizing amino acid changes rather than synonymous changes that increase translational accuracy. In the large populations we study, and on short evolutionary timescales, the path of least resistance in TEM-1 evolution consists of reducing the consequences of translation errors rather than the errors themselves. PMID:26392536

  8. A tem study of Y-Ba-Cu-O superconductor material prepared by plasma spraying

    SciTech Connect

    Lu, J.; Qiao, G.W.

    1988-01-01

    A transmission electron microscopy (TEM) study was made on Y-Ba-Cu-O superconductors prepared by plasma spraying which is a useful technique in forming and manufacturing of brittle materials. Amophous region and transitional phases with certain orientation relationship were found between YBa/sub 2/Cu/sub 3/O/sub 7-x/ grains.

  9. Structure and Dynamics of Domains in Ferroelectric Nanostructures. In-situ TEM Studies

    SciTech Connect

    Pan, Xiaoqing

    2015-06-30

    The goal of this project was to explore the structure and dynamic behaviors of ferroelectric domains in ferroelectric thin films and nanostructures by advanced transmission electron microscopy (TEM) techniques in close collaboration with phase field modeling. The experimental techniques used include aberration-corrected sub-Å resolution TEM and in-situ TEM using a novel scanning tunneling microscopy (STM) - TEM holder that allows the direct observation of nucleation and dynamic evolution of ferroelectric domains under applied electric field. Specifically, this project was aimed to (1) to study the roles of static electrical boundary conditions and electrical charge in controlling the equilibrium domain structures of BiFeO3 thin films with controlled substrate constraints, (2) to explore the fundamental mechanisms of ferroelectric domain nucleation, growth, and switching under an applied electric field in both uniform thin films and nanostructures, and to understand the roles of crystal defects such as dislocations and interfaces in these processes, (3) to understand the physics of ferroelectric domain walls and the influence of defects on the electrical switching of ferroelectric domains.

  10. Double aberration-corrected TEM/STEM of tungstated zirconia nanocatalysts for the synthesis of paracetamol

    NASA Astrophysics Data System (ADS)

    Yoshida, K.; Shiju, N. R.; Brown, D. R.; Boyes, E. D.; Gai, P. L.

    2010-07-01

    We report highly active tungstated zirconia nanocatalysts for the synthesis of paracetamol by Beckmann rearrangement of 4-hydroxyacetophenone oxime. Double aberration-corrected (2AC)-TEM/STEM studies were performed in a JEOL 2200FS FEG TEM/STEM at the 1 Angstrom (1 Å = 0.1 nanometer) level. Observations at close to zero defocus were carried out using the AC-TEM as well as AC-STEM including high angle annular dark field (HAADF) imaging, from the same areas of the catalyst crystallites. The studies from the same areas have revealed the location and the nanostructure of the polytungstate species (clusters) and the nanograins of zirconia. The AC (S)TEM was crucial to observe the nanostructure and location of polytungstate clusters on the zirconia grains. Polytungstate clusters as small as 0.5 nm have been identified using the HAADF-STEM. The nanostructures of the catalyst and the W surface density have been correlated with paracetamol reaction studies. The results demonstrate the nature of active sites and high activity of the tungstated zirconia nanocatalyst, which is an environmentally clean alternative to the current homogeneous process.