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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. 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.

  3. 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.

  4. 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.

  5. 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.

  6. Preparation of biocompatible magnetite-carboxymethyl cellulose nanocomposite: Characterization of nanocomposite by FTIR, XRD, FESEM and TEM

    NASA Astrophysics Data System (ADS)

    Habibi, Neda

    2014-10-01

    The preparation and characterization of magnetite-carboxymethyl cellulose nano-composite (M-CMC) material is described. Magnetite nano-particles were synthesized by a modified co-precipitation method using ferrous chloride tetrahydrate and ferric chloride hexahydrate in ammonium hydroxide solution. The M-CMC nano-composite particles were synthesized by embedding the magnetite nanoparticles inside carboxymethyl cellulose (CMC) using a freshly prepared mixture of Fe3O4 with CMC precursor. Morphology, particle size, and structural properties of magnetite-carboxymethyl cellulose nano-composite was accomplished using X-ray powder diffraction (XRD), transmission electron microscopy (TEM), Fourier transformed infrared (FTIR) and field emission scanning electron microscopy (FESEM) analysis. As a result, magnetite nano-particles with an average size of 35 nm were obtained. The biocompatible Fe3O4-carboxymethyl cellulose nano-composite particles obtained from the natural CMC polymers have a potential range of application in biomedical field.

  7. A TEM and XRD Study of (BiS) 1+δ(Nb 1+ɛS 2) n Misfit Layer Structures

    NASA Astrophysics Data System (ADS)

    Otero-Diaz, L. C.; Withers, R. L.; Gomez-Herrero, A.; Welberry, T. R.; Schmid, S.

    1995-02-01

    Monolayer and bilayer lamellar misfit layered chalcogenides within the BiS-NbS 2 system have been synthesized and studied via TEM and XRD. Both BiS and NbS 2 parent substructures are shown to have very close to orthorhombic symmetry in the former case, but definite monoclinic symmetry in the latter. Stacking disorder and its effect upon electron diffraction patterns is investigated via higher order Laue zone (HOLZ) diffraction. In addition to the usual set of reflections for such systems, an additional set of weak, somewhat diffuse satellite reflections (not previously reported before for any other misfit layered chalcogenide) have been observed. Bilayer tubular crystals have also been studied by XRD. A close relationship with the corresponding lamellar bilayer phase is established, and some unusual features of its reciprocal lattice are pointed out.

  8. 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.

  9. 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

  10. Vanga Bhasma and its XRD analysis

    PubMed Central

    Hiremath, Rudramma; Jha, C.B.; Narang, K.K.

    2010-01-01

    Bhasmas are potent Ayurvedic medicaments, biologically active and powerful healing preparations in all aspects. Properly prepared Bhasmas have not reported any serious untoward effects in clinical practice. Vanga Bhasma is an effective Ayurvedic medicine among various Bhasmas which are classically explained and advised specially in genitourinary disorders. XRD peaks of Vanga Bhasma are identified to be as Tindioxide (SnO2) PMID:22557364

  11. Diversity of TEM Mutants in Proteus mirabilis

    PubMed Central

    Bonnet, R.; De Champs, C.; Sirot, D.; Chanal, C.; Labia, R.; Sirot, J.

    1999-01-01

    In a survey of resistance to amoxicillin among clinical isolates of Proteus mirabilis, 10 TEM-type β-lactamases were characterized: (i) the well-known penicillinases TEM-1 and TEM-2, the extended-spectrum β-lactamases (ESBLs) TEM-3 and TEM-24, and the inhibitor-resistant TEM (IRT) TEM-44 and (ii) five novel enzymes, a penicillinase TEM-57 similar to TEM-1, an ESBL TEM-66 similar to TEM-3, and three IRTs, TEM-65, TEM-73, and TEM-74. The penicillinase TEM-57 and the ESBL TEM-66 differed from TEM-1 and TEM-3, respectively, by the amino acid substitution Gly-92→Asp (nucleotide mutation G-477→A). This substitution could have accounted for the decrease in pIs (5.2 for TEM-57 and 6.0 for TEM-66) but did not necessarily affect the intrinsic activities of these enzymes. The IRT TEM-65 was an IRT-1-like IRT (Cys-244) related to TEM-2 (Lys-39). The two other IRTs, TEM-73 and TEM-74, were related to IRT-1 (Cys-244) and IRT-2 (Ser-244), respectively, and harbored the amino acid substitutions Leu-21→Phe and Thr-265→Met. In this study, the ESBLs TEM-66, TEM-24, and TEM-3 were encoded by large (170- to 180-kb) conjugative plasmids that exhibited similar patterns after digestion and hybridization with the TEM and AAC(6′)I probes. The three IRTs TEM-65, TEM-73, and TEM-74 were encoded by plasmids that ranged in size from 42 to 70 kb but for which no transfer was obtained. The characterization of five new plasmid-mediated TEM-type β-lactamases and the first report of TEM-24 in P. mirabilis are evidence of the wide diversity of β-lactamases produced in this species and of its possible role as a β-lactamase-encoding plasmid reservoir. PMID:10543745

  12. 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.

  13. 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.

  14. 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.

  15. TEM-109 (CMT-5), a Natural Complex Mutant of TEM-1 β-Lactamase Combining the Amino Acid Substitutions of TEM-6 and TEM-33 (IRT-5)†

    PubMed Central

    Robin, F.; Delmas, J.; Chanal, C.; Sirot, D.; Sirot, J.; Bonnet, R.

    2005-01-01

    Escherichia coli CF349 exhibited a complex β-lactam resistance phenotype, including resistance to amoxicillin and ticarcillin alone and in combination with clavulanate and to some extended-spectrum cephalosporins. The double-disk synergy test was positive. CF349 harbored an 85-kb conjugative plasmid which encoded a β-lactamase of pI 5.9. The corresponding bla gene was identified by PCR and sequencing as a blaTEM gene. The deduced protein sequence revealed a new complex mutant of TEM-1 β-lactamase designated TEM-109 (CMT-5). TEM-109 contained both the substitutions Glu104Lys and Arg164His of the expanded-spectrum β-lactamase (ESBL) TEM-6 and Met69Leu of the inhibitor-resistant TEM-33 (IRT-5). TEM-109 exhibited hydrolytic activity against ceftazidime similar to that of TEM-6 (kcat, 56 s−1 and 105 s−1, respectively; Km values, 226 and 247 μM, respectively). The 50% inhibitory concentrations of clavulanate and tazobactam (0.13 μM and 0.27 μM, respectively) were 5- to 10-fold higher for TEM-109 than for TEM-6 (0.01 and 0.06 μM, respectively) but were almost 10-fold lower than those for TEM-33. The characterization of this novel CMT, which exhibits a low level of resistance to inhibitors, highlights the emergence of this new ESBL type. PMID:16251281

  16. Evolution of TEM-Type Enzymes: Biochemical and Genetic Characterization of Two New Complex Mutant TEM Enzymes, TEM-151 and TEM-152, from a Single Patient▿ †

    PubMed Central

    Robin, Frédéric; Delmas, Julien; Schweitzer, Cédric; Tournilhac, Olivier; Lesens, Olivier; Chanal, Catherine; Bonnet, Richard

    2007-01-01

    Two clinical isolates of Escherichia coli, CF1179 and CF1295, were isolated from a patient hospitalized in the hematology unit of the University Hospital of Clermont-Ferrand, Clermont-Ferrand, France. They were resistant to penicillin-clavulanate combinations and to ceftazidime. The double-disk synergy test was positive only for isolate CF1179. Molecular comparison of the isolates showed that they were clonally related. E. coli recombinant strains exhibiting the resistance phenotype of the clinical strains were obtained by cloning. The clones corresponding to strains CF1179 and CF1295 produced TEM-type beta-lactamases with pI values of 5.7 and 5.3, respectively. Sequencing analysis revealed two novel blaTEM genes encoding closely related complex mutant TEM enzymes, designated TEM-151 (pI 5.3) and TEM-152 (pI 5.7). These two genes also harbored a new promoter region which presented a 9-bp deletion. The two novel β-lactamases differed from the parental enzyme, TEM-1, by the substitution Arg164His, previously observed in extended-spectrum beta-lactamases (ESBLs), and by the substitutions Met69Val and Asn276Asp, previously observed in the inhibitor-resistant penicillinase TEM-36/IRT-7. They differed by two amino acid substitutions: TEM-152 harbored a Glu240Lys ESBL-type substitution and TEM-151 had an Ala284Gly substitution. Functional analysis of TEM-151 and TEM-152 showed that both enzymes had hydrolytic activity against ceftazidime (kcat, 5 and 16 s−1, respectively). TEM-152 was more resistant than TEM-151 to the inhibitor clavulanic acid (50% inhibitory concentrations, 1 versus 0.17 μM). These results confirm the evolution of TEM-type enzymes toward complex enzymes harboring the two kinds of substitutions which confer an extended spectrum of action against beta-lactam antibiotics and resistance to inhibitors. PMID:17220412

  17. 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.

  18. New TEM Variant (TEM-92) Produced by Proteus mirabilis and Providencia stuartii Isolates

    PubMed Central

    de Champs, Christophe; Monne, Claire; Bonnet, Richard; Sougakoff, Wladimir; Sirot, Danielle; Chanal, Catherine; Sirot, Jacques

    2001-01-01

    The sequences of the blaTEM genes encoding TEM-92 in Proteus mirabilis and Providencia stuartii isolates were determined and were found to be identical. Except for positions 218 (Lys-6) and 512 (Lys-104), the nucleotide sequence of blaTEM-92 was identical to that of blaTEM-20, including the sequence of the promoter region harboring a 135-bp deletion combined with a G-162→T substitution. The deduced amino acid sequence of TEM-92 differed from that of TEM-52 by the presence of a substitution (Gln-6→Lys) in the peptide signal. PMID:11257046

  19. XRD and FTIR crystallinity indices in sound human tooth enamel and synthetic hydroxyapatite.

    PubMed

    Reyes-Gasga, José; Martínez-Piñeiro, Esmeralda L; Rodríguez-Álvarez, Galois; Tiznado-Orozco, Gaby E; García-García, Ramiro; Brès, Etienne F

    2013-12-01

    The crystallinity index (CI) is a measure of the percentage of crystalline material in a given sample and it is also correlated to the degree of order within the crystals. In the literature two ways are reported to measure the CI: X-ray diffraction and infrared spectroscopy. Although the CI determined by these techniques has been adopted in the field of archeology as a structural order measure in the bone with the idea that it can help e.g. in the sequencing of the bones in chronological and/or stratigraphic order, some debate remains about the reliability of the CI values. To investigate similarities and differences between the two techniques, the CI of sound human tooth enamel and synthetic hydroxyapatite (HAP) was measured in this work by X-ray diffraction (XRD) and Fourier Transform Infrared spectroscopy (FTIR), at room temperature and after heat treatment. Although the (CI)XRD index is related to the crystal structure of the samples and the (CI)FTIR index is related to the vibration modes of the molecular bonds, both indices showed similar qualitative behavior for heat-treated samples. At room temperature, the (CI)XRD value indicated that enamel is more crystalline than synthetic HAP, while (CI)FTIR indicated the opposite. Scanning (SEM) and transmission (TEM) images were also used to corroborate the measured CI values.

  20. TEM calibration methods for critical dimension standards

    NASA Astrophysics Data System (ADS)

    Orji, Ndubuisi G.; Dixson, Ronald G.; Garcia-Gutierrez, Domingo I.; Bunday, Benjamin D.; Bishop, Michael; Cresswell, Michael W.; Allen, Richard A.; Allgair, John A.

    2007-03-01

    One of the key challenges in critical dimension (CD) metrology is finding suitable calibration standards. Over the last few years there has been some interest in using features measured with the transmission electron microscope (TEM) as primary standards for linewidth measurements. This is because some modes of TEM can produce lattice-resolved images having scale traceability to the SI (Systeme International d'Unites or International System of Units) definition of length through an atomic lattice constant. As interest in using calibration samples that are closer to the length scales being measured increases, so will the use of these TEM techniques. An area where lattice-traceable images produced by TEM has been used as a primary standard is in critical dimension atomic force microscope (CD-AFM) tip width calibration. Two modes of TEM that produce crystal lattice-traceable images are high resolution transmission electron microscope (HR-TEM) and high angle annular dark field scanning transmission electron microscope (HAADF-STEM). HR-TEM produces lattice-traceable images by interference patterns of the diffracted and transmitted beams rather than the actual atomic columns, while HAADF-STEM produces direct images of the crystal lattice. The difference in how both of these techniques work could cause subtle variations in the way feature edges are defined. In this paper, we present results from width samples measured using HR-TEM and HAADF-STEM. Next we compare the results with measurements taken from the same location by two different CD-AFMs. Both of the CD-AFM instruments used for this work have been calibrated using a single crystal critical dimension reference material (SCCDRM). These standards, developed by the National Institute of Standards and Technology (NIST) and SEMATECH, used HR-TEM for traceable tip-width calibration. Consequently, the present work and the previous SCCDRM work provide a mutual cross-check on the traceability of the width calibration

  1. 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.

  2. 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.

  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. 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

  5. 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...

  6. 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.

  7. 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.

  8. 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.

  9. Porosity investigation of compacted bentonite using XRD profile modeling

    NASA Astrophysics Data System (ADS)

    Holmboe, Michael; Wold, Susanna; Jonsson, Mats

    2012-02-01

    Many countries intend to use compacted bentonite as a barrier in their deep geological repositories for nuclear waste. In order to describe and predict hydraulic conductivity or radionuclide transport through the bentonite barrier, fundamental understanding of the microstructure of compacted bentonite is needed. This study examined the interlayer swelling and overall microstructure of Wyoming Bentonite MX-80 and the corresponding homo-ionic Na + and Ca 2 + forms, using XRD with samples saturated under confined swelling conditions and free swelling conditions. For the samples saturated under confined conditions, the interparticle, or so-called free or external porosity was estimated by comparing the experimental interlayer distances obtained from one-dimensional XRD profile fitting against the maximum interlayer distances possible for the corresponding water content. The results showed that interlayer porosity dominated total porosity, irrespective of water content, and that the interparticle porosity was lower than previously reported in the literature. At compactions relevant for the saturated bentonite barrier (1.4-1.8 g/cm 3), the interparticle porosity was estimated to ≤ 3%.

  10. 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.

  11. 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

  12. Insights into the fine-grained fraction of serpentine mud from the Southern Chamorro seamount (ODP Leg 195): A combined XRD, RFA and TEM-EDS study

    NASA Astrophysics Data System (ADS)

    Lischka, M.; Meschede, M.; Warr, L. N.

    2009-12-01

    Serpentine mud volcanoes in the outer forearc of the Izu-Bonin-Mariana subduction system occur in a restricted zone, 50km - 120 km away from the trench axis [Fryer et al., 1985]. The morphotectonic elements of the forearc are dominated by horst and graben structures, caused by extensional movements and normal fault systems related to seamount subduction [Fryer et al., 2000; Stern and Smooth, 1998]. These faults may provide conduits for the diapiric uprising of low density serpentine, extruding at the seafloor in stratovolcanic like structures. Released fluids from the subducted slab at estimated depths of approximately 30km are considered to hydrate the forearc mantle wedge along those fractures [Benton et al., 2001; Mottl et al., 2003; Rübke et al., 2004]. During the formation of the fault gouge, serpentine-bodies entrained xenoliths and xenocrysts from the surrounding rocks and are exhumed towards the surface [Fryer et al., 1990]. In our investigation we focus on the silty to clay-sized particle fraction of the serpentine mud matrix, drilled during ODP Leg 195 at site 1200E. We analysed the bulk mineral composition with X-ray diffraction methods on random powder samples, supplemented by X-ray fluorescence measurements on 25 samples. To obtain more insights into the mineralogy fabric and microstructure of the samples, electron microscopy and electron dispersive spectroscopy were used to determine the crystal-chemistry and alteration textures. Particular emphasis was given on determining serpentine polymorphs and the nature of other phyllosilicates and their geochemical composition and constraints. Geochemical observation of the secondary mineral phases should allow us to reconstruct the processes linked with the migration of fluids and volatile components during subduction related metamorphism affecting the mantle wedge. Based on the new data we characterize the conditions of alteration products within a subduction factory, related to the diapiric deposition of serpentine mud volcanoes.

  13. 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.

  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. 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

  16. Shells on nanowires detected by analytical TEM

    NASA Astrophysics Data System (ADS)

    Thomas, Jürgen; Gemming, Thomas

    2005-09-01

    Nanostructures in the form of nanowires or filled nanotubes and nanoparticles covered by shells are of great interest in materials science. They allow the creation of new materials with tailored new properties. For the characterisation of these structures and their shells by means of analytical transmission electron microscopy (TEM), especially by energy dispersive X-ray spectroscopy (EDXS), and electron energy loss spectroscopy (EELS), the accurate analysis of linescan intensity profiles is necessary. A mathematical model is described, which is suitable for this analysis. It considers the finite electron beam size, the beam convergence, and the beam broadening within the specimen. It is shown that the beam size influences the measured result of core radius and shell thickness. On the other hand, the influence of the beam broadening within the specimen is negligible. At EELS, the specimen thickness must be smaller than the mean free path for inelastic scattering. Otherwise, artifacts of the signal profile of a nanowire can pretend a nanotube.

  17. 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.

  18. 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.

  19. Biological applications of energy-filtered TEM.

    PubMed

    Saunders, Martin; Shaw, Jeremy A

    2014-01-01

    The techniques of electron energy-loss spectroscopy (EELS) and energy-filtered TEM (EFTEM) are routinely applied in the physical sciences to map the distribution of elements at the nanoscale. EELS can also provide details of the bonding/valence of elements through variations in the fine structure of elemental peaks in the spectrum. While applications of these techniques in biology are less prevalent, their ability to detect both the light elements (e.g., C, N, O, P, S) that form the building blocks of biological systems and heavier elements (e.g., metals) makes them potentially important techniques for investigating local chemical variations in tissues and cells. Successful application of EELS and EFTEM in biology requires both an understanding of the techniques themselves and expertise in specimen preparation. Care must be taken to avoid the diffusion of elements during the preparation process to avoid artifacts in the resulting element maps. The power of the techniques is demonstrated here using tissue from a marine mollusc (chiton). PMID:24357386

  20. Mirrored low-energy channel for the MiniXRD

    NASA Astrophysics Data System (ADS)

    Dutra, E. C.; MacNeil, L. P.; Compton, S. M.; Jacoby, B. A.; Raphaelian, M. L.

    2015-08-01

    X-ray Diodes (XRDs) are currently used for spectroscopic measurements, measuring X-ray flux, and estimating spectral shape of the VUV to soft X-ray spectrum. A niche exists for an inexpensive, robust X-ray diode that can be used for experiments in hostile environments on multiple platforms, including explosively driven experiments that have the potential for destroying the diode during the experiment. A multiple channel stacked filtered array was developed with a small field of view where a wider parallel array could not be used, but filtered channels for energies lower than 1000 eV were too fragile to deploy under normal conditions. To achieve both the robustness and the required low-energy detection ability, we designed a small low-energy mirrored channel with a spectral sensitivity from 30 to 1000 eV. The stacked MiniXRD X-ray diode system design incorporates the mirrored low-energy channel on the front of the stacked filtered channels to allow the system to work within a small field of view. We will present results that demonstrate this is a promising solution for low-energy spectrum measurements.

  1. 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.

  2. 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

  3. 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

  4. In situ TEM of radiation effects in complex ceramics.

    PubMed

    Lian, Jie; Wang, L M; Sun, Kai; Ewing, Rodney C

    2009-03-01

    In situ transmission electron microscopy (TEM) has been extensively applied to study radiation effects in a wide variety of materials, such as metals, ceramics and semiconductors and is an indispensable tool in obtaining a fundamental understanding of energetic beam-matter interactions, damage events, and materials' behavior under intense radiation environments. In this article, in situ TEM observations of radiation effects in complex ceramics (e.g., oxides, silicates, and phosphates) subjected to energetic ion and electron irradiations have been summarized with a focus on irradiation-induced microstructural evolution, changes in microchemistry, and the formation of nanostructures. New results for in situ TEM observation of radiation effects in pyrochlore, A(2)B(2)O(7), and zircon, ZrSiO(4), subjected to multiple beam irradiations are presented, and the effects of simultaneous irradiations of alpha-decay and beta-decay on the microstructural evolution of potential nuclear waste forms are discussed. Furthermore, in situ TEM results of radiation effects in a sodium borosilicate glass subjected to electron-beam exposure are introduced to highlight the important applications of advanced analytical TEM techniques, including Z-contrast imaging, energy filtered TEM (EFTEM), and electron energy loss spectroscopy (EELS), in studying radiation effects in materials microstructural evolution and microchemical changes. By combining ex situ TEM and advanced analytical TEM techniques with in situ TEM observations under energetic beam irradiations, one can obtain invaluable information on the phase stability and response behaviors of materials under a wide range of irradiation conditions.

  5. Characterization of the Novel CMT Enzyme TEM-154 ▿

    PubMed Central

    Robin, Frédéric; Delmas, Julien; Machado, Elisabete; Bouchon, Bernadette; Peixe, Luísa; Bonnet, Richard

    2011-01-01

    TEM-154, identified in Portugal in 2004, associated the substitutions observed in the extended-spectrum β-lactamase (ESBL) TEM-12 and in the inhibitor-resistant penicillinase (IRT) TEM-33. This enzyme exhibited hydrolytic activity against ceftazidime and a low level of resistance to clavulanic acid. Surprisingly, the substitution Met69Leu enhanced the catalytic efficiency of oxyimino β-lactams conferred by the substitution Arg164Ser. Its discovery confirms the dissemination of the complex mutant group of TEM enzymes in European countries. PMID:21173189

  6. 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.

  7. 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

  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. Design, fabrication, and applications of in situ fluid cell TEM.

    PubMed

    Li, Dongsheng; Nielsen, Michael H; De Yoreo, James J

    2013-01-01

    In situ fluid cell TEM is a powerful new tool for understanding dynamic processes during liquid phase chemical reactions, including mineral formation. This technique, which operates in the high vacuum of a TEM chamber, provides information on crystal structure, phase, morphology, size, aggregation/segregation, and crystal growth mechanisms in real time. In situ TEM records both crystal structure and morphology at spatial resolutions down to the atomic level with high temporal resolution of up to 10(-6)s per image, giving it distinct advantages over other in situ techniques such as optical microscopy, AFM, or X-ray scattering or diffraction. This chapter addresses the design, fabrication, and assembly of TEM fluid cells and applications of fluid cell TEM to understanding mechanisms of mineralization.

  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. 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.

  12. 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

  13. 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.

  14. 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.

  15. 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

  16. 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.

  17. 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.

  18. 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.

  19. Zwitterionic polymersomes in an ionic liquid: room temperature TEM characterization.

    PubMed

    Maddikeri, Raghavendra R; Colak, Semra; Gido, Samuel P; Tew, Gregory N

    2011-10-10

    Conventional transmission electron microscopy (TEM) was utilized to characterize vesicles formed by the spontaneous self-assembly of a novel zwitterionic block copolymer in the ionic liquid (2-hydroxyethyl)dimethylammonium methanesulfonate as well as in 0.1 M phosphate buffered saline (PBS). This block copolymer was synthesized via ring-opening metathesis polymerization (ROMP) of a norbornene-based sulfobetaine, followed by its end-functionalization with polystyrene to generate the necessary amphiphilic structure. The ionic liquid enabled the visualization of the vesicles in their swollen state by TEM, demonstrating a new method for improved characterization of polymer vesicles. PMID:21902263

  20. 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.

  1. Direct electron detection for TEM with column parallel CCD

    NASA Astrophysics Data System (ADS)

    Moldovan, Grigore; Jeffery, Ben; Nomerotski, Andrei; Kirkland, Angus

    2009-06-01

    Step improvements in electron detectors are needed for transmission electron microscopes (TEM) to take full advantage of latest developments in electron optics and electron sources. This work presents beam tests performed with column parallel charge-coupled devices (CPCCD) and discusses measured cluster properties. Excellent signal-to-noise ratio is found, demonstrating that CPCCD are well suited for TEM. Large variations in cluster-integrated intensity and size are observed, attributed to the strong scattering of 120-200 keV electrons in silicon. Spatial momentum analysis of clusters reveals strong asymmetry indicating that position resolution could be limited for certain cluster shapes.

  2. 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.

  3. Mineralogical Composition of the Mexican Ordinary Chondrite Type Meteorite: A Raman, Infrared and XRD Study

    NASA Astrophysics Data System (ADS)

    Ostrooumov, M.

    2016-08-01

    The Raman microprobe (RMP), infrared (IR) and XRD analysis have been applied to the examination of mineralogical composition of seven mexican meteorites: Aldama, Cosina, El Pozo, Escalon, Nuevo Mercurio,Pacula, Zapotitlan Salinas.

  4. Investigation of gold-bearing veins using magnetics and TEM

    NASA Astrophysics Data System (ADS)

    Davis, L.; Groom, R.

    2012-12-01

    Gold-bearing fractures have been mined at Charters Towers, Queensland for a century. The ore occurs in quartz-sulfide veins hosted in granitoids. The gold is found in lenses within the veins. The purpose of our work was to determine if geophysical methods could be used to identify and delineate known lode-bearing veins. The study site is around the Warrior Mine immediately south of the town. Two structures are being mined at 100-300 m depth: Warrior and Sons of Freedom. While IP is typically used to locate disseminated sulfides, we used a different approach: we integrated airborne magnetic data with ground TEM data to map the geometries of the gold-bearing fracture zones. TEM is advantageous because it does not involve injection of current into the ground with the uncertainty of current flow patterns in such resistive, fractured rocks. Fixed loop TEM surveying was utilized as this approach is much faster to perform than moving loop surveys. Although TEM is commonly used for mapping layered structures and strong conductors, it is much less used for detecting weak conductors, such as those found in gold exploration, contaminant plumes, or geotechnical applications. Here the fracture zones are highly weathered and wet thus producing weak conductors. Upon mapping the vertical derivative of the RTP magnetic data, many linear anomalies were noted, including over both mined structures. These anomalies all indicate negative susceptibility, as would be expected because the structures are depleted in magnetite with respect to the granitoids. Modeling of the RTP total field and derivatives confirms a negative susceptibility. The RTP data indicate the approximate dip, which agrees with known information. Depth resolution is limited in standard 3D inversions, which utilize orthogonal grids with the normal axis in the vertical direction. In this study, we use a dipping grid which strikes and dips according to known information, and have obtained good results. TEM surveying at

  5. TEM Derivative-Producing Enterobacter aerogenes Strains: Dissemination of a Prevalent Clone

    PubMed Central

    Dumarche, P.; De Champs, C.; Sirot, D.; Chanal, C.; Bonnet, R.; Sirot, J.

    2002-01-01

    TEM-24 (CAZ-6) extended-spectrum β-lactamase (ESBL) was detected in 1988 in Clermont-Ferrand, France, in Klebsiella pneumoniae (blaTEM-24) and Enterobacter aerogenes (blaTEM-24b), and since 1994, a TEM-24-producing E. aerogenes clonal strain has been observed elsewhere in the country. To determine if the spread of this clonal strain was restricted to TEM-24-producing E. aerogenes strains, 84 E. aerogenes strains (non-TEM/SHV-producing strains, TEM-1- or -2-producing strains, and different ESBL-producing strains), isolated from 1988 to 1999 in Clermont-Ferrand (n = 59) and in 11 other French hospitals in 1998 (n = 25), were studied. A clonal strain was found for TEM-24- but also for TEM-3- and TEM-1- or 2-producing isolates. This study shows that there is a clonal strain dependent on acquisition of the TEM-type enzyme (TEM-24 and other TEM types). PMID:11897606

  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. Preparation of zeolites for TEM (Transmission Electron Microscopy) using microtomy

    SciTech Connect

    Csencsits, R.; Gronsky, R.

    1987-12-01

    The application of microtomy to Transmission Electron Microscopy (TEM) specimen preparation of zeolite catalysts is explained. Using a new acrylic resin (LR White) thin sections (less than or equal to60 nm) may be cut with relative ease. Although the details described are specific to catalysts, microtomy and the use of the acrylic resin are applicable to any hard ceramic powder sample. 3 figs.

  8. High-resolution analytical TEM of nanostructured materials.

    PubMed

    Schneider, R

    2002-10-01

    This paper briefly reviews the potential applicability of analytical transmission electron microscopy (TEM) to elucidate both structural and chemical peculiarities of materials at high lateral resolution. Examples of analytical TEM investigations performed by energy-dispersive X-ray spectroscopy (EDXS), electron energy loss spectroscopy (EELS), and energy-filtered TEM (EFTEM) are presented for different materials systems including metals, ceramics, and compound semiconductors. In particular, results are given of imaging the element distribution in the interface region between gamma matrix and gamma' precipitate in the nickel-based superalloy SC16 by energy-filtered TEM. For core-shell structured BaTiO(3) particles the chemical composition and even the chemical bonding were revealed by EELS at a resolution of about 1 nm. A sub-nanometer resolution is demonstrated by energy-selective images of the Ga distribution in the surrounding of (In,Ga)As quantum dots. Moreover, the element distribution in (Al,Ga)As/AlAs multilayers with linear concentration gradients in a range of about 10 nm was investigated by EDXS line-profile analyses and EFTEM. PMID:12397484

  9. High-resolution analytical TEM of nanostructured materials.

    PubMed

    Schneider, R

    2002-10-01

    This paper briefly reviews the potential applicability of analytical transmission electron microscopy (TEM) to elucidate both structural and chemical peculiarities of materials at high lateral resolution. Examples of analytical TEM investigations performed by energy-dispersive X-ray spectroscopy (EDXS), electron energy loss spectroscopy (EELS), and energy-filtered TEM (EFTEM) are presented for different materials systems including metals, ceramics, and compound semiconductors. In particular, results are given of imaging the element distribution in the interface region between gamma matrix and gamma' precipitate in the nickel-based superalloy SC16 by energy-filtered TEM. For core-shell structured BaTiO(3) particles the chemical composition and even the chemical bonding were revealed by EELS at a resolution of about 1 nm. A sub-nanometer resolution is demonstrated by energy-selective images of the Ga distribution in the surrounding of (In,Ga)As quantum dots. Moreover, the element distribution in (Al,Ga)As/AlAs multilayers with linear concentration gradients in a range of about 10 nm was investigated by EDXS line-profile analyses and EFTEM.

  10. 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

  11. 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.

  12. In situ TEM of biological assemblies in liquid.

    PubMed

    Dukes, Madeline J; Gilmore, Brian L; Tanner, Justin R; McDonald, Sarah M; Kelly, Deborah F

    2013-12-30

    Researchers regularly use Transmission Electron Microscopes (TEMs) to examine biological entities and to assess new materials. Here, we describe an additional application for these instruments- viewing viral assemblies in a liquid environment. This exciting and novel method of visualizing biological structures utilizes a recently developed microfluidic-based specimen holder. Our video article demonstrates how to assemble and use a microfluidic holder to image liquid specimens within a TEM. In particular, we use simian rotavirus double-layered particles (DLPs) as our model system. We also describe steps to coat the surface of the liquid chamber with affinity biofilms that tether DLPs to the viewing window. This permits us to image assemblies in a manner that is suitable for 3D structure determination. Thus, we present a first glimpse of subviral particles in a native liquid environment.

  13. In situ TEM of Biological Assemblies in Liquid

    PubMed Central

    McDonald, Sarah M.; Kelly, Deborah F.

    2013-01-01

    Researchers regularly use Transmission Electron Microscopes (TEMs) to examine biological entities and to assess new materials. Here, we describe an additional application for these instruments- viewing viral assemblies in a liquid environment. This exciting and novel method of visualizing biological structures utilizes a recently developed microfluidic-based specimen holder. Our video article demonstrates how to assemble and use a microfluidic holder to image liquid specimens within a TEM. In particular, we use simian rotavirus double-layered particles (DLPs) as our model system. We also describe steps to coat the surface of the liquid chamber with affinity biofilms that tether DLPs to the viewing window. This permits us to image assemblies in a manner that is suitable for 3D structure determination. Thus, we present a first glimpse of subviral particles in a native liquid environment. PMID:24429390

  14. 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).

  15. 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

  16. 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.

  17. 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.

  18. 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

  19. SimulaTEM: multislice simulations for general objects.

    PubMed

    Gómez-Rodríguez, A; Beltrán-Del-Río, L M; Herrera-Becerra, R

    2010-01-01

    In this work we present the program SimulaTEM for the simulation of high resolution micrographs and diffraction patterns. This is a program based on the multislice approach that does not assume a periodic object. It can calculate images from finite objects, from amorphous samples, from crystals, quasicrystals, grain boundaries, nanoparticles or arbitrary objects provided the coordinates of all the atoms can be supplied.

  20. 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.

  1. Aberration-Corrected TEM Imaging of Oxygen Occupancy in YSZ.

    PubMed

    An, Jihwan; Koh, Ai Leen; Park, Joong Sun; Sinclair, Robert; Gür, Turgut M; Prinz, Fritz B

    2013-04-01

    We present atomic-scale imaging of oxygen columns and show quantitative analysis on the occupancy of the columns in yttria-stabilized zirconia (YSZ) using aberration-corrected TEM operated under the negative Cs condition. Also, individual contributions both from oxygen column occupancy and the static displacement of oxygen atoms due to occupancy change to the observed column intensities of TEM images were systematically investigated using HRTEM simulation. We found that oxygen column intensity is governed primarily by column occupancy rather than by static displacement of oxygen atoms. Utilizing the aberration-corrected TEM capability and HRTEM simulation results, we experimentally verified that oxygen vacancies segregate near the single grain boundary of a YSZ bicrystal. The methodology and the high spatial resolution characterization tool employed in the present study provide insights into the distribution of oxygen vacancies in the bulk as well as near grain boundaries and pave the way for further investigation and atomic-scale analysis in other important oxide materials.

  2. 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.

  3. Molecular epidemiology of TEM-3 (CTX-1) beta-lactamase.

    PubMed Central

    Petit, A; Gerbaud, G; Sirot, D; Courvalin, P; Sirot, J

    1990-01-01

    A total of 33 clinical isolates encoding TEM-3 (CTX-1) from four French hospitals were studied. The strains belonged to seven species, Klebsiella pneumoniae (n = 24), Escherichia coli (n = 3), Serratia marcescens (n = 2), Citrobacter freundii (n = 1), Enterobacter aerogenes (n = 1), Enterobacter cloacae (n = 1), and Klebsiella oxytoca (n = 1). All the strains harbored an Inc7 or M self-transferable plasmid with a size of approximately 85 kilobases. The plasmids had closely related EcoRI, HincII, HindIII, and PvuII restriction endonuclease-generated patterns and conferred resistance to all beta-lactams, except cephamycins and imipenem; to tetracycline, because of the presence of the genes blatem-3 and tetC, respectively, as determined by hybridization with specific probes; and to sulfonamide. Depending on the presence or absence and level of expression of the genes aacA4, aadA, and dfrI and of insertion element IS15, four types of plasmids could be distinguished. Plasmid pCFF04, the prototype plasmid encoding TEM-3, was widespread and appeared, by Southern hybridization, as the progenitor of the other types of replicons. The plasmid epidemic responsible for dissemination of TEM-3 in clinical isolates of members of the family Enterobacteriaceae may have originated in S. marcescens since pCFF04 was first detected in this species. Images PMID:2327769

  4. 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.

  5. XRD, SEM and EXAFS investigation of cobalt (II) macro cyclic complexes

    NASA Astrophysics Data System (ADS)

    Mishra, Ashutosh; Ninama, Samrath; Mishra, Niyati

    2012-06-01

    Cobalt (II) complexes were synthesis by chemical rout method. The samples were analyzed by X-ray diffraction (XRD), scanning electron microscopy (SEM) and Extended X-ray absorption fine structure (EXAFS). XRD analysis shows that sample is crystalline in nature and having particle size in the range of few micro meters, SEM is designed for studying of the surfaces of solid objects and EXAFS technique extract the local structure of complexes. The nearest neighboring atom distances commonly known as `bond length' were calculated using different methods and also compared with IFEFFIT method.

  6. 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.

  7. 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

  8. Chemical Species, Micromorphology, and XRD Fingerprint Analysis of Tibetan Medicine Zuotai Containing Mercury

    PubMed Central

    Li, Cen; Yang, Hongxia; Xiao, Yuancan; Zhandui; Sanglao; Wang, Zhang; Ladan, Duojie; Bi, Hongtao

    2016-01-01

    Zuotai (gTso thal) is one of the famous drugs containing mercury in Tibetan medicine. However, little is known about the chemical substance basis of its pharmacodynamics and the intrinsic link of different samples sources so far. Given this, energy dispersive spectrometry of X-ray (EDX), scanning electron microscopy (SEM), atomic force microscopy (AFM), and powder X-ray diffraction (XRD) were used to assay the elements, micromorphology, and phase composition of nine Zuotai samples from different regions, respectively; the XRD fingerprint features of Zuotai were analyzed by multivariate statistical analysis. EDX result shows that Zuotai contains Hg, S, O, Fe, Al, Cu, and other elements. SEM and AFM observations suggest that Zuotai is a kind of ancient nanodrug. Its particles are mainly in the range of 100–800 nm, which commonly further aggregate into 1–30 μm loosely amorphous particles. XRD test shows that β-HgS, S8, and α-HgS are its main phase compositions. XRD fingerprint analysis indicates that the similarity degrees of nine samples are very high, and the results of multivariate statistical analysis are broadly consistent with sample sources. The present research has revealed the physicochemical characteristics of Zuotai, and it would play a positive role in interpreting this mysterious Tibetan drug. PMID:27738409

  9. Making an Asteroid: Effects of Thermal Metamorphism on CO3 Meteorites as Determined by XRD

    NASA Astrophysics Data System (ADS)

    Bonato, E.; King, A. J.; Schofield, P. F.; Lee, M. R.; Russell, S. S.

    2016-08-01

    Investigation of the effects of thermal metamorphism in CO3 meteorites through the characterisation of amorphous silicates present in the matrix. Quantitative phase analyses results for CO 3.0–3.8 meteorites obtained with PSD-XRD will be discussed.

  10. 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.

  11. A new procedure for making TEM specimens of superconductor devices

    SciTech Connect

    Huang, Y.; Merkle, K.L.

    1997-04-01

    A new procedure is developed for making TEM specimens of thin film devices. In this procedure the sample is flatly polished to an overall ion-mill-ready thickness so that any point in the 2-D sample pane can be thinned to an electron-transparent thickness by subsequent ion-milling. Using this procedure, small regions of interest can be easily reached in both cross-section and plan-view samples. This is especially useful in device studies. Applications of this procedure to the study of superconductor devices yield good results. This procedure, using commercially available equipment and relatively cheap materials, is simple and easy to realize.

  12. 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.

  13. EXAFS and XRD Studies with Subpicometer Accuracy: The Case of ReO3

    SciTech Connect

    Purans, Juris; Dalba, Giuseppe; Fornasini, Paolo; Kuzmin, Alexei; De Panfilis, Simone; Rocca, Francesco

    2007-02-02

    EXAFS has been measured on ReO3 from 30 to 600 K; XRD has been contemporarily measured above 300 K. In this way, it has been possible to compare the expansion of the lattice parameter (XRD) and of the bond lengths (EXAFS), measured at the same time. EXAFS was interpreted by the cumulant approach, using ReO3 measured at low temperature as reference. According to our results, ReO3 shows a complicated behavior of thermal expansion: (i) ultra low or negative expansion below 100 K, (ii) moderate positive expansion above 150 K up to 500 K, (iii) negative expansion from 500K. up to the decomposition temperature. The EXAFS parallel and perpendicular MSRD (mean square relative displacements) have been calculated for the 1st and 4th shells. An unexpected result is that the perpendicular MSRD of the first coordination shell has a weak temperature dependence.

  14. 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.

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

    NASA Astrophysics Data System (ADS)

    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.

  16. 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.

  17. (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

  18. 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

  19. [Study on the vibrational spectra and XRD characters of Huanglong jade from Longling County, Yunnan Province].

    PubMed

    Pei, Jing-cheng; Fan, Lu-wei; Xie, Hao

    2014-12-01

    Based on the conventional test methods, the infrared absorption spectrum, Raman spectrum and X-ray diffraction (XRD) were employed to study the characters of the vibration spectrum and mineral composition of Huanglong jade. The testing results show that Huanglong jade shows typical vibrational spectrum characteristics of quartziferous jade. The main infrared absorption bands at 1162, 1076, 800, 779, 691, 530 and 466 cm(-1) were induced by the asymmetric stretching vibration, symmetrical stretching vibration and bending vibration of Si-O-Si separately. Especially the absorption band near 800 cm(-1) is split, which indicates that Huanglong jade has good crystallinity. In Raman spectrum, the main strong vibration bands at 463 and 355 cm(-1) were attributed to bending vibration of Si-O-Si. XRD test confirmed that Quartz is main mineral composition of Huanglong jade and there is a small amount of hematite in red color samples which induced the red color of Huanglong jade. This is the first report on the infrared, Raman and XRD spectra feature of Huanglong jade. It will provide a scientific basis for the identification, naming and other research for huanglong jade.

  20. Matching 4.7-Å XRD spacing in amelogenin nanoribbons and enamel matrix.

    PubMed

    Sanii, B; Martinez-Avila, O; Simpliciano, C; Zuckermann, R N; Habelitz, S

    2014-09-01

    The recent discovery of conditions that induce nanoribbon structures of amelogenin protein in vitro raises questions about their role in enamel formation. Nanoribbons of recombinant human full-length amelogenin (rH174) are about 17 nm wide and self-align into parallel bundles; thus, they could act as templates for crystallization of nanofibrous apatite comprising dental enamel. Here we analyzed the secondary structures of nanoribbon amelogenin by x-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) and tested if the structural motif matches previous data on the organic matrix of enamel. XRD analysis showed that a peak corresponding to 4.7 Å is present in nanoribbons of amelogenin. In addition, FTIR analysis showed that amelogenin in the form of nanoribbons was comprised of β-sheets by up to 75%, while amelogenin nanospheres had predominantly random-coil structure. The observation of a 4.7-Å XRD spacing confirms the presence of β-sheets and illustrates structural parallels between the in vitro assemblies and structural motifs in developing enamel.

  1. Mineralogical composition of the meteorite El Pozo (Mexico): a Raman, infrared and XRD study.

    PubMed

    Ostrooumov, Mikhail; Hernández-Bernal, Maria del Sol

    2011-12-01

    The Raman (RMP), infrared (IR) and XRD analysis have been applied to the examination of mineralogical composition of El Pozo meteorite (an ordinary chondrite L5 type; village Valle of Allende, founded in State of Chihuahua, Mexico: 26°56'N and 105°24'W, 1998). RMP measurements in the range of 100-3500 cm(-1) revealed principal characteristic bands of the major minerals: olivine, two polymorph modifications of pyroxene (OPx and CPx) and plagioclase. Some bands of the minor minerals (hematite and goethite) were also identified. All these minerals were clearly distinguished using IR and XRD techniques. XRD technique has shown the presence of some metallic phases such as kamacite and taenite as well as troilite and chromite. These minerals do not have characteristic Raman spectra because Fe-Ni metals have no active modes for Raman spectroscopy and troilite is a weak Raman scatterer. Raman mapping microspectroscopy was a key part in the investigation of El Pozo meteorite's spatial distribution of the main minerals because these samples are structurally and chemically complex and heterogeneous. The mineral mapping by Raman spectroscopy has provided information for a certain spatial region on which a spatial distribution coexists of the three typical mineral assemblages: olivine; olivine+orthopyroxene; and orthopyroxene.

  2. 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.

  3. 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.

  4. 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.

  5. TSAR modeling of a TEM horn and surrounding structure

    SciTech Connect

    Ng, W.C.; Pennock, S.T.

    1993-11-01

    Modeling of a TEM horn was performed with the TSAR FDTD electromagnetics code. The modeling was done in stages, beginning with the simplest case, the bare antenna itself. Complexity was added in the form of a dielectric lens, an enclosing cylinder, a layer of absorber inside the cylinder, resistive terminations between the horn and cylinder, and a flat plate over all, electrically separate from the cylinder. The final configuration included all of the above, plus a ring of ferrite inside the cylinder, just ahead of the horn. Predictions of the far-field were made at roughly ten degree increments, more closely spaced near boresight, in both vertical and horizontal planes, through the antenna`s centerline. Time histories at those points were evaluated, and from the time histories power densities were calculated. Both time histories and power densities will be presented for the configurations modeled.

  6. Loosely coupled coaxial TEM applicators for deep-heating.

    PubMed

    Harrison, W H; Storm, F K

    1989-01-01

    The development of a coaxial TEM (transverse electromagnetic) deep-heating, non-contacting applicator employing two axially spaced concentric sleeves is described which has electrostatic characteristics and has been named the ESA. Thermal data obtained with the FDA/CDRH elliptic-shaped human torso phantom (with fat overlay) showed nearly uniform heating (+/- 10%) throughout the inner cross-section. Saline tank measurements on a torso cross-section confirmed similar SAR uniformity. Animal experiments with a pig, both with and without blood flow, verified deep-heating and suggested that some preferential central heating occurred. The absence of excessive surface heating indicated that the major portion of the E-field excitation is axially aligned. The non-contacting applicator does not require a water bolus, and experiments showed that moderate patient movement had minor effect on performance.

  7. 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.

  8. 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.

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

    PubMed

    Evans, James E; Browning, Nigel D

    2013-02-01

    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

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

    SciTech Connect

    Evans, James E.; Browning, Nigel D.

    2013-02-18

    Biological processes can occur over a wide range of spatial and temporal scales; from femtoseconds to hours and from angstroms to meters. Although no single experimental method can fully cover this entire phase space, many new biological insights can be expected from a better understanding of the processes that occur on the very fast timescales and very small length scales. In this regard, new instruments that use fast x-ray or electron pulses are now available that are expected to reveal new mechanistic insights for macromolecular protein dynamics. To ensure that any observed conformational change is physiologically relevant and not constrained by three-dimensional crystal packing, it would be preferable for experiments to utilize smaller protein samples such as single particles or two-dimensional crystals that mimic the target protein’s native environment. These samples aren’t typically amenable to x-ray analysis, but transmission electron microscopy has successfully imaged such sample geometries for over 40 years and permits data acquisition using both direct imaging and diffraction modes. While conventional transmission electron microscopes (TEM) have only visualized biological samples with atomic resolution in an arrested or frozen state, the recent development of the dynamic TEM (DTEM) extends electron microscopy capabilities into dynamics. A new 2nd generation DTEM that 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 the micro- and nanosecond timescale. In addition to the enhanced temporal resolution, the DTEM also operates in the pump-probe regime that can permit visualizing reactions propagating in real-time. This article reviews the experimental parameters necessary for coupling DTEM with in situ liquid microscopy to allow direct imaging of protein conformational dynamics in a fully hydrated environment.

  11. 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.

  12. 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).

  13. Evolution of microstructure during the thermal activation of chromium-promoted tin(IV), oxide catalysts: An FT-IR, FT-Raman, XRD, TEM, and XANES/EXAFS study

    SciTech Connect

    Harrison, P.G.; Lloyd, N.C.; Daniell, W.; Bailey, C.; Azelee, W.

    1999-04-01

    The control of noxious emissions resulting either from the combustion of fossil fuels or from other industrial activities is one of the most immediate and compelling problems faced by nearly every country in the world. The chemical transformations occurring during the thermal activation of chromium-promoted tin(IV) oxide catalysts have been investigated by vibrational spectroscopy (FT-IR and FT-Raman), powder X-ray diffraction, transmission electron microscopy, and extended X-ray absorption fine structure and near-edge structure. Three methods of catalyst preparation have been employed: impregnation of SnO{sub 2} using aqueous CrO{sub 3} solutions, impregnation of SnO{sub 2} using aqueous chromium(III) nitrate solutions, and coprecipitation from aqueous solutions containing both tin(IV) and chromium(III) ions. The freshly prepared gel catalyst materials comprise small (ca. 1--2 nm) particles of hydrous tin(IV) oxide, on the surface of which are sorbed chromate(VI) anions, {l_brace}Cr(H{sub 2}O){sub 6}{sup 3+}{r_brace} cations, or polymeric {gamma}-CrOOH depending on the preparative route. In all three cases, however, calcination at 573 K results in the formation of the mixed-valence chromium compound Cr{sub 5}O{sub 12}. At higher calcination temperatures Cr{sub 2}O{sub 3} is formed, which becomes more crystalline the higher the temperature. Concurrently, the size of the tin(IV) oxide particles increases, only slowly initially (ca. {times}2 by 673 K and ca. {times}4 by 873 K), but sintering to very large particles occurs at higher temperatures. No incorporation of chromium into the tin(IV) oxide lattice occurs even at high temperature.

  14. Influence of smectite suspension structure on sheet orientation in dry sediments: XRD and AFM applications.

    PubMed

    Zbik, Marek S; Frost, Ray L

    2010-06-15

    The structure-building phenomena within clay aggregates are governed by forces acting between clay particles. Measurements of such forces are important to understand in order to manipulate the aggregate structure for applications such as dewatering of mineral processing tailings. A parallel particle orientation is required when conducting XRD investigation on the oriented samples and conduct force measurements acting between basal planes of clay mineral platelets using atomic force microscopy (AFM). To investigate how smectite clay platelets were oriented on silicon wafer substrate when dried from suspension range of methods like SEM, XRD and AFM were employed. From these investigations, we conclude that high clay concentrations and larger particle diameters (up to 5 microm) in suspension result in random orientation of platelets in the substrate. The best possible laminar orientation in the clay dry film, represented in the XRD 001/020 intensity ratio of 47 was obtained by drying thin layers from 0.02 wt.% clay suspensions of the natural pH. Conducted AFM investigations show that smectite studied in water based electrolytes show very long-range repulsive forces lower in strength than electrostatic forces from double-layer repulsion. It was suggested that these forces may have structural nature. Smectite surface layers rehydrate in water environment forms surface gel with spongy and cellular texture which cushion approaching AFM probe. This structural effect can be measured in distances larger than 1000 nm from substrate surface and when probe penetrate this gel layer, structural linkages are forming between substrate and clay covered probe. These linkages prevent subsequently smooth detachments of AFM probe on way back when retrieval. This effect of tearing new formed structure apart involves larger adhesion-like forces measured in retrieval. It is also suggested that these effect may be enhanced by the nano-clay particles interaction.

  15. 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

  16. [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

  17. A Raman, infrared and XRD analysis of the instability in volcanic opals from Mexico.

    PubMed

    Ostrooumov, Mikhail

    2007-12-15

    A series of natural volcanic opal samples with the destabilization phenomena from Mexican deposits (states of Queretaro and Jalisco) was investigated by Raman microprobe (RMP), infrared spectrometry and XRD analysis. These techniques show that at low and room temperatures the unaltered transparent opals may be transformed into destabilized white opals, which are a mixture of different polymorphs of tridymite and alpha-cristobalite with various degrees of crystallinity. We found systematic changes in frequencies of both the Raman and the infrared bands, caused by increasing regularities of bond-lengths and bond-angles Si-O-Si groups under the effect of stability. Micro-Raman spectrometry confirms that in the destabilized opal the principal mineral phases are MC (monoclinic ordered)- and MX (incommensurate monoclinic)-tridymites that are characterized by more structural order in comparison with other structural modification of this phase in unaltered opal (POn pseudo-orthorhombic disordered tridymite). XRD investigations show that in the sequence from unaltered to destabilized opal the position of principal maximum (4.30, 4.10 and 2.50 A) shifts towards higher d-spacing. This XRD shifting to higher d-spacing can largely be explained by an increasing amount of tridymite stacking and unresolved superposition of cristobalite and tridymite reflections. The destabilization phenomena in volcanic opals is due to the structural ordering/disordering that is characterized mainly by the formation of the different tridymite polymorphs (MC and MX) in the destabilized opal-CT as well as the decreasing content of molecular water in the structure. PMID:17720618

  18. A Raman, infrared and XRD analysis of the instability in volcanic opals from Mexico.

    PubMed

    Ostrooumov, Mikhail

    2007-12-15

    A series of natural volcanic opal samples with the destabilization phenomena from Mexican deposits (states of Queretaro and Jalisco) was investigated by Raman microprobe (RMP), infrared spectrometry and XRD analysis. These techniques show that at low and room temperatures the unaltered transparent opals may be transformed into destabilized white opals, which are a mixture of different polymorphs of tridymite and alpha-cristobalite with various degrees of crystallinity. We found systematic changes in frequencies of both the Raman and the infrared bands, caused by increasing regularities of bond-lengths and bond-angles Si-O-Si groups under the effect of stability. Micro-Raman spectrometry confirms that in the destabilized opal the principal mineral phases are MC (monoclinic ordered)- and MX (incommensurate monoclinic)-tridymites that are characterized by more structural order in comparison with other structural modification of this phase in unaltered opal (POn pseudo-orthorhombic disordered tridymite). XRD investigations show that in the sequence from unaltered to destabilized opal the position of principal maximum (4.30, 4.10 and 2.50 A) shifts towards higher d-spacing. This XRD shifting to higher d-spacing can largely be explained by an increasing amount of tridymite stacking and unresolved superposition of cristobalite and tridymite reflections. The destabilization phenomena in volcanic opals is due to the structural ordering/disordering that is characterized mainly by the formation of the different tridymite polymorphs (MC and MX) in the destabilized opal-CT as well as the decreasing content of molecular water in the structure.

  19. [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.

  20. 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.

  1. 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

  2. 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

  3. 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.

  4. EXAFS and XRD studies of copper and cobalt complexes of amino acid

    NASA Astrophysics Data System (ADS)

    Mishra, A.; Yadav, A.; Ninama, S.; Trivedi, A.

    2012-05-01

    The present paper deals with the synthesis of transition metal schiff base complexes of Para amino benzoic acid (PABA) by chemical root method. The synthesized metal complexes were characterized by XRD analysis, Extended X-ray absorption fine structure (EXAFS) is a technique that has been used for determining the metal ligand bond length using conventional X-ray source and also by EXAFS analysis using IFEFFIT programming. Bond lengths determined from these data analysis methods are compared with the bond lengths obtained from LSS, Levy's and Lytle's methods. All the complexes show the crystalline simple cubic structure. Bond lengths of the complexes are in good agreement obtained by theoretical and experimental methods.

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

    NASA Astrophysics Data System (ADS)

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

    2014-02-01

    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.

  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 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

  8. 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.

  9. 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.

  10. 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.

  11. [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.

  12. 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.

  13. Using Simultaneous SHG and XRD Capabilities to Examine Phase Transitions of HMX and TATB

    SciTech Connect

    Saw, C K; Zaug, J; Farber, D; Ruddle, C

    2001-06-19

    Simultaneous SHG (second harmonic generation) and XRD (x-ray diffraction) capabilities have been developed at SSRL (Stanford Synchrotron Radiation laboratory) to examine the phase behavior of energetic materials, for example, HMX (octahydro- 1,3,5,7-tetranitro- 1,3,5,7-tetrmcine) and TATB (1,3,5-triamino-2,4,6 trinitrobenzene). This unique capability provides information on the evolution at the molecular level (centro and non-centrosymmetric) on material stability, phase transformation or decomposition reactions, which are important to continue refinement of computational predictions of material properties. This paper reports x-ray diffraction experiments on both HMX and TATB with increasing temperature and on simultaneous SHG and XRD experiments at fixed temperature. Our results indicate that, for HMX, the {beta} to {delta} transformation occurs over a range of temperature which do not correlate to the previously reported fast rise in SHG signal close to 17OOC as a phase transformation. No phase transition is observed for TATB, even though, previous paper shows an increase in the SHG signal.

  14. 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.

  15. Effect of relative humidity constraint on the metal exchanged montmorillonite performance: An XRD profile modeling approach

    NASA Astrophysics Data System (ADS)

    Oueslati, Walid; Ben Rhaiem, Hafsia; Ben Haj Amara, Abdesslem

    2012-11-01

    This work aims at examining the effect of an applied hydrous strain on the cation exchange process of a dioctahedral smectite by quantitative XRD analysis. The hydrous constraint is created by a continuous, in situ, hydration-dehydration cycles using variation of %RH (relative humidity) rate. In order to examine the effect of the retained materials stress on the cation exchange capacity of the host materials, the starting, the intermediate and the final stressed samples are deposed in contact with saturated Cd(II), Co(II), Zn(II) and Ni(II) chloride solutions. To characterize structural changes, an XRD profile modeling approach is used. This investigation allowed us to determine parameters related to the nature, abundance, size, position, organization of exchangeable cation and water molecule in the interlamellar space, along the c* axis. Qualitatively, the hydration behavior is affected by the number of hydration-dehydration cycle, and an interstratified hydration phases due probably to a new organization of the interlamellar space content is observed. Quantitatively, the theoretical mixed layer structure (MLS) suggests the coexistence of more one "crystallite" specie which are saturated by more than one exchangeable cations indicating a partial saturation of all exchangeable sites. Using optimum structural parameter values, deduced from the theoritecals models, some equations which described the evolution of exchangeable cation amount versus the applied hydrous strain were derived.

  16. 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.

  17. 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.

  18. Development of a CCD array detector for combined XRD\\XRF applications

    NASA Astrophysics Data System (ADS)

    Intisar, Amir; Hutchinson, Ian; Holland, Andrew; Simpson, David; Pool, Peter

    2008-07-01

    This project is based on the design and testing of a CCD (charge coupled device) based detector to be used for the simultaneous collection of x-ray diffraction (XRD) and x-ray fluorescence (XRF) data from powdered rock samples. The detector designed for this project uses four e2v technologies CCD 30-11 (FI, AIMO) devices tiled in a curved geometry to allow the centre of each of the four CCDs to be exactly 120 mm from the sample. The CCDs are operated in single photon counting mode which allows the detector to simultaneously determine the spatial position of diffracted x-rays as well as resolve the energy of characteristic x-rays fluoresced from the sample. Energy discrimination is then used to reveal the XRD data and radial integration is performed on the four CCD images to extract the "2θ vs. intensity" spectrum. The project also involves the use of a high brightness x-ray micro-source from Bede Scientific Instruments, used to deliver a focused beam of low divergent x-rays to the sample. Collimation and monochromation are also introduced into the system to produce a 93% monochromatic beam of CuKθ x-rays, delivered to the powder sample through a 50 µm spot. Details into the design of the CCD array are discussed as well as results presented from various samples.

  19. Upgrades to the XRD1 beamline optics and endstation at the LNLS

    NASA Astrophysics Data System (ADS)

    Canova, H.; Fontoura, A.; Neuenschwander, R. T.; Diaz, B.; Rodella, C. B.

    2014-03-01

    XRD1 was the first X-ray diffraction beamline to be built at the LNLS and after approximately 12 years of operation it was substantially updated to improve beam stability, increase the reliability of the monochromator movement as well as provide an experimental hutch that would meet the demands of users. The improvements included the construction of an independent concrete slab below the mirror and monochromator to minimize the vibrations originating from the floor. In addition, the installation of new monochromator mechanisms as well as the replacement of the two Si(111) crystals were performed in order to attain higher precision, stability and reproducibility during operation. Moreover, the diffractometer was replaced by a 3-circle heavy duty diffractometer from Newport to collect XRD patterns primarily in capillary geometry. A robotic arm was installed for fast and automated replacement of samples as well as to secure a cryojet or a hot air blower in front of the sample during measurements. In addition, a housing equipped with 24 Mythen detectors was installed at the beamline allowing for extremely fast data acquisition. Another upgrade was the integration of motors and control systems from PXI National Instruments and Galil controllers with Phytron. These systems are crucial for the next upgrade that is underway at the beamline: enabling remote access for users to collect their measurements without the need to travel to the LNLS.

  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. 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.

  2. 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.

  3. Development of "oligotyping" for characterization and molecular epidemiology of TEM beta-lactamases in members of the family Enterobacteriaceae.

    PubMed Central

    Mabilat, C; Courvalin, P

    1990-01-01

    Based on the DNA sequences of blaTEM-1 and blaTEM-2, which encode parental penicillinases TEM-1 and TEM-2, respectively, and blaTEM-3, blaTEM-4, blaTEM-5, blaTEM-6, and blaTEM-7, which encode extended-spectrum beta-lactamases, we designed heptadecanucleotides to discriminate point mutations in five loci. Determination of the hybridization profiles by colony hybridization with this selection of probes, termed "oligotyping," allowed characterization of the TEM variants present in 265 clinical isolates of the family Enterobacteriaceae that exhibit synergism between a penicillinase inhibitor and broad-spectrum cephaslosporins. Among the 222 strains harboring TEM enzymes, Klebsiella pneumoniae (48%) and Escherichia coli (21%) were predominant, and TEM-3 was the most common enzyme (60%). Penicillinases TEM-1 and TEM-2 were detected alone (15 and 1%, respectively), combined (1%), or associated with another TEM beta-lactamase (17 and 6%, respectively). Fourteen variants, including seven new enzymes, were detected. One, TEM-13, was a new penicillinase with the same isoelectric point and substrate range as TEM-2 but differed by a single amino acid substitution, whereas the others, TEM-14 to TEM-19, were extended-spectrum beta-lactamases that consisted of novel combinations of known amino acid substitutions. Different TEM variants were found to coexist within the same cells. A patient could harbor two or three different strains that encoded the same enzyme or two indistinguishable isolates that produced distinct TEM beta-lactamases. PMID:2073111

  4. 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.

  5. Inhibitor-resistant TEM (IRT) beta-lactamases with different substitutions at position 244.

    PubMed Central

    Bret, L; Chaibi, E B; Chanal-Claris, C; Sirot, D; Labia, R; Sirot, J

    1997-01-01

    A novel inhibitor-resistant TEM (IRT) beta-lactamase was detected in an Escherichia coli isolate resistant to amoxicillin-clavulanate and susceptible to cephalothin. The substrate and inhibitor profiles of this beta-lactamase were similar to those of IRT-1 and IRT-2. The novel IRT's bla gene was sequenced, and the deduced amino acid sequence showed the amino acid replacement Arg for His-244 of the TEM-1 sequence. Substitutions for Arg-244 have been reported in three TEM-1 mutants: IRT-1 (which corresponds to TEM-31) (Cys), IRT-2/TEM-30 (Ser), and TEM-41 (Thr). We designated this novel beta-lactamase, which corresponds to TEM-51, IRT-15. PMID:9371365

  6. 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.

  7. SHI Induced Modifications in CdS/CuInSe2 Thin Film: XRD Analysis

    NASA Astrophysics Data System (ADS)

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

    2011-07-01

    CuInSe2 (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 Au9+ swift heavy ion (SHI) at 5×1011 and 5×1012 ions/cm2 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 (Au9+) ions in CuInSe2 thin films.

  8. 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.

  9. 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.

  10. 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.

  11. 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.

  12. 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.

  13. 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.

  14. XRD and VCD: a marriage of love or convenience? Honeymoon around a cyclic urea derivative.

    PubMed

    Gherase, Dragos; Naubron, Jean-Valère; Roussel, Christian; Giorgi, Michel

    2012-07-01

    The structures and absolute configurations of the enantiomers (3aR,8aR)-2,2-dimethyl-4,4,8,8-tetraphenyl-4,5,6,7,8,8a-hexahydro-3aH-1,3-dioxolo[4,5-e][1,3]diazepin-6-one 0.33-hydrate, C(32)H(30)N(2)O(3)·0.33H(2)O, (Ia), and (3aS,8aS)-2,2-dimethyl-4,4,8,8-tetraphenyl-4,5,6,7,8,8a-hexahydro-3aH-1,3-dioxolo[4,5-e][1,3]diazepin-6-one 0.39-hydrate, C(32)H(30)N(2)O(3)·0.39H(2)O, (Ib), have been elucidated unambiguously using the complementary power of single-crystal X-ray diffraction (XRD) and vibrational circular dichroism (VCD). The enantiomers crystallize in the Sohncke space group P2(1)2(1)2 and pack as dimers stabilized by two symmetric hydrogen bonds involving one amide group each of the cyclic urea moiety. This double interaction is capped by a water molecule that partially occupies a site lying on the twofold axis and forms an uncommon hydrogen bond between the two monomers. A comparison between the solid-state VCD characterizations and the Bayesian statistics on Bijvoet differences determined from the XRD measurements reveals a tendency towards the correct determination of the absolute configuration by this latter method.

  15. 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

  16. Thermal behavior of polyhalite: a high-temperature synchrotron XRD study

    NASA Astrophysics Data System (ADS)

    Xu, Hongwu; Guo, Xiaofeng; Bai, Jianming

    2016-09-01

    As an accessory mineral in marine evaporites, polyhalite, K2MgCa2(SO4)4·2H2O, coexists with halite (NaCl) in salt formations, which have been considered as potential repositories for permanent storage of high-level nuclear wastes. However, because of the heat generated by radioactive decays in the wastes, polyhalite may dehydrate, and the released water will dissolve its neighboring salt, potentially affecting the repository integrity. Thus, studying the thermal behavior of polyhalite is important. In this work, a polyhalite sample containing a small amount of halite was collected from the Salado formation at the WIPP site in Carlsbad, New Mexico. To determine its thermal behavior, in situ high-temperature synchrotron X-ray diffraction was conducted from room temperature to 1066 K with the sample powders sealed in a silica-glass capillary. At about 506 K, polyhalite started to decompose into water vapor, anhydrite (CaSO4) and two langbeinite-type phases, K2Ca x Mg2-x (SO4)3, with different Ca/Mg ratios. XRD peaks of the minor halite disappeared, presumably due to its dissolution by water vapor. With further increasing temperature, the two langbeinite solid solution phases displayed complex variations in crystallinity, composition and their molar ratio and then were combined into the single-phase triple salt, K2CaMg(SO4)3, at ~919 K. Rietveld analyses of the XRD data allowed determination of structural parameters of polyhalite and its decomposed anhydrite and langbeinite phases as a function of temperature. From the results, the thermal expansion coefficients of these phases have been derived, and the structural mechanisms of their thermal behavior been discussed.

  17. 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.

  18. Reduction of mixed Mn-Zr oxides: in situ XPS and XRD studies.

    PubMed

    Bulavchenko, O A; Vinokurov, Z S; Afonasenko, T N; Tsyrul'nikov, P G; Tsybulya, S V; Saraev, A A; Kaichev, V V

    2015-09-21

    A series of mixed Mn-Zr oxides with different molar ratios Mn/Zr (0.1-9) have been prepared by coprecipitation of manganese and zirconium nitrates and characterized by X-ray diffraction (XRD) and BET methods. It has been found that at concentrations of Mn below 30 at%, the samples are single-phase solid solutions (MnxZr1-xO2-δ) based on a ZrO2 structure. X-ray photoelectron spectroscopy (XPS) measurements showed that manganese in these solutions exists mainly in the Mn(4+) state on the surface. An increase in Mn content mostly leads to an increase in the number of Mn cations in the structure of solid solutions; however, a part of the manganese cations form Mn2O3 and Mn3O4 in the crystalline and amorphous states. The reduction of these oxides with hydrogen was studied by a temperature-programmed reduction technique, in situ XRD, and near ambient pressure XPS in the temperature range from 100 to 650 °C. It was shown that the reduction of the solid solutions MnxZr1-xO2-δ proceeds via two stages. During the first stage, at temperatures between 100 and 500 °C, the Mn cations incorporated into the solid solutions MnxZr1-xO2-δ undergo partial reduction. During the second stage, at temperatures between 500 and 700 °C, Mn cations segregate on the surface of the solid solution. In the samples with more than 30 at% Mn, the reduction of manganese oxides was observed: Mn2O3 → Mn3O4 → MnO.

  19. 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

  20. 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

  1. 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

  2. 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.

  3. 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

  4. 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.

  5. 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

  6. 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

  7. Data from the Mars Science Laboratory CheMin XRD/XRF instrument

    NASA Astrophysics Data System (ADS)

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

    2013-04-01

    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 (~An50), forsteritic olivine (~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 ~27° 2θ (Co Kα) and may include volcanic glass, impact glass, and poorly crystalline phases including iron oxyhydroxides; a rise at lower 2θ 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 <150 µm, and delivered to

  8. 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

  9. 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.

  10. 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.

  11. 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.

  12. 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.

  13. 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.

  14. 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.

  15. 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.

  16. 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)

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

    NASA Astrophysics Data System (ADS)

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

    2013-03-01

    We present the results of x-ray diffraction and x-ray absorption spectroscopy experiments in CuAlO2 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 AlO6 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.

  18. 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

  19. IR and XRD Study of the Tribochemical Reactions of Copper Sulfate with Alkali Halides

    NASA Astrophysics Data System (ADS)

    Fernández, J.; González, E.; de Oñate, J.; López, R.; Navarro, E.

    1993-12-01

    Tribochemical reactions of CuSO 4 · 5H 2O and CuSO 4 during milling with KCl, KBr, and KI have been studied by IR and XRD techniques. The reactions are rather similar for the hydrated and anhydrous salts, but proceed faster with the former. With KCl, the reaction leads directly to CuK 2SO 4Cl 2 also known as the mineral chlorothionite. With KBr, the mixed salts CuK 2(SO 4) 2 · 2H 2O and CuK 2 (SO 4) 2 · 6H 2O are first obtained which transform to a new compound upon further milling, that we postulate as CuK 2SO 4Br 2. With KI, there is a fast reaction to a mixture of CuK 2(SO 4) 2 · 6H 2O, γ-CuI, and I 2, later proceeding to K 2SO 4, γ-CuI, and I 2.

  20. 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

  1. 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.

  2. 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

  3. 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

  4. 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.

  5. Towards an integrative structural biology approach: combining Cryo-TEM, X-ray crystallography, and NMR.

    PubMed

    Lengyel, Jeffrey; Hnath, Eric; Storms, Marc; Wohlfarth, Thomas

    2014-09-01

    Cryo-transmission electron microscopy (Cryo-TEM) and particularly single particle analysis is rapidly becoming the premier method for determining the three-dimensional structure of protein complexes, and viruses. In the last several years there have been dramatic technological improvements in Cryo-TEM, such as advancements in automation and use of improved detectors, as well as improved image processing techniques. While Cryo-TEM was once thought of as a low resolution structural technique, the method is currently capable of generating nearly atomic resolution structures on a routine basis. Moreover, the combination of Cryo-TEM and other methods such as X-ray crystallography, nuclear magnetic resonance spectroscopy, and molecular dynamics modeling are allowing researchers to address scientific questions previously thought intractable. Future technological developments are widely believed to further enhance the method and it is not inconceivable that Cryo-TEM could become as routine as X-ray crystallography for protein structure determination.

  6. Virulence Factors and TEM-Type β-Lactamases Produced by Two Isolates of an Epidemic Klebsiella pneumoniae Strain

    PubMed Central

    Hennequin, Claire; Gniadkowski, Marek; Beyrouthy, Racha; Empel, Joanna; Gibold, Lucie; Bonnet, Richard

    2012-01-01

    Two Klebsiella pneumoniae isolates of the same strain, identified in Poland, produced either TEM-47 or TEM-68, which differed by the Arg275Leu substitution. They harbored a few virulence factors, including an iron-chelating factor and capsule overproduction, suggesting that these factors were sufficient to enhance their nosocomial potency. TEM-68 and TEM-47 had similar enzymatic activities, but TEM-68 was less susceptible to inhibitors than TEM-47. These results confirm the role of the Arg275Leu substitution in the evolution of TEM enzymes. PMID:22106220

  7. 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

  8. 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.

  9. 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.

  10. 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.

  11. 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.

  12. [Gel derived bioceramics as a bone substitute--in vivo study. II. Studies with SEM/EDAX, FTIR, XRD].

    PubMed

    Niedzielski, Kryspin; Łaczka, Maria; Cholewa-Kowalska, Katarzyna; Synder, Marek

    2002-01-01

    A study based on SEM, EDAX, Fourier Transform Infrared Spectroscopy (FTIR), X-ray diffraction (XRD) methods was performed. This initial study allowed us to conclude that the analyzed ceramic material S2 is a good bone substitute for filling bone defects.

  13. 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.

  14. A joint TEM-HLEM geophysical approach to borehole sitting in deeply weathered granitic terrains.

    PubMed

    Meju, M A; Fontes, S L; Ulugergerli, E U; La Terra, E F; Germano, C R; Carvalho, R M

    2001-01-01

    The accurate location of aquiferous fracture zones in granite beneath a > 50 m thick weathered mantle in semi-arid regions is a major hydrogeological problem. It is expected that the zone of intensive fracturing will be more susceptible to weathering and thus be characterized by the thickest development of saprolite, a good electrically conductive target for deep-probing electromagnetic systems. The single-loop transient electromagnetic (TEM) technique is well known to have the capability for detecting concealed steep mineralized targets in mining environments and can be adapted to this hydrogeological problem. We propose that combining the conventional frequency-domain horizontal-loop electromagnetic (HLEM) and single-loop TEM is an effective practical approach to locating concealed aquiferous fracture zones. In the supporting case studies presented here, we deployed multifrequency HLEM profiling (with 50 m transmitter-receiver separation) and TEM soundings with contiguous 10 or 20 m sided loops along the survey lines in a granitic terrain affected by deep (> 50 m) weathering in northeast Brazil. A somewhat layered structure consisting of resistive hardpan/leached zone, conductive saprolite, and resistive basement is identifiable in the typical TEM depth sounding data. We obtained coincident HLEM and TEM anomalies at all the sites, enabling a relatively straightforward selection of potential drilling positions. Simple resistivity-depth transformation of the TEM data was done for each site, yielding an approximate section from which drilling depths were estimated. All of the boreholes located were successful. Although our results appear to indicate that the single-loop TEM method could be used independently for borehole sitting in deeply weathered granitic terrains and that the weathering profile over granite can be mapped using TEM depth soundings of appropriate observational bandwidth, we recommend a joint electromagnetic approach for optimal well sitting.

  15. 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

  16. 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.

  17. 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.

  18. 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.

  19. 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.

  20. TEM-72, a new extended-spectrum beta-lactamase detected in Proteus mirabilis and Morganella morganii in Italy.

    PubMed

    Perilli, M; Segatore, B; de Massis, M R; Riccio, M L; Bianchi, C; Zollo, A; Rossolini, G M; Amicosante, G

    2000-09-01

    A new natural TEM-2 derivative, named TEM-72, was identified in a Proteus mirabilis strain and in a Morganella morganii strain isolated in Italy in 1999. Compared to TEM-1, TEM-72 contains the following amino acid substitutions: Q39K, M182T, G238S, and E240K. Kinetic analysis showed that TEM-72 exhibits an extended-spectrum activity, including activity against oxyimino-cephalosporins and aztreonam. Expression of bla(TEM-72) in Escherichia coli was capable of decreasing the host susceptibility to the above drugs.

  1. Identification of TEM-135 β-lactamase in Neisseria gonorrhoeae strains carrying African and Toronto plasmids in Argentina.

    PubMed

    Gianecini, R; Oviedo, C; Littvik, A; Mendez, E; Piccoli, L; Montibello, S; Galarza, P

    2015-01-01

    One hundred forty-three penicillinase-producing Neisseria gonorrhoeae (PPNG) isolates obtained in Argentina from 2008 and 2012 were examined to detect blaTEM-135 genes and to investigate plasmid profiles and multiantigen sequence types. Forty-two PPNG isolates were found to carry TEM-135, and two contained a new TEM derivative characterized as TEM-220. The blaTEM-135 allele was carried by the Toronto/Rio and African plasmids. Molecular epidemiology revealed that two blaTEM-135 isolates were related to previously described isolates from Thailand and China, indicating a common evolutionary origin.

  2. Identification of TEM-135 β-Lactamase in Neisseria gonorrhoeae Strains Carrying African and Toronto Plasmids in Argentina

    PubMed Central

    Gianecini, R.; Oviedo, C.; Littvik, A.; Mendez, E.; Piccoli, L.; Montibello, S.

    2014-01-01

    One hundred forty-three penicillinase-producing Neisseria gonorrhoeae (PPNG) isolates obtained in Argentina from 2008 and 2012 were examined to detect blaTEM-135 genes and to investigate plasmid profiles and multiantigen sequence types. Forty-two PPNG isolates were found to carry TEM-135, and two contained a new TEM derivative characterized as TEM-220. The blaTEM-135 allele was carried by the Toronto/Rio and African plasmids. Molecular epidemiology revealed that two blaTEM-135 isolates were related to previously described isolates from Thailand and China, indicating a common evolutionary origin. PMID:25367903

  3. 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.

  4. VES/TEM 1D joint inversion by using Controlled Random Search (CRS) algorithm

    NASA Astrophysics Data System (ADS)

    Bortolozo, Cassiano Antonio; Porsani, Jorge Luís; Santos, Fernando Acácio Monteiro dos; Almeida, Emerson Rodrigo

    2015-01-01

    Electrical (DC) and Transient Electromagnetic (TEM) soundings are used in a great number of environmental, hydrological, and mining exploration studies. Usually, data interpretation is accomplished by individual 1D models resulting often in ambiguous models. This fact can be explained by the way as the two different methodologies sample the medium beneath surface. Vertical Electrical Sounding (VES) is good in marking resistive structures, while Transient Electromagnetic sounding (TEM) is very sensitive to conductive structures. Another difference is VES is better to detect shallow structures, while TEM soundings can reach deeper layers. A Matlab program for 1D joint inversion of VES and TEM soundings was developed aiming at exploring the best of both methods. The program uses CRS - Controlled Random Search - algorithm for both single and 1D joint inversions. Usually inversion programs use Marquadt type algorithms but for electrical and electromagnetic methods, these algorithms may find a local minimum or not converge. Initially, the algorithm was tested with synthetic data, and then it was used to invert experimental data from two places in Paraná sedimentary basin (Bebedouro and Pirassununga cities), both located in São Paulo State, Brazil. Geoelectric model obtained from VES and TEM data 1D joint inversion is similar to the real geological condition, and ambiguities were minimized. Results with synthetic and real data show that 1D VES/TEM joint inversion better recovers simulated models and shows a great potential in geological studies, especially in hydrogeological studies.

  5. TEM-1-encoding small plasmids impose dissimilar fitness costs on Haemophilus influenzae and Haemophilus parainfluenzae.

    PubMed

    Søndergaard, Annette; Lund, Marianne; Nørskov-Lauritsen, Niels

    2015-12-01

    Only two beta-lactamases, TEM-1 and ROB-1, have been observed in Haemophilus influenzae, while four different TEM but no ROB enzymes have been found in Haemophilus parainfluenzae. In order to investigate the mechanisms behind the dissemination of small beta-lactamase-encoding plasmids in H. influenzae and H. parainfluenzae, we assessed the fitness cost of three TEM-1- (pPN223, pA1209, pA1606), one TEM-15- (pSF3) and one ROB-1-bearing (pB1000) plasmid when expressed in either bacterial species. All plasmids were stable in H. influenzae and H. parainfluenzae except pB1000, which showed on average (sample mean) 76% curing in H. parainfluenzae after 5  days of subculture. Competition assays between isogenic strains with and without plasmid showed no competitive disadvantage of pPN223 and pA1606 in H. influenzae, or of pA1209 in H. parainfluenzae. In contrast, pSF3 and pB1000 were associated with significant competitive disadvantages in both species. Some of the competitive disadvantages may be related to differences in plasmid copy number and mRNA expression of the beta-lactamase genes, as revealed by quantitative PCR analysis. In conclusion, plasmids encoding TEM beta-lactamases isolated from H. influenzae and H. parainfluenzae can be stably transferred between species. The fast curing of pB1000 in H. parainfluenzae observed in this study correlates to the fact that ROB-1 has never been reported for this species. TEM-1-encoding plasmids are associated with the lowest level of fitness cost, but different TEM-1 plasmids confer different levels of fitness cost on the two hosts.

  6. 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.

  7. 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.

  8. 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.

  9. Some critical aspects of FT-IR, TGA, powder XRD, EDAX and SEM studies of calcium oxalate urinary calculi.

    PubMed

    Joshi, Vimal S; Vasant, Sonal R; Bhatt, J G; Joshi, Mihir J

    2014-06-01

    Urinary calculi constitute one of the oldest afflictions of humans as well as animals, which are occurring globally. The calculi vary in shape, size and composition, which influence their clinical course. They are usually of the mixed-type with varying percentages of the ingredients. In medical management of urinary calculi, either the nature of calculi is to be known or the exact composition of calculi is required. In the present study, two selected calculi were recovered after surgery from two different patients for detailed examination and investigated by using Fourier-Transform infrared spectroscopy (FT-IR), thermo-gravimetric analysis (TGA), powder X-ray diffraction (XRD), scanning electron microscopy and energy dispersive analysis of X-rays (EDAX) techniques. The study demonstrated that the nature of urinary calculi and presence of major phase in mixed calculi could be identified by FT-IR, TGA and powder XRD, however, the exact content of various elements could be found by EDAX only.

  10. 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.

  11. Noncovalent Interaction Energies in Covalent Complexes: TEM-1 beta-Lactamase and beta-Lactams

    SciTech Connect

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

    2010-03-08

    The class A {beta}-lactamase TEM-1 is a key bacterial resistance enzyme against {beta}-lactam antibiotics, but little is known about the energetic bases for complementarity between TEM-1 and its inhibitors. Most inhibitors form a covalent adduct with the catalytic Ser70, making the measurement of equilibriumconstants, and hence interaction energies, technically difficult. This study evaluates noncovalent interactions withincovalent complexes by examining the differential stability of TEM-1 and its inhibitor adducts. The thermal denaturation of TEM-1 follows a two-state, reversible model with a melting temperature (T{sub m}) of 51.6 C and a van't Hoff enthalpy of unfolding ({Delta}H{sub VH}) of 146.2 kcal/mol at pH 7.0. The stability of the enzyme changes on forming an inhibitor adduct. As expected, some inhibitors stabilize TEM-1; transition-state analogues increase the T{sub m} by up to 3.7 C(1.7 kcal/mol). Surprisingly, all {beta}-lactam covalent acyl-enzyme complexes tested destabilize TEM-1 significantly relative to the apoenzyme. For instance, the clinically used inhibitor clavulanic acid and the {beta}-lactamase-resistant {beta}-lactams moxalactam and imipenem destabilize TEM-1 by over 2.6 C (1.2 kcal/mol) in their covalent adducts. Based on the structure of the TEM-1/imipenem complex (Maveyraud et al., J Am Chem Soc 1998;120:9748-52), destabilization by moxalactam and imipenem is thought to be caused by a steric clash between the side-chain of Asn132 and the 6(7)-{alpha} group of these {beta}-lactams. To test this hypothesis, the mutant enzyme N132A was made. In contrast with wild-type, the covalent complexes between N132A and both imipenem and moxalactam stabilize the enzyme, consistent with the hypothesis. To investigate the structural bases of this dramatic change instability, the structure of N132A/imipenem was determined by X-ray crystallography. In the complex with N132A, imipenemadopts a very different conformation from that observed in the wild

  12. TEM-158 (CMT-9), a New Member of the CMT-Type Extended-Spectrum β-Lactamases▿

    PubMed Central

    Robin, Frédéric; Delmas, Julien; Brebion, Amélie; Dubois, Damien; Constantin, Jean-Michel; Bonnet, Richard

    2007-01-01

    TEM-158 was found to include the substitutions previously observed for TEM-12 and TEM-35. This enzyme presented hydrolytic activity against ceftazidime and a high level of resistance against clavulanate, which can alter its detection. Its discovery highlights the need for accurate detection methods. PMID:17709463

  13. Characterization of small inclusions: SEM vs TEM, or is it even worth considering SEM?

    SciTech Connect

    Blais, C.; L`Esperance, G.; Baril, E.; Forget, C.

    1996-12-31

    Inclusions of technological importance are often in the size range from 0.1 to 1 {mu}m. These inclusions are generally too thick for EEL-spectrometry and require the use of EDS to characterize their chemical composition. Recent Monte Carlo simulations indicated that scanning electron electron microscopes (SEM`s) equipped with a field emission gun (FEG) might challenge transmission electron microscopes (TEM`s) for the characterization of small inclusions. In the light of these results, we investigated the possibility of using a FEGSEM to characterize inclusions found in micro-alloyed steel welds used for arctic applications. The main setbacks of using EDS for such a task are due to the presence of small phases of unknown thicknesses, non-homogeneity of the X-ray generation volumes, variation in absorption along the path length of the X-rays, etc. Even though these problems are encountered in both the SEM and the TEM, the relative ease of imaging the very small inclusions in TEM confers a definite advantage to this technique. Furthermore, TEM allows to obtain convergent-beam electron diffraction patterns (CBED) which complement the chemical composition characterization, thereby allowing the unambiguous identification of the phases present (chemistry and crystal structure).

  14. TEM Observations of Corrosion Behaviors of Platinized Carbon Blacks under Thermal and Electrochemical Conditions

    SciTech Connect

    Liu, Z.Y.; Zhang, J.L.; Yu, P.T.; Zhang, J.X.; Makharia, R.; More, Karren Leslie; Stach, Eric

    2010-01-01

    Carbon blacks such as Vulcan XC-72 are widely used to support platinum (Pt) or Pt alloy catalysts in proton exchange membrane fuel cells. Despite their widespread use, carbon blacks are susceptible to corrosion during fuel cell operations. In this work, the corrosion behaviors of platinized Vulcan XC-72 nanoparticles under thermal and electrochemical conditions were monitored by transmission electron microscopy (TEM). The thermal corrosion experiment was carried out in a gas-cell TEM, which allows for a direct observation of the thermal oxidation behavior of the nanoparticles. The electrochemical corrosion experiment was performed outside of the TEM by loading the nanoparticles on a TEM grid and then electrochemically corroding them step by step followed by taking TEM images from exactly the same nanoparticles after each step. This work revealed four types of structural changes: (i) total removal of structurally weak aggregates, (ii) breakdown of aggregates via neck-breaking, (iii) center-hollowed primary particles caused by an inside-out corrosion starting from the center to outer region, and (iv) gradual decrease in the size of primary particles caused by a uniform removal of material from the surface. These structural changes took place in sequence or simultaneously depending on the competition of carbon corrosion dynamical processes. The results obtained from this work provide insight on carbon corrosion and its effects on fuel cells' long-term performance and durability.

  15. 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

  16. 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

  17. E240V substitution increases catalytic efficiency toward ceftazidime in a new natural TEM-type extended-spectrum beta-lactamase, TEM-149, from Enterobacter aerogenes and Serratia marcescens clinical isolates.

    PubMed

    Perilli, Mariagrazia; Celenza, Giuseppe; De Santis, Francesca; Pellegrini, Cristina; Forcella, Chiara; Rossolini, Gian Maria; Stefani, Stefania; Amicosante, Gianfranco

    2008-03-01

    The aim of this study was to characterize a novel extended-spectrum beta-lactamase that belongs to the TEM family, the TEM-149 enzyme, and that was isolated from the urine of two hospitalized patients from different hospitals in southern Italy. The peculiarity of this enzyme was the finding of a valine residue at position 240. The array of amino acid substitutions found in TEM-149 was as follows: E104K, R164S, M182T, and E240V. A reversion of a threonine residue at position 182 was also performed to create a new mutant, TEM-149 T182M, in order to assess the contribution of this substitution on the kinetic profile and the stability of TEM-149. The bla TEM-149 and bla TEM-149/T182M genes were cloned into pBC-SK, and the corresponding enzymes were purified from recombinant Escherichia coli HB101 by the same procedure. Both enzymes hydrolyzed all beta-lactams tested, with a preference for ceftazidime, which was found to be the best substrate. By comparison of the kinetic parameters of the TEM-149 and the TEM-149 T182M enzymes, a reduction of the catalytic efficiency for the TEM-149 T182M mutant was observed against all substrates tested except benzylpenicillin, cefotaxime, and aztreonam. Tazobactam, clavulanic acid, and sulbactam were good inhibitors of the TEM-149 beta-lactamase.

  18. Transmission EELS of oxide superconductors with a cold field emission TEM.

    PubMed

    Wang, Y Y; Zhang, H; Dravid, V P

    1995-02-15

    Electron energy loss spectrometry (EELS) with a cold field emission gun (cFEG) transmission electron microscope (TEM) is implemented to analyze the evolution of the electronic structure and dielectric function of oxide superconductors. The O-K core loss spectra of p-type doped oxide superconductors are analyzed in terms of holes formation on oxygen sites, while low loss spectra are analyzed for free carrier plasmas, other spectral excitations, and their crystallographic confinement. It is illustrated that the transmission EELS with a cFEG TEM very much complement soft X-ray absorption spectroscopy and optical spectroscopy, with the added advantages of high spatial resolution (approximately 1-100 nm), and is compatible with other analytical, diffraction, and imaging techniques, which are readily available in a cFEG TEM.

  19. Cryogenic transmission electron microscopy (cryo-TEM) for studying the morphology of colloidal drug delivery systems.

    PubMed

    Kuntsche, Judith; Horst, Jennifer C; Bunjes, Heike

    2011-09-30

    Cryogenic transmission electron microscopy (cryo-TEM) has evolved into an indispensable tool for the characterization of colloidal drug delivery systems. It can be applied to study the size, shape and internal structure of nanoparticulate carrier systems as well as the overall colloidal composition of the corresponding dispersions. This review gives a short overview over the instrumentation used in cryo-TEM experiments and over the sample preparation procedure. Selected examples of cryo-TEM studies on colloidal drug carrier systems, including liposomes, colloidal lipid emulsions, solid lipid nanoparticles, thermotropic and lyotropic liquid crystalline nanoparticles, polymer-based colloids and delivery systems for nucleic acids, are presented in order to illustrate the wealth of information that can be obtained by this technique.

  20. 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.

  1. 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

  2. Imaging modes for direct electron detection in TEM with column parallel CCD

    NASA Astrophysics Data System (ADS)

    Moldovan, Grigore; Jeffery, Ben; Nomerotski, Andrei; Kirkland, Angus

    2009-08-01

    Electron imaging detectors have become the main limiting factor in transmission electron microscopy (TEM). A transition is now being made from indirect scintillator-coupled cameras to directly exposed detectors, which propose imaging modes that are novel in TEM. This work uses a dataset recoded with a directly exposed column parallel charge-coupled-device (CCD) to characterize modulation transfer and detective quantum efficiency of integrating, binary and counting imaging modes. Results presented here demonstrate that counting mode produces final images with largest contrast and highest efficiency because it takes into account the large lateral displacement of beam electrons in the detector. Counting imaging mode is recommended in TEM to take advantage from the higher sensitivity of directly exposed detectors.

  3. 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.

  4. First characterization of inhibitor-resistant TEM (IRT) beta-lactamases in Klebsiella pneumoniae strains.

    PubMed Central

    Lemozy, J; Sirot, D; Chanal, C; Huc, C; Labia, R; Dabernat, H; Sirot, J

    1995-01-01

    Two clinical strains of Klebsiella pneumoniae, TP 01 and TP 02, presented resistance to amoxicillin-clavulanate and were fully susceptible to cephalothin. These strains produced two beta-lactamases, SHV-1 and a TEM enzyme with a pI of 5.2. The previously described changes Arg-244-->Cys and Arg-244-->Ser in IRT-1 and IRT-2 (A. Belaaouaj, C. Lapoumeroulie, M. M. Caniça, G. Vedel, P. Nevot, R. Krishnamoorthy, and G. Paul, FEMS Microbiol. Lett. 120:75-80, 1994) were found in TEM enzymes from the TP 01 and TP 02 strains, respectively. This is the first report of inhibitor-resistant TEM (IRT) in species other than Escherichia coli from the family Enterobacteriaceae. PMID:8585751

  5. 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.

  6. 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.

  7. Electrochemical loading of TEM grids used for the study of potential dependent morphology of polyaniline nanofibres.

    PubMed

    Bhadu, Gopala Ram; Paul, Anirban; Perween, Mosarrat; Gupta, Rajeev; Chaudhari, Jayesh C; Srivastava, Divesh N

    2016-03-01

    An electrochemical method for loading electroactive materials over the TEM grid is reported. The protocol has been demonstrated using polyaniline as an example. The electroactive polymer was directly deposited over the Au TEM grid, used as working electrode in a 3 electrode electrochemical cell. The undisturbed as-deposited morphologies under the influence of various counter ions and ex situ electrochemical states have been studied and compared. Contrary to behaviour in bulk the individual polyaniline fibre was found thinner at anodic potentials. The movement of counter ions as a function of the electrochemical state of the polymer was studied using STEM-EDX elemental mapping. PMID:26694198

  8. 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

  9. 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.

  10. TEM-24 Produced by Four Different Species of Enterobacteriaceae, Including Providencia rettgeri, in a Single Patient

    PubMed Central

    Marchandin, Helene; Carriere, Christian; Sirot, Danielle; Pierre, Helene Jean-; Darbas, Helene

    1999-01-01

    Four species of members of the family Enterobacteriaceae harboring extended-spectrum β-lactamase (ESBL) were recovered in a single patient hospitalized in an intensive care unit. Among these isolates, we describe for the first time an ESBL-producing Providencia rettgeri strain. Bacteria from the same species were shown to be genetically related by pulsed-field gel electrophoresis analysis. These strains produced the same TEM derivative ESBL, characterized as TEM-24. This enzyme had the peculiarity of being encoded by a large conjugative plasmid of 180 kb, never previously described for such an ESBL. PMID:10428940

  11. Electrochemical loading of TEM grids used for the study of potential dependent morphology of polyaniline nanofibres.

    PubMed

    Bhadu, Gopala Ram; Paul, Anirban; Perween, Mosarrat; Gupta, Rajeev; Chaudhari, Jayesh C; Srivastava, Divesh N

    2016-03-01

    An electrochemical method for loading electroactive materials over the TEM grid is reported. The protocol has been demonstrated using polyaniline as an example. The electroactive polymer was directly deposited over the Au TEM grid, used as working electrode in a 3 electrode electrochemical cell. The undisturbed as-deposited morphologies under the influence of various counter ions and ex situ electrochemical states have been studied and compared. Contrary to behaviour in bulk the individual polyaniline fibre was found thinner at anodic potentials. The movement of counter ions as a function of the electrochemical state of the polymer was studied using STEM-EDX elemental mapping.

  12. TEM7 (PLXDC1), a key prognostic predictor for resectable gastric cancer, promotes cancer cell migration and invasion

    PubMed Central

    Zhang, Zi-Zhen; Hua, Rong; Zhang, Jun-Feng; Zhao, Wen-Yi; Zhao, En-Hao; Tu, Lin; Wang, Chao-Jie; Cao, Hui; Zhang, Zhi-Gang

    2015-01-01

    Tumor endothelial marker 7 (TEM7) is a new candidate of molecular target for antiangiogenic therapy. This study aims to evaluate its expression in gastric cancer (GC) and to explore the correlation between its expression and the clinical outcome of patients. Expression of TEM7 was analyzed in both tumor tissues and cell lines of GC by real-time quantitative RT-PCR (qRT-PCR) and Western blot. RNA interference (RNAi) approaches were used to investigate the biological functions of TEM7. The effects of TEM7 on cell migration and invasion were evaluated by Transwell assays. In vitro experiments revealed that TEM7 was significantly overexpressed in GC cell lines (N87, AGS and SGC-7901) by 2-fold to 4-fold, and knockdown of TEM7 could significantly inhibit cancer cell migration and invasion. For GC patients, TEM7 gene expression was elevated in tumors in most cases (25/31), and its expression was closely correlated with tumor differentiation, depth of cancer invasion, lymphatic metastasis and TNM stage. The overall survival of TEM7 (-) group was significantly higher than that of TEM7 (+) group (P = 0.048) and TEM7 (++) group (P = 0.003). TEM7 is highly expressed in GC and is likely correlated with tumor invasion and migration, and thus its expression is closely related to the clinical outcome of patients. PMID:25973314

  13. [Research on characteristics of soil clay mineral evolution in paddy field and dry land by XRD spectrum].

    PubMed

    Zhang, Zhi-dan; Li, Qiao; Luo, Xiang-li; Jiang, Hai-chao; Zheng, Qing-fu; Zhao, Lan-po; Wang, Ji-hong

    2014-08-01

    The present paper took the typical saline-alkali soil in Jilin province as study object, and determinated the soil clay mineral composition characteristics of soil in paddy field and dry land. Then XRD spectrum was used to analyze the evolutionary mechanism of clay mineral in the two kinds of soil. The results showed that the physical and chemical properties of soil in paddy field were better than those in dry land, and paddy field would promote the weathering of mineral particles in saline-alkali soil and enhance the silt content. Paddy field soil showed a strong potassium-removal process, with a higher degree of clay mineral hydration and lower degree of illite crystallinity. Analysis of XRD spectrum showed that the clay mineral composition was similar in two kinds of soil, while the intensity and position of diffraction peak showed difference. The evolution process of clay mineral in dry land was S/I mixture-->vermiculite, while in paddy field it was S/I mixture-->vermiculite-->kaolinite. One kind of hydroxylated 'chlorite' mineral would appear in saline-alkali soil in long-term cultivated paddy field. Taking into account that the physical and chemical properties of soil in paddy field were better then those in dry land, we could know that paddy field could help much improve soil structure, cultivate high-fertility soil and improve saline-alkali soil. This paper used XRD spectrum to determine the characteristics of clay minerals comprehensively, and analyzed two'kinds of land use comparatively, and was a new perspective of soil minerals study. PMID:25508755

  14. [Research on characteristics of soil clay mineral evolution in paddy field and dry land by XRD spectrum].

    PubMed

    Zhang, Zhi-dan; Li, Qiao; Luo, Xiang-li; Jiang, Hai-chao; Zheng, Qing-fu; Zhao, Lan-po; Wang, Ji-hong

    2014-08-01

    The present paper took the typical saline-alkali soil in Jilin province as study object, and determinated the soil clay mineral composition characteristics of soil in paddy field and dry land. Then XRD spectrum was used to analyze the evolutionary mechanism of clay mineral in the two kinds of soil. The results showed that the physical and chemical properties of soil in paddy field were better than those in dry land, and paddy field would promote the weathering of mineral particles in saline-alkali soil and enhance the silt content. Paddy field soil showed a strong potassium-removal process, with a higher degree of clay mineral hydration and lower degree of illite crystallinity. Analysis of XRD spectrum showed that the clay mineral composition was similar in two kinds of soil, while the intensity and position of diffraction peak showed difference. The evolution process of clay mineral in dry land was S/I mixture-->vermiculite, while in paddy field it was S/I mixture-->vermiculite-->kaolinite. One kind of hydroxylated 'chlorite' mineral would appear in saline-alkali soil in long-term cultivated paddy field. Taking into account that the physical and chemical properties of soil in paddy field were better then those in dry land, we could know that paddy field could help much improve soil structure, cultivate high-fertility soil and improve saline-alkali soil. This paper used XRD spectrum to determine the characteristics of clay minerals comprehensively, and analyzed two'kinds of land use comparatively, and was a new perspective of soil minerals study. PMID:25474976

  15. Powder-XRD and (14) N magic angle-spinning solid-state NMR spectroscopy of some metal nitrides.

    PubMed

    Kempgens, Pierre; Britton, Jonathan

    2016-05-01

    Some metal nitrides (TiN, ZrN, InN, GaN, Ca3 N2 , Mg3 N2 , and Ge3 N4 ) have been studied by powder X-ray diffraction (XRD) and (14) N magic angle-spinning (MAS) solid-state NMR spectroscopy. For Ca3 N2 , Mg3 N2 , and Ge3 N4 , no (14) N NMR signal was observed. Low speed (νr  = 2 kHz for TiN, ZrN, and GaN; νr  = 1 kHz for InN) and 'high speed' (νr  = 15 kHz for TiN; νr  = 5 kHz for ZrN; νr  = 10 kHz for InN and GaN) MAS NMR experiments were performed. For TiN, ZrN, InN, and GaN, powder-XRD was used to identify the phases present in each sample. The number of peaks observed for each sample in their (14) N MAS solid-state NMR spectrum matches perfectly well with the number of nitrogen-containing phases identified by powder-XRD. The (14) N MAS solid-state NMR spectra are symmetric and dominated by the quadrupolar interaction. The envelopes of the spinning sidebands manifold are Lorentzian, and it is concluded that there is a distribution of the quadrupolar coupling constants Qcc 's arising from structural defects in the compounds studied.

  16. [Research on characteristics of soil clay mineral evolution in paddy field and dry land by XRD spectrum].

    PubMed

    Zhang, Zhi-dan; Li, Qiao; Luo, Xiang-li; Jiang, Hai-chao; Zheng, Qing-fu; Zhao, Lan-po; Wang, Ji-hong

    2014-08-01

    The present paper took the typical saline-alkali soil in Jilin province as study object, and determinated the soil clay mineral composition characteristics of soil in paddy field and dry land. Then XRD spectrum was used to analyze the evolutionary mechanism of clay mineral in the two kinds of soil. The results showed that the physical and chemical properties of soil in paddy field were better than those in dry land, and paddy field would promote the weathering of mineral particles in saline-alkali soil and enhance the silt content. Paddy field soil showed a strong potassium-removal process, with a higher degree of clay mineral hydration and lower degree of illite crystallinity. Analysis of XRD spectrum showed that the clay mineral composition was similar in two kinds of soil, while the intensity and position of diffraction peak showed difference. The evolution process of clay mineral in dry land was S/I mixture-->vermiculite, while in paddy field it was S/I mixture-->vermiculite-->kaolinite. One kind of hydroxylated 'chlorite' mineral would appear in saline-alkali soil in long-term cultivated paddy field. Taking into account that the physical and chemical properties of soil in paddy field were better then those in dry land, we could know that paddy field could help much improve soil structure, cultivate high-fertility soil and improve saline-alkali soil. This paper used XRD spectrum to determine the characteristics of clay minerals comprehensively, and analyzed two'kinds of land use comparatively, and was a new perspective of soil minerals study.

  17. Astrobiological Significance of Definitive Mineralogical Analysis of Martian Surface Samples Using the CheMin XRD/XRF Instrument

    NASA Technical Reports Server (NTRS)

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

    2004-01-01

    The search for evidence of habitability, or of extant or extinct life on Mars, will initially be a search for evidence of past or present conditions supportive of life. The three key requirements for the emergence of life are thought to be liquid water; a suitable energy source; and chemical building blocks. CheMin is a miniaturized XRD/XRF (X-Ray diffraction / X-ray fluorescence) instrument which has been developed for definitive mineralogic analysis of soils and rocks on the Martian surface. The CheMin instrument can provide information that is highly relevant to each of these habitability requirements as summarized below.

  18. 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.

  19. Molecular dynamics simulations and morphology analysis of TEM imaged PVDF nanofibers

    NASA Astrophysics Data System (ADS)

    Miao, Jiayuan; Reneker, Darrell; Tsige, Mesfin; Taylor, Philip

    With the goal of elucidating the structure of polyvinylidene fluoride (PVDF) nanofibers, all-atom molecular dynamics simulations were performed, and the results compared with structures observed in high resolution transmission electron microscopy (TEM) at the molecular level. Simulation shows that the stability of the β-phase component in a PVDF nanofiber is influenced by its thickness and processing history. When exposed to irradiation, as in a TEM observation, the structure is then further modified by the effects of chain scission. The transformation from the β phase into a paraelectric phase can explain the spindle formation and serpentine motion of molecular segments observed by Zhong et al. (Polymer, 54, 2013, 3745-3756) in irradiated PVDF nanofibers. From a comparison between simulated and experimental TEM images it was possible to identify numerous features that are useful in unveiling the inherent structure of PVDF nanofibers. The experimental TEM images appear to match well with those predicted by a model based on α-phase PVDF, while also being consistent with an alternative model (Nanoscale 2015, DOI: 10.1039/c5nr01619c). Work supported by the Petroleum Research Fund of the ACS.

  20. Engineering allosteric regulation into the hinge region of a circularly permuted TEM-1 beta-lactamase.

    PubMed

    Mathieu, Valéry; Fastrez, Jacques; Soumillion, Patrice

    2010-09-01

    In nature, the activity of many enzymes involved in important biochemical pathways is controlled by binding a ligand in a site remote from the active site. The allosteric sites are frequently located in hinge regulatory subunits, in which a conformational change can occur and propagate to the active site. The enzymatic activity is then enhanced or decreased depending on the type of effectors. Many artificial binding sites have been created to engineer an allosteric regulation. Generally, these sites were engineered near the active site in loops or at the surface of contiguous helices or strands but rarely in hinge regions. This work aims at exploring the possibility of regulating a monomeric enzyme whose active site is located at the interface between two domains. We anticipated that binding of a ligand in the hinge region linking the domains would modify their positioning and, consequently, modulate the activity. Here, we describe the design of two mutants in a circularly permuted TEM-1 (cpTEM-1) beta-lactamase. The first one, cpTEM-1-His(3) was created by a rational design. It shows little regulation upon metal ion binding except for a weak activation with Zn(2+). The second one, cpTEM-1-3M-His(2), was selected by a directed evolution strategy. It is allosterically down-regulated by Zn(2+), Ni(2+) and Co(2+) with binding affinities around 300 microM.

  1. Comparative investigation of Fourier Transform Infrared (FT-IR) spectroscopy and X-ray Diffraction (XRD) in the determination of cotton fiber crystallinity

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Despite considerable efforts in developing the curve-fitting protocol to evaluate the crystallinity index (CI) from the X-ray diffraction (XRD) measurement, in its present state XRD procedure can only provide a qualitative or semi-quantitative assessment of the amounts of crystalline or amorphous po...

  2. In situ TEM straining of nanograined free-standing thin films reveals various unexpected deformation mechanisms.

    SciTech Connect

    Follstaedt, David Martin; Knapp, James Arthur; Clark, Blythe G.; Hattar, Khalid M.; Robertson, Ian M.

    2010-04-01

    In-situ transmission electron microscopy (TEM) straining experiments provide direct detailed observation of the deformation and failure mechanisms active at a length scale relevant to nanomaterials. This presentation will detail continued investigations into the active mechanisms governing high purity nanograined pulsed-laser deposited (PLD) nickel, as well as recent work into dislocation-particle interactions in nanostructured PLD aluminum-alumina alloys. Straining experiments performed on nanograined PLD free-standing nanograined Ni films with an engineered grain size distribution revealed that the addition of ductility with limited decrease in strength, reported in such metals, can be attributed to the simultaneous activity of three deformation mechanisms in front of the crack tip. At the crack tip, a grain agglomeration mechanism occurs where several nanograins appear to rotate, resulting in a very thin, larger grain immediately prior to failure. In the classical plastic zone in front of the crack tip, a multitude of mechanisms were found to operate in the larger grains including: dislocation pile-up, twinning, and stress-assisted grain growth. The region outside of the plastic zone showed signs of elasticity with limited indications of dislocation activity. The insight gained from in-situ TEM straining experiments of nanograined PLD Ni provides feedback for models of the deformation and failure in nanograined FCC metals, and suggests a greater complexity in the active mechanisms. The investigation into the deformation and failure mechanisms of FCC metals via in-situ TEM straining experiments has been expanded to the effect of hard particles on the active mechanisms in nanograined aluminum with alumina particles. The microstructures investigated were developed with varying composition, grain size, and particle distribution via tailoring of the PLD conditions and subsequent annealing. In order to develop microstructures suitable for in-situ deformation testing

  3. Development and Application of Operando TEM to a Ruthenium Catalyst for CO Oxidation

    NASA Astrophysics Data System (ADS)

    Miller, Benjamin Kyle

    Operando transmission electron microscopy (TEM) is an extension of in-situ TEM in which the performance of the material being observed is measured simultaneously. This is of great value, since structure-performance relationships lie at the heart of materials science. For catalyst materials, like the SiO2-supported Ru nanoparticles studied, the important performance metric, catalyst activity, is measured inside the microscope by determining the gas composition during imaging. This is accomplished by acquisition of electron energy loss spectra (EELS) of the gas in the environmental TEM while catalysis is taking place. In this work, automated methods for rapidly quantifying low-loss and core-loss EELS of gases were developed. A new sample preparation method was also established to increase catalytic conversion inside a differentially-pumped environmental TEM, and the maximum CO conversion observed was about 80%. A system for mixing gases and delivering them to the environmental TEM was designed and built, and a method for locating and imaging nanoparticles in zone axis orientations while minimizing electron dose rate was determined. After atomic resolution images of Ru nanoparticles observed during CO oxidation were obtained, the shape and surface structures of these particles was investigated. A Wulff model structure for Ru particles was compared to experimental images both by manually rotating the model, and by automatically determining a matching orientation using cross-correlation of shape signatures. From this analysis, it was determined that most Ru particles are close to Wulff-shaped during CO oxidation. While thick oxide layers were not observed to form on Ru during CO oxidation, thin RuO2 layers on the surface of Ru nanoparticles were imaged with atomic resolution for the first time. The activity of these layers is discussed in the context of the literature on the subject, which has thus far been inconclusive. We conclude that disordered oxidized ruthenium

  4. Nanoleakage within the hybrid layer: a correlative FEISEM/TEM investigation.

    PubMed

    Suppa, Pietro; Breschi, Lorenzo; Ruggeri, Alessandra; Mazzotti, Giovanni; Prati, Carlo; Chersoni, Stefano; Di Lenarda, Roberto; Pashley, David H; Tay, Franklin R

    2005-04-01

    The aim of this study was to compare the nanoleakage patterns of the resin-dentin interfaces of three dentin bonding systems at both TEM and field emission in lens SEM (FEI-SEM) levels. A standardized smear layer was created with 180-grit silicon carbide paper (SiC) on dentin disks obtained from 18 noncarious human third molars. Specimens were randomly divided into three groups and bonded with a two-step total etching adhesive (Single Bond, SB), a two-step, self-etching adhesive (Clearfil SE BOND, SEB), and a one-step, self-etching adhesive (XENO III, XEIII). Nanoleakage was evaluated by using an ammoniacal silver-nitrate solution. Specimens were processed for TEM and FEI-SEM observation. The TEM of SB revealed silver deposits in adhesive and hybrid layers (HL). High-magnification FEI-SEM micrographs clearly identified these deposits as spherical clusters mainly associated with nonembedded collagen fibrils. TEM and FEI-SEM examination of SEB revealed some clusters of silver deposits within porosities and small channels of the HL. Additional silver deposits were observed between the peritubular dentin walls and the resin tags. XEIII revealed very fine and diffuse silver grains throughout the entire HL. SEM visualization of nanoleakage at a high level of resolution has not been previously described. FEI-SEM technology supported the TEM visualization with three-dimensional morphological data of the relations between the HL constituents and nanoleakage. The results of the present study confirm the hypothesis that both total- and self-etch adhesives are not able to fully infiltrate the dentin substrate. PMID:15678495

  5. Thromboelastometry (TEM) findings in disseminated intravascular coagulation in a pig model of endotoxinemia.

    PubMed

    Schöchl, Herbert; Solomon, Cristina; Schulz, Arthur; Voelckel, Wolfgang; Hanke, Alexander; Van Griensven, Martijn; Redl, Heinz; Bahrami, Soheyl

    2011-01-01

    Standard coagulation tests have a low specificity and sensitivity for diagnosing disseminated intravascular coagulation. The aim of this study was to determine whether whole blood thromboelastometry (TEM) detects lipopolysaccharide (LPS)-induced changes in coagulation. Blood samples from 10 pigs were drawn at baseline, before and at the end of LPS infusion and 2, 3, 4 and 5 h after the start of endotoxinemia. Simultaneous to TEM, standard coagulation tests and extended coagulation analysis including tissue plasminogen activator (t-PA) and plasminogen activator inhibitor 1 (PAI-1) were performed. Endotoxinemia resulted in a significant acceleration of the nonactivated TEM (NATEM) clotting time 2 h after the end of LPS infusion; in contrast, the changes in international normalized ratio and activated partial thromboplastin time suggested delayed initiation of coagulation. NATEM maximum clot firmness (MCF) and fibrin-based thromboelastometry test (FIBTEM)-MCF decreased significantly from baseline until the last time point (from 64.6 ± 7.8 and 35.1 ± 12.8 mm to 52.8 ± 4.6 and 21.4 ± 11.8 mm, respectively; P = 0.01 for both parameters). A sharp, transient increase of t-PA had no effect on maximum lysis in the NATEM test. PAI-1 increased significantly 3 h after the start of LPS infusion, paralleled by a decrease in maximum lysis. In conclusion, TEM was superior to standard coagulation tests in reflecting initial activation of coagulation during endotoxinemia. TEM further suggested consumption of coagulation substrate; at the same time, inhibition of plasminogen activation was accompanied by improved clot stability. Further investigations are necessary to establish the clinical relevance of these findings.

  6. Synthesis of metal complexes involving Schiff base ligand with methylenedioxy moiety: Spectral, thermal, XRD and antimicrobial studies

    NASA Astrophysics Data System (ADS)

    Sundararajan, M. L.; Jeyakumar, T.; Anandakumaran, J.; Karpanai Selvan, B.

    2014-10-01

    Metal complexes of Zn(II), Cd(II), Ni(II), Cu(II), Fe(III), Co(II), Mn(II) Hg(II), and Ag(I) have been synthesized from Schiff base ligand, prepared by the condensation of 3,4-(methylenedioxy)aniline and 5-bromo salicylaldehyde. All the compounds have been characterized by using elemental analysis, molar conductance, FT-IR, UV-Vis, 1H NMR, 13C NMR, mass spectra, powder XRD and thermal analysis (TG/DTA) technique. The elemental analysis suggests the stoichiometry to be 1:1 (metal:ligand). The FT-IR, 1H NMR, 13C NMR and UV-Vis spectral data suggest that the ligand coordinate to the metal atom by imino nitrogen and phenolic oxygen as bidentate manner. Mass spectral data further support the molecular mass of the compounds and their structure. Powder XRD indicates the crystalline state and morphology of the ligand and its metal complexes. The thermal behaviors of the complexes prove the presence of lattice as well as coordinated water molecules in the complexes. Melting point supports the thermal stability of all the compounds. The in vitro antimicrobial effects of the synthesized compounds were tested against five bacterial and three fungal species by well diffusion method. Antioxidant activities have also been performed for all the compounds. Metal complexes show more biological activity than the Schiff base.

  7. Combined in situ XRD and in situ XANES studies on the reduction behavior of a rhenium promoted cobalt catalyst.

    PubMed

    Kumar, Nitin; Payzant, E A; Jothimurugesan, K; Spivey, J J

    2011-08-28

    A 10% Co-4% Re/(2% Zr/SiO(2)) catalyst was prepared by co-impregnation using a silica support modified by 2% Zr. The catalyst was characterized by temperature programmed reduction (TPR), in situ XRD and in situ XANES analysis where it was simultaneously exposed to H(2) using a temperature programmed ramp. The results showed the two step reduction of large crystalline Co(3)O(4) with CoO as an intermediate. TPR results showed that the reduction of highly dispersed Co(3)O(4) was facilitated by reduced rhenium by a H(2)-spillover mechanism. In situ XRD results showed the presence of both, Co-hcp and Co-fcc phases in the reduced catalyst at 400 °C. However, the Co-hcp phase was more abundant, which is thought to be the more active phase as compared to the Co-fcc phase for CO hydrogenation. CO hydrogenation at 270 °C and 5 bar pressure produces no detectable change in the phases during the time of experiment. In situ XANES results showed a decrease in the metallic cobalt in the presence of H(2)/CO, which can be attributed due to oxidation of the catalyst by reaction under these conditions. PMID:21743918

  8. Synthesis of metal complexes involving Schiff base ligand with methylenedioxy moiety: spectral, thermal, XRD and antimicrobial studies.

    PubMed

    Sundararajan, M L; Jeyakumar, T; Anandakumaran, J; Karpanai Selvan, B

    2014-10-15

    Metal complexes of Zn(II), Cd(II), Ni(II), Cu(II), Fe(III), Co(II), Mn(II) Hg(II), and Ag(I) have been synthesized from Schiff base ligand, prepared by the condensation of 3,4-(methylenedioxy)aniline and 5-bromo salicylaldehyde. All the compounds have been characterized by using elemental analysis, molar conductance, FT-IR, UV-Vis, (1)H NMR, (13)C NMR, mass spectra, powder XRD and thermal analysis (TG/DTA) technique. The elemental analysis suggests the stoichiometry to be 1:1 (metal:ligand). The FT-IR, (1)H NMR, (13)C NMR and UV-Vis spectral data suggest that the ligand coordinate to the metal atom by imino nitrogen and phenolic oxygen as bidentate manner. Mass spectral data further support the molecular mass of the compounds and their structure. Powder XRD indicates the crystalline state and morphology of the ligand and its metal complexes. The thermal behaviors of the complexes prove the presence of lattice as well as coordinated water molecules in the complexes. Melting point supports the thermal stability of all the compounds. The in vitro antimicrobial effects of the synthesized compounds were tested against five bacterial and three fungal species by well diffusion method. Antioxidant activities have also been performed for all the compounds. Metal complexes show more biological activity than the Schiff base. PMID:24820326

  9. XRD analysis on ZnO and Au film crystal orientation in ZnO/Au/SiO2 structure

    NASA Astrophysics Data System (ADS)

    Qin, Huibin; Yu, Hong; Chen, Yunxang

    2000-05-01

    The orientation of the Zn/Au/Si structure was examined by XRD. The experiment showed that the ZnO/Au/Si films deposited by magnetron sputtering were possessed of a preferred orientation in C axis perpendicular to the film surface. The (111) of Au film was possessed of a preferred <111> orientation which was perpendicular to the film surface also. The XRD (theta) approximately 2 (theta) scan irradiated that there were only (001) peaks in excellent orientated ZnO films. The rock cure scan demonstrated that the C axis of ZnO film was not exactly perpendicular to the surface, the angular divergence was about 2 degree(s), and the space divergence angle about 1.5 degree(s). Expert the (kkk) main peaks of Au film there were weak diffraction peaks, such as (002), (022), and (311) peaks. The phenomena indicated that in Au film there was not only (111) plane in parallel to the surface of substrate. As there was only 12% dis-matching between Au (111) and ZnO (001), the Au (111) oriented film was facilitated for the ZnO (001) orientation in C axis and deposing parameters adjustment.

  10. Thermoluminescence (TL) properties and x-ray diffraction (XRD) analysis of high purity CaSO4:Dy TL material

    NASA Astrophysics Data System (ADS)

    Kamarudin, Nadira; Abdullah, Wan Saffiey Wan; Hamid, Muhammad Azmi Abdul; Dollah, Mohd Taufik

    2014-09-01

    This paper presents the characterization and TL properties of dysprosium (Dy) doped calcium sulfate (CaSO4) TL material produced by co-precipitation technique with 0.5mol% concentration of dopant. The morphology of the produced TL material was studied using scanning electron microscope (SEM) and the micrograph shows that rectangular parallelepiped shaped crystal with the average of 150 μm in length were produced. The crystallinity of the produced powder was studied using x-ray powder diffraction (XRD). The XRD spectra show that the TL material produced is high purity anhydrite CaSO4 with average crystallite size of 74 nm with orthorhombic crystal system. The TL behavior of produced CaSO4:Dy was studied using a TLD reader after exposure to gamma ray by Co60 source with the doses of 1,5 and 10 Gy. The glow curve shows linear response with glow peak around 230°C which is desired development in the field of radiation dosimetry.

  11. Lead Speciation in House Dust from Canadian Urban Homes Using EXAFS Micro-XRF and Micro-XRD

    SciTech Connect

    L MacLean; S Beauchemin; P Rasmussen

    2011-12-31

    X-ray absorption fine-structure (XAFS) spectroscopy, micro-X-ray fluorescence ({mu}XRF), and micro-X-ray diffraction ({mu}XRD) were used to determine the speciation of Pb in house dust samples from four Canadian urban homes having elevated Pb concentrations (>1000 mg Pb kg{sup -1}). Linear combination fitting of the XAFS data, supported by {mu}XRF and {mu}XRD, shows that Pb is complexed in a variety of molecular environments, associated with both the inorganic and organic fractions of the dust samples. The inorganic species of lead identified were as follows: Pb metal, Pb carbonate, Pb hydroxyl carbonate, Pb oxide, and Pb adsorbed to iron oxyhydroxides. Pb carbonate and/or Pb hydroxyl carbonate occurred in all four dust samples and accounted for 28 to 75% of total Pb. Pb citrate and Pb bound to humate were the organic species identified. The results of this study demonstrate the ability of XAFS to identify Pb speciation in house dust and show the potential to identify Pb sources from new homes versus older homes. Understanding Pb speciation and how it influences bioaccessibility is important for human health risk assessment and risk management decisions which aim to improve indoor environmental health.

  12. TEM1 expression in cancer-associated fibroblasts is correlated with a poor prognosis in patients with gastric cancer

    PubMed Central

    Fujii, Satoshi; Fujihara, Ayano; Natori, Kei; Abe, Anna; Kuboki, Yasutoshi; Higuchi, Youichi; Aizawa, Masaki; Kuwata, Takeshi; Kinoshita, Takahiro; Yasui, Wataru; Ochiai, Atsushi

    2015-01-01

    The cancer stroma, including cancer-associated fibroblasts (CAFs), is known to contribute to cancer cell progression and metastasis, suggesting that functional proteins expressed specifically in CAFs might be candidate molecular targets for cancer treatment. The purpose of the present study was to explore the possibility of using TEM1 (tumor endothelial marker 1), which is known to be expressed in several types of mesenchymal cells, as a molecular target by examining the impact of TEM1 expression on clinicopathological factors in gastric cancer patients. A total of 945 consecutive patients with gastric cancer who underwent surgery at the National Cancer Center Hospital East between January 2003 and July 2007 were examined using a tissue microarray approach. TEM1 expression in CAFs or vessel-associated cells was determined using immunohistochemical staining. Three items (CAF-TEM1-positivity, CAF-TEM1-intensity, and vessel-TEM1-intensity) were then examined to determine the correlations between the TEM1 expression status and the recurrence-free survival (RFS), overall survival (OS), cancer-related survival (COS), and other clinicopathological factors. Significant correlations between CAF-TEM1-positivity or CAF-TEM1-intensity and RFS, OS, or COS were observed (P < 0.001, Kaplan–Meier curves); however, no significant correlation between vessel-TEM1-intensity and RFS, OS, or COS was observed. A univariate analysis showed that CAF-TEM1-positivity and CAF-TEM1-intensity were each correlated with a scirrhous subtype, tumor depth, nodal status, distant metastasis, serosal invasion, lymphatic or venous vessel infiltrations, and pTMN stage. This study suggests that the inhibition of TEM1 expression specifically in the CAFs of gastric carcinoma might represent a new strategy for the treatment of gastric cancer. PMID:26336878

  13. Landed XRD/XRF analysis of prime targets in the search for past or present Martian life

    NASA Astrophysics Data System (ADS)

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

    1998-12-01

    Mars landers seeking evidence for past or present life will be guided by information from orbital mapping and from previous surface exploration. Several target options have been proposed, including sites that may harbor extant life and sites most likely to preserve evidence of past life. These sites have specific mineralogic characteristics. Extant life might be gathered around the sinters and associated mineral deposits of rare active fumaroles, or held within brine pockets and inclusions in a few evaporite-mineral deposits. Possibilities for fossilization include deltaic and lake-bottom sediments of once-flooded craters, sinters formed by ancient hot-spring deposits, and the carbonate deposits associated with some evaporite systems. However, the highly varied mineralogy of fossil occurrences on Earth leads to the inference that Mars, an equally complex planet, could host a broad variety of potential fossilizing deposits. The abundance of volcanic systems on Mars and evidence for close associations between volcanism and water release suggest possibilities of organism entrapment and mineralization in volcaniclastic deposits, as found in some instances on Earth. Thus the targets being considered for exploration include a wide variety of unique deposits that would be characterized by silica or various nonsilicate minerals. Beyond these ``special'' deposits and in the most general case, an ability to distinguish mineralized from uncemented volcanic detritus may be the key to success in finding possible fossilbearing authigenic mineralogies. A prototype miniaturized X ray diffraction/X ray fluorescence (XRD/XRF) instrument has been evaluated with silica, carbonate, and sulfate minerals and with a basalt, to examine the capabilities of this tool in mineralogic and petrologic exploration for exobiological goals. This instrument, CHEMIN (chemical and mineralogical analyzer), is based on an innovative low-power X ray tube, transmission geometry, and CCD collection and

  14. Landed XRD/XRF analysis of prime targets in the search for past or present Martian life.

    PubMed

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

    1998-12-25

    Mars landers seeking evidence for past or present life will be guided by information from orbital mapping and from previous surface exploration. Several target options have been proposed, including sites that may harbor extant life and sites most likely to preserve evidence of past life These sites have specific mineralogic characteristics. Extant life might be gathered around the sinters and associated mineral deposits of rare active fumaroles, or held within brine pockets and inclusions in a few evaporite-mineral deposits. Possibilities for fossilization include deltaic and lake-bottom sediments of once-flooded craters, sinters formed by ancient hot-spring deposits, and the carbonate deposits associated with some evaporite systems. However, the highly varied mineralogy of fossil occurrences on Earth leads to the inference that Mars, an equally complex planet, could host a broad variety of potential fossilizing deposits. The abundance of volcanic systems on Mars and evidence for close associations between volcanism and water release suggest possibilities of organism entrapment and mineralization in volcaniclastic deposits, as found in some instances on Earth. Thus the targets being considered for exploration include a wide variety of unique deposits that would be characterized by silica or various nonsilicate minerals. Beyond these "special" deposits and in the most general case, an ability to distinguish mineralized from uncemented volcanic detritus may be the key to success in finding possible fossil-bearing authigenic mineralogies. A prototype miniaturized X ray diffraction/X ray fluorescence (XRD/XRF) instrument has been evaluated with silica, carbonate, and sulfate minerals and with a basalt, to examine the capabilities of this tool in mineralogic and petrologic exploration for exobiological goals. This instrument. CHEMIN (chemical and mineralogical analyzer), is based on an innovative low-power X ray tube, transmission geometry, and CCD collection and

  15. Landed XRD/XRF analysis of prime targets in the search for past or present Martian life.

    PubMed

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

    1998-12-25

    Mars landers seeking evidence for past or present life will be guided by information from orbital mapping and from previous surface exploration. Several target options have been proposed, including sites that may harbor extant life and sites most likely to preserve evidence of past life These sites have specific mineralogic characteristics. Extant life might be gathered around the sinters and associated mineral deposits of rare active fumaroles, or held within brine pockets and inclusions in a few evaporite-mineral deposits. Possibilities for fossilization include deltaic and lake-bottom sediments of once-flooded craters, sinters formed by ancient hot-spring deposits, and the carbonate deposits associated with some evaporite systems. However, the highly varied mineralogy of fossil occurrences on Earth leads to the inference that Mars, an equally complex planet, could host a broad variety of potential fossilizing deposits. The abundance of volcanic systems on Mars and evidence for close associations between volcanism and water release suggest possibilities of organism entrapment and mineralization in volcaniclastic deposits, as found in some instances on Earth. Thus the targets being considered for exploration include a wide variety of unique deposits that would be characterized by silica or various nonsilicate minerals. Beyond these "special" deposits and in the most general case, an ability to distinguish mineralized from uncemented volcanic detritus may be the key to success in finding possible fossil-bearing authigenic mineralogies. A prototype miniaturized X ray diffraction/X ray fluorescence (XRD/XRF) instrument has been evaluated with silica, carbonate, and sulfate minerals and with a basalt, to examine the capabilities of this tool in mineralogic and petrologic exploration for exobiological goals. This instrument. CHEMIN (chemical and mineralogical analyzer), is based on an innovative low-power X ray tube, transmission geometry, and CCD collection and

  16. The influence of transformation twins on seismic-frequency anelasticity in perovskite: an investigation using stroboscopic XRD-DMA

    NASA Astrophysics Data System (ADS)

    Harrison, R.; Redfern, S.; Buckley, A.; Salje, E.

    2003-04-01

    Recent experimental and theoretical studies suggest that the lower mantle is significantly anelastic. The origin of this anelasticity remains uncertain, however. One possible cause is the viscous motion of twin domain walls. Here we use a combination of dynamical mechanical analysis (DMA) and stroboscopic X-ray diffraction (XRD) to study the effect of domain walls on seismic-frequency anelasticity in perovskite at high temperature. We apply the technique to single crystal LaAlO_3, a close structural analogue of the MgSiO_3 perovskite phase believed to make up more than 70% of the Earth's lower mantle. We demonstrate that superelastic behaviour associated with the motion of domain walls dominates the mechanical response over a temperature range spanning several hundred degrees. This is accompanied by a factor-of-ten decrease in the effective Young's modulus below the cubic to rhombohedral phase transition and a rapid increase in attenuation. Freezing of domain walls at lower temperatures leads to mechanical stiffening and a broad peak in attenuation (tand >0.9 at 200^oC and 1 Hz). The observations indicate that domain walls are strongly pinned by oxygen vacancies. The combination of DMA and XRD permits the response of domain walls to a dynamic force to be observed in-situ for the very first time. The XRD-DMA machine consists of a standard Perkin-Elmer DMA-7e in three-point bend geometry, combined with a conventional X-ray source and position sensitive detector. The X-ray source is movable, allowing X-rays to be focused on the underside of the sample at a wide range of incident angles. Measuring diffracted intensity as a function of incident angle results in a conventional rocking curve, permitting the twin microstructure to be quantified. During a DMA measurement, X-rays are binned into four separate spectra, which are synchronised to four different stages of the dynamic force cycle. In this way, changes in microstructure which occur directly in response to the

  17. Development, optimization, and validation of novel anti-TEM1/CD248 affinity agent for optical imaging in cancer

    PubMed Central

    Hu, Jia; Feng, Yi; Hasegawa, Kosei; Peng, Xiaohui; Duan, Xingmei; Zhao, Aizhi; Mikitsh, John L.; Muzykantov, Vladimir R.; Chacko, Ann-Marie; Pryma, Daniel A.; Dunn, Steven M.; Coukos, George

    2014-01-01

    Tumor Endothelial Marker-1 (TEM1/CD248) is a tumor vascular marker with high therapeutic and diagnostic potentials. Immuno-imaging with TEM1-specific antibodies can help to detect cancerous lesions, monitor tumor responses, and select patients that are most likely to benefit from TEM1-targeted therapies. In particular, near infrared(NIR) optical imaging with biomarker-specific antibodies can provide real-time, tomographic information without exposing the subjects to radioactivity. To maximize the theranostic potential of TEM1, we developed a panel of all human, multivalent Fc-fusion proteins based on a previously identified single chain antibody (scFv78) that recognizes both human and mouse TEM1. By characterizing avidity, stability, and pharmacokinectics, we identified one fusion protein, 78Fc, with desirable characteristics for immuno-imaging applications. The biodistribution of radiolabeled 78Fc showed that this antibody had minimal binding to normal organs, which have low expression of TEM1. Next, we developed a 78Fc-based tracer and tested its performance in different TEM1-expressing mouse models. The NIR imaging and tomography results suggest that the 78Fc-NIR tracer performs well in distinguishing mouse- or human-TEM1 expressing tumor grafts from normal organs and control grafts in vivo. From these results we conclude that further development and optimization of 78Fc as a TEM1-targeted imaging agent for use in clinical settings is warranted. PMID:25051365

  18. Scalable pumping approach for extracting the maximum TEM(00) solar laser power.

    PubMed

    Liang, Dawei; Almeida, Joana; Vistas, Cláudia R

    2014-10-20

    A scalable TEM(00) solar laser pumping approach is composed of four pairs of first-stage Fresnel lens-folding mirror collectors, four fused-silica secondary concentrators with light guides of rectangular cross-section for radiation homogenization, four hollow two-dimensional compound parabolic concentrators for further concentration of uniform radiations from the light guides to a 3 mm diameter, 76 mm length Nd:YAG rod within four V-shaped pumping cavities. An asymmetric resonator ensures an efficient large-mode matching between pump light and oscillating laser light. Laser power of 59.1 W TEM(00) is calculated by ZEMAX and LASCAD numerical analysis, revealing 20 times improvement in brightness figure of merit.

  19. TEM wave propagation in a microstrip line on a substrate of circular segment cross section

    NASA Astrophysics Data System (ADS)

    Malits, P.; Haridim, M.; Chulski, S.

    2015-12-01

    TEM mode wave propagation in a microstrip transmission line on a dielectric substrate of circular segment cross section is of concern. A suggested design of a microstrip is convenient for manufacturing and allows to miniaturize microstrips since there is no lateral fringing effect of the substrate in the transmitted fundamental TEM mode. By using the bipolar orthogonal coordinates, the plane potential problem is reformulated in the form of trigonometric dual integral equations. The discontinuous integrals containing Legendre functions of complex degree and the Abel integral equation are employed to reduce the dual equations to a Fredholm equation of the second kind. The structure of the Fredholm integral equation allows to obtain a simple approximate solution. Basing on this solution, rigorous approximate formulas for the characteristic impedance are derived. The characteristic impedance of a microstrip transmission line on a silicon substrate is computed and plotted as an example.

  20. TEM identification of subsurface phases in ternary U-Pu-Zr fuel

    NASA Astrophysics Data System (ADS)

    Aitkaliyeva, Assel; Madden, James W.; Papesch, Cynthia A.; Cole, James I.

    2016-05-01

    Phases and microstructure in as-cast, annealed at 850 °C, and subsequently cooled U-23Pu-9Zr fuel were characterized using scanning and transmission electron microscopy techniques. SEM examination shows formation of three phases in the alloy that were identified in TEM using selective area diffraction pattern analysis: α-Zr globular and elongated δ-UZr2 inclusions and a thick oxide layer formed on top of β-Pu phase, which has been initially assumed to be ζ-(U, Pu). However, further examination of the cross-sectional TEM specimens identified the matrix phases as δ-UZr2, β-Pu, and (U, Zr)ht. Two types of inclusions were observed in the immediate vicinity of the specimen surface and they were consistent with α-Zr and ζ-(U, Pu).

  1. Particle size determination using TEM: a discussion of image acquisition and analysis for the novice microscopist.

    PubMed

    Pyrz, William D; Buttrey, Douglas J

    2008-10-21

    As nanoparticle synthesis capabilities advance, there is an increasing need for reliable nanoparticle size distribution analysis. Transmission electron microscopy (TEM) can be used to directly image nanoparticles at scales approaching a single atom. However, the advantage gained by being able to "see" these nanoparticles comes with several tradeoffs that must be addressed and balanced. For effective nanoparticle characterization, the proper selection of imaging type (bright vs dark field), magnification, and analysis method (manual vs automated) is critical. These decisions control the measurement resolution, the contrast between the particle and background, the number of particles in each image, the subsequent analysis efficiency, and the proper determination of the particle-background boundary and affect the significance of electron beam damage to the sample. In this work, the relationship between the critical decisions required for TEM analysis of small nanoparticles and the statistical effects of these factors on the resulting size distribution is presented.

  2. Direct observation of catalytic oxidation of particulate matter using in situ TEM.

    PubMed

    Kamatani, Kohei; Higuchi, Kimitaka; Yamamoto, Yuta; Arai, Shigeo; Tanaka, Nobuo; Ogura, Masaru

    2015-07-08

    The ability to observe chemical reactions at the molecular level convincingly demonstrates the physical and chemical phenomena occurring throughout a reaction mechanism. Videos obtained through in situ transmission electron microscopy (TEM) revealed the oxidation of catalytic soot under practical reaction conditions. Carbon oxidation reactions using Ag/SiO2 or Cs2CO3/nepheline catalysts were performed at 330 °C under an O2 flow of 0.5 Pa in the TEM measurement chamber. Ag/SiO2 catalyzed the reaction at the interface of the mobile Ag species and carbon, while the Cs species was fixed on the nepheline surface during the reaction. In the latter case, carbon particles moved, remained attached to the Cs2CO3/nepheline surface, and were consumed at the interface by the oxidation reaction. Using this technique, we were able to visualize such mobile and immobile catalysis according to different mechanisms.

  3. A TEM-horn antenna with dielectric lens for fast impulse response

    SciTech Connect

    Aurand, J.F.

    1995-12-31

    We designed and constructed a pair of TEM-horn antennas specifically for the very fast time-domain boresight response. Two physical topologies were made. A printed-board configuration has much slower transient response, which we think is due to pulse-smearing of the antenna currents in the dielectric substrate of the printed wiring boards. The solid state version has a 20 ps transition duration response in the main beam endfire (boresight) direction, which is the fastest we have seen to date. And since the antenna has a round trip antenna current propagation time of 6 ns, it offers clean radiated electromagnetic field measurement capability with a clear time of several nanoseconds. The printed board version has resistive loading at the aperture end of the conductors, which should offer better low- frequency performance. The dielectric lens certainly does improve the transient performance of the TEM horn, and was simple to design.

  4. Theoretical analysis and modeling of Thickness-Expansion Mode (TEM) sensors for fluid characterization.

    PubMed

    Elvira, Luis; Resa, Pablo; Castro, Pedro

    2013-03-01

    In this paper, the principles of Thickness-Expansion Mode (TEM) resonators for the characterization of fluids are described. From the measurement of the resonance parameters of a TEM piezoelectric transducer, the compressional acoustic impedance of gases and liquids can be determined. Since the propagation of mechanical waves into the fluid is not necessary, information in a wide range of frequencies can be obtained. Alternatively, these sensors can be driven in combination with other ultrasonic techniques to simultaneously determine the density, speed of sound and viscosity of samples. Some potential applications include the probe monitoring of processes and the characterization of fluids under harsh conditions. The main experimental criteria for the design and construction of high-resolution impedance meters (such as piezoelectric material, protective coating or thermal response) have been studied using equivalent electrical circuit modeling and finite element analysis. PMID:23206416

  5. Direct observation of catalytic oxidation of particulate matter using in situ TEM

    PubMed Central

    Kamatani, Kohei; Higuchi, Kimitaka; Yamamoto, Yuta; Arai, Shigeo; Tanaka, Nobuo; Ogura, Masaru

    2015-01-01

    The ability to observe chemical reactions at the molecular level convincingly demonstrates the physical and chemical phenomena occurring throughout a reaction mechanism. Videos obtained through in situ transmission electron microscopy (TEM) revealed the oxidation of catalytic soot under practical reaction conditions. Carbon oxidation reactions using Ag/SiO2 or Cs2CO3/nepheline catalysts were performed at 330 °C under an O2 flow of 0.5 Pa in the TEM measurement chamber. Ag/SiO2 catalyzed the reaction at the interface of the mobile Ag species and carbon, while the Cs species was fixed on the nepheline surface during the reaction. In the latter case, carbon particles moved, remained attached to the Cs2CO3/nepheline surface, and were consumed at the interface by the oxidation reaction. Using this technique, we were able to visualize such mobile and immobile catalysis according to different mechanisms. PMID:26154580

  6. Analytical study of raw Swarna Makshika (Chalcopyrite) and its Bhasma through TEM and EDAX.

    PubMed

    Mohapatra, Sudhaldev; Jha, Chandra Bhushan

    2013-04-01

    Ayurveda, the Indian System of Medicine deals with a number of metals and minerals. Swarna Makshika (SM), a chalcopyrite one such minerals has iron (Fe), copper (Cu), and sulphur (S) as major ingredients along with other trace elements of therapeutic importance. Studies related with characterization of SM are very few. In the current study SM and SM Bhasma were analysed through Transmission Electron Microscope (TEM) and Energy Dispersive X-Ray Analysis (EDAX). Analysis reveals the presence of iron, copper, and sulphur in SM. In addition to these elements, SM Bhasma found to contain Potassium, Magnesium, Aluminum, and Silicon in trace amount. TEM study reveals that, grain size of the SM (5-10 microns) is significantly reduced in SM Bhasma to 50-200 nm.

  7. Analytical study of raw Swarna Makshika (Chalcopyrite) and its Bhasma through TEM and EDAX

    PubMed Central

    Mohapatra, Sudhaldev; Jha, Chandra Bhushan

    2013-01-01

    Ayurveda, the Indian System of Medicine deals with a number of metals and minerals. Swarna Makshika (SM), a chalcopyrite one such minerals has iron (Fe), copper (Cu), and sulphur (S) as major ingredients along with other trace elements of therapeutic importance. Studies related with characterization of SM are very few. In the current study SM and SM Bhasma were analysed through Transmission Electron Microscope (TEM) and Energy Dispersive X-Ray Analysis (EDAX). Analysis reveals the presence of iron, copper, and sulphur in SM. In addition to these elements, SM Bhasma found to contain Potassium, Magnesium, Aluminum, and Silicon in trace amount. TEM study reveals that, grain size of the SM (5-10 microns) is significantly reduced in SM Bhasma to 50-200 nm. PMID:24250132

  8. Real-Time XRD Studies of Li-O2 Electrochemical Reaction in Nonaqueous Lithium-Oxygen Battery.

    PubMed

    Lim, Hyunseob; Yilmaz, Eda; Byon, Hye Ryung

    2012-11-01

    Understanding of electrochemical process in rechargeable Li-O2 battery has suffered from lack of proper analytical tool, especially related to the identification of chemical species and number of electrons involved in the discharge/recharge process. Here we present a simple and straightforward analytical method for simultaneously attaining chemical and quantified information of Li2O2 (discharge product) and byproducts using in situ XRD measurement. By real-time monitoring of solid-state Li2O2 peak area, the accurate efficiency of Li2O2 formation and the number of electrons can be evaluated during full discharge. Furthermore, by observation of sequential area change of Li2O2 peak during recharge, we found nonlinearity of Li2O2 decomposition rate for the first time in ether-based electrolyte. PMID:26296031

  9. Spectral Resolution for Five-Element, Filtered, X-Ray Detector (XRD) Arrays Using the Methods of Backus and Gilbert

    SciTech Connect

    FEHL,DAVID LEE; BIGGS,F.; CHANDLER,GORDON A.; STYGAR,WILLIAM A.

    2000-01-17

    The generalized method of Backus and Gilbert (BG) is described and applied to the inverse problem of obtaining spectra from a 5-channel, filtered array of x-ray detectors (XRD's). This diagnostic is routinely fielded on the Z facility at Sandia National Laboratories to study soft x-ray photons ({le}2300 eV), emitted by high density Z-pinch plasmas. The BG method defines spectral resolution limits on the system of response functions that are in good agreement with the unfold method currently in use. The resolution so defined is independent of the source spectrum. For noise-free, simulated data the BG approximating function is also in reasonable agreement with the source spectrum (150 eV black-body) and the unfold. This function may be used as an initial trial function for iterative methods or a regularization model.

  10. Reciprocal space XRD mapping with varied incident angle as a probe of structure variation within surface depth

    SciTech Connect

    Yang, Qiguang; Williams, Frances; Zhao, Xin; Reece, Charles E.; Krishnan, Mahadevan

    2013-09-01

    In this study, we used a differential-depth X-Ray diffraction Reciprocal Spacing Mapping (XRD RSM) technique to investigate the crystal quality of a variety of SRF-relevant Nb film and bulk materials. By choosing different X-ray probing depths, the RSM study successfully revealed evolution the of materials microstructure after different materials processes, such as energetic condensation or surface polishing. The RSM data clearly measured the materials crystal quality at different thickness. Through a novel differential-depth RSM technique, this study found: I. for a heteroepitaxy Nb film Nb(100)/MgO(100), the film thickening process, via a cathodic arc-discharge Nb ion deposition, created a near-perfect single crystal Nb on the surfaces top-layer; II. for a mechanically polished single-crystal bulk Nb material, the microstructure on the top surface layer is more disordered than that in-grain.

  11. Characterization of minerals in air dust particles in the state of Tamilnadu, India through FTIR, XRD and SEM analyses

    NASA Astrophysics Data System (ADS)

    Senthil Kumar, R.; Rajkumar, P.

    2014-11-01

    The abstract of this paper explains the presence of minerals in air which causes great concern regarding public health issues. The spectroscopic investigation of air dust particles of several samples in various locations in the state of Tamilnadu, India is reported. Qualitative analyses were carried out to determine the major and minor constituent minerals present in the samples based on the FTIR, XRD absorption peaks. This study also identified the minerals like quartz, asbestos, kaolinite, calcite, hematite, montmorillonite, nacrite and several other trace minerals in the air dust particles. The presents of quartz is mainly found in all the samples invariably. Hence the percentage of quartz and its crystalline nature were determined with the help of extinction co-efficient and crystallinity index respectively. The shape and size of the particulates are studied with SEM analysis.

  12. Real-Time XRD Studies of Li-O2 Electrochemical Reaction in Nonaqueous Lithium-Oxygen Battery.

    PubMed

    Lim, Hyunseob; Yilmaz, Eda; Byon, Hye Ryung

    2012-11-01

    Understanding of electrochemical process in rechargeable Li-O2 battery has suffered from lack of proper analytical tool, especially related to the identification of chemical species and number of electrons involved in the discharge/recharge process. Here we present a simple and straightforward analytical method for simultaneously attaining chemical and quantified information of Li2O2 (discharge product) and byproducts using in situ XRD measurement. By real-time monitoring of solid-state Li2O2 peak area, the accurate efficiency of Li2O2 formation and the number of electrons can be evaluated during full discharge. Furthermore, by observation of sequential area change of Li2O2 peak during recharge, we found nonlinearity of Li2O2 decomposition rate for the first time in ether-based electrolyte.

  13. InP sample preparation for the TEM by photochemical etching, ion milling, and chemical thinning.

    PubMed

    Lowes, T D; Cassidy, D T

    1992-11-01

    Photochemical etching (PCE) as a method for preparation of InP semiconductor plan view samples for the transmission electron microscope is demonstrated and compared to the methods of ion milling and chemical thinning. PCE can produce small area samples for TEM analysis quickly and accurately. Also, the resulting thin regions are surrounded by a built-in stabilizing structure that improves handleability and reduces the occurrence of handling induced fracture.

  14. Experimental Space Weathering of Ordinary Chondrites by Nanopulse Laser: TEM Results

    NASA Technical Reports Server (NTRS)

    Noble, S. K.; Hiroi, T.; Keller, L. P.; Pieters, C. M.

    2011-01-01

    A set of ordinary chondrite meteorites has been subjected to artificial space weathering by nanopulse laser to simulate the effects of micrometeorite bombardment. Three meteorites, an H (Ehole), L (Chateau Renard - CR), and LL (Appley Bridge - AB) were lasered following the method of Sasaki et al [1]. Near IR spectra were taken before and after exposure to examine the optical changes induced and the samples were examined by scanning and transmission electron microscopy (SEM and TEM) to understand the physical changes.

  15. Thermal stress induced voids in nanoscale copper interconnects by in-situ TEM heating

    NASA Astrophysics Data System (ADS)

    An, Jin Ho

    Stress induced void formation in Cu interconnects, due to thermal stresses generated during the processing of semiconductors, is an increasing reliability issue in the semiconductor industry as Cu interconnects are being downscaled to follow the demand for faster chip speed. In this work, 1.8 micron and 180 nm wide Cu interconnects, fabricated by Freescale Semiconductors, were subjected to thermal cycles, in-situ in the TEM, to investigate the stress relaxation mechanisms as a function of interconnect linewidth. The experiments show that the 1.8 micron Cu interconnect lines relax the thermal stresses through dislocation nucleation and motion while the Cu interconnect 180 nm lines exhibit void formation. Void formation in 180 nm lines occurs predominantly at triple junctions where the Ta diffusion barrier meets a Cu grain boundary. In order to understand void formation in 180 nm lines, the grain orientation and local stresses are determined. In particular, Nanobeam Diffraction (NBD) in the TEM is used to obtain the diffraction pattern of each grain, from which the crystal orientation is evaluated by the ACT (Automated Crystallography for TEM) software. In addition, 2D Finite Element Method (FEM) simulations are performed using the Object Oriented Finite Modeling (OOF2) software to correlate grain orientation with local stresses, and consequently void formation. According to the experimental and simulation results obtained, void formation in 180nm Cu interconnects does not seem to be solely dependent on local stresses, but a combination of diffusion paths available, stress gradients and possibly the presence of defects. In addition, based on the in-situ TEM observations, void growth seems to occur through grain boundary and/or interfacial diffusion. However, in-situ STEM observations of fully opened voids post-failure show pileup of material at the Cu grain surfaces. This means that surface or interface diffusion is also very active during void growth in the presence

  16. Spotiton: A prototype for an integrated inkjet dispense and vitrification system for cryo-TEM

    PubMed Central

    Jain, Tilak; Sheehan, Patrick; Crum, John; Carragher, Bridget; Potter, Clinton S.

    2012-01-01

    Over the last three decades, Cryo-TEM has developed into a powerful technique for high-resolution imaging of biological macromolecules in their native vitrified state. However, the technique for vitrifying specimens onto EM grids is essentially unchanged – application of ~ 3 µL sample to a grid, followed by blotting and rapid plunge freezing into liquid ethane. Several trials are often required to obtain suitable thin (few hundred nanometers or less) vitrified layers amenable for cryo-TEM imaging, which results in waste of precious sample and resources. While commercially available instruments provide some level of automation to control the vitrification process in an effort to increase quality and reproducibility, obtaining satisfactory vitrified specimens remains a bottleneck in the Cryo-TEM pipeline. We describe here a completely novel method for EM specimen preparation based on small volume (picoliter to nanoliter) dispensing using inkjet technology. A first prototype system (Spotiton v0.5) demonstrates feasibility of this new approach for specimen vitrification. A piezo-electric inkjet dispenser is integrated with optical real-time cameras (100 Hz frame rate) to analyze picoliter to nanoliter droplet profiles in-flight and spreading dynamics on the grid, and thus provides a method to optimize timing of the process. Using TEM imaging and biochemical assays we demonstrate that the piezo-electric inkjet mechanism does not disrupt the structural or functional integrity of macromolecules. These preliminary studies provide insight into the factors and components that will need further development to enable a robust and repeatable technique for specimen vitrification using this novel approach. PMID:22569522

  17. TEM and HRXRD Analysis of LP MOVPE Grown InGaP/GaAs epilayers

    SciTech Connect

    Pelosi, Claudio; Bosi, Matteo; Attolini, Giovanni; Germini, Fabrizio; Frigeri, Cesare; Prutskij, Tatiana

    2007-04-10

    The diffusion phenomena at interfaces between GaAs/InGaP layers grown by low pressure MOVPE have been studied by dark field (DF) transmission Electron Microscopy (TEM) and High resolution X-ray Diffractometry (HRXRD). By comparing the results of the two techniques a mismatched layer containing P or P and In has been evidenced. The causes of this behavior are briefly discussed.

  18. TEM00 terawatt amplification by use of micro-optic spatial mode conversion.

    PubMed

    DiChiara, Anthony; Chowdhury, Enam A; Ongadi, George; Walker, Barry C; Tamosaitis, Robert S

    2003-11-01

    Micro-optic technology is used in a terawatt multipass Ti:sapphire amplifier to convert high-multimode, 532-nm radiation from an unstable resonator Nd:YAG laser into a TEM00 amplified output without sacrificing the amplifier-to-pump energy conversion efficiency. Experimental measurements and Fourier analysis of the spatial mode show a 3.8-fold increase in the peak irradiance and an order-of-magnitude improvement in the spatial contrast. PMID:14587830

  19. Comparison of preparation techniques for nuclear materials for transmission electron microscopy (TEM)

    SciTech Connect

    Aitkaliyeva, Assel; Madden, James W.; Miller, Brandon D; Cole, James I; Gan, Jian

    2015-04-01

    Preparation of highly radioactive and irradiated nuclear fuels and materials for transmission electron microscopy (TEM) is conjoined with a set of unique challenges, including but not limited to personnel radiation exposure and contamination. The paper evaluates three specimen preparation techniques for preparation of irradiated materials and determines which technique yields to the most reliable characterization of radiation damage microstructure. Various specimen preparation artifacts associated with each technique are considered and ways of minimizing these artifacts are addressed.

  20. Edge-melting: nanoscale key-mechanism to explain nanoparticle formation from heated TEM grids

    NASA Astrophysics Data System (ADS)

    Cesaria, Maura; Taurino, Antonietta; Catalano, Massimo; Caricato, Anna Paola; Martino, Maurizio

    2016-03-01

    In this study, we examine at both experimental and fundamental levels, the experimental evidence of nanoparticle formation in transmission electron microscopy (TEM) metal grids annealed at temperatures lower than the melting point of the corresponding metal bulk material. Our experimental investigation considers the most thermally unstable TEM grids (i.e. Cu-grids) and inspects the possible sources and mechanisms of contamination of thin films, conventionally deposited on carbon-coated Cu-grids. The investigations are supported by morphological-compositional analyses performed in different regions of the TEM sample. Then, a general model is formulated and discussed in order to explain the grid thermal instability, based on the critical role of edge-melting (i.e. melting initiated at edges and corners of the grid bars), the enhanced rate of evaporation from a liquid surface and the polycristallinity of the grid bars. Hence, we totally disregard conventional arguments such as bulk evaporation and metal vapor pressure and, in order to emphasize and clarify the alternative point of view of our model, we also overview the nano-scale melting phenomenology relevant to our discussion and survey the discrepancies reported in the literature.

  1. 2.5 D Transrotational Microcrystals and Nanostructures Revealed by TEM in Crystallizing Amorphous Films

    NASA Astrophysics Data System (ADS)

    Kolosov, Vladimir

    2015-03-01

    Unexpected transrotational microcrystals can be grown in thin 10-100 nm amorphous films. Crystals of different morphology (from nanowhiskers to spherulites, complex textures) and chemical nature (oxides, chalcogenides, metals and alloys) grown in thin films prepared by various methods are studied by transmission electron microscopy (TEM). We use primarily our TEM bend-contour method and SAED (HREM, AFM are also performed). The phenomenon resides in strong (up to 300 degrees/ μm) regular internal bending of crystal lattice planes in a growing crystal. It can be traced inside TEM in situ. Usual translation is complicated by slight regular rotation of the crystal unit cell (transrotation) most prominent at the mesoscale. Different geometries of transrotation of positive and negative curvature are revealed. Transrotational crystal resembles ideal single crystal enclosed in a curved space. It can be also considered similar to hypothetical endless 2.5 D analogy of MW nanotube/nano-onion halves. Transrotation is strongly increasing as the film gets thinner in the range 100-15 nm. Transrotations supplement dislocations and disclinations. New transrotational nanocrystalline model of amorphous state is proposed. Support of Ministry of Higher Education and Science is acknowledged.

  2. Coarsening of Pd nanoparticles in an oxidizing atmosphere studied by in situ TEM

    NASA Astrophysics Data System (ADS)

    Simonsen, Søren Bredmose; Chorkendorff, Ib; Dahl, Søren; Skoglundh, Magnus; Helveg, Stig

    2016-06-01

    The coarsening of supported palladium nanoparticles in an oxidizing atmosphere was studied in situ by means of transmission electron microscopy (TEM). Specifically, the Pd nanoparticles were dispersed on a planar and amorphous Al2O3 support and were observed during the exposure to 10 mbar technical air at 650 °C. Time-resolved TEM image series reveal that the Pd nanoparticles were immobile and that a few percent of the nanoparticles grew or shrank, indicating a coarsening process mediated by the Ostwald ripening mechanism. The TEM image contrast suggests that the largest nanoparticles tended to wet the Al2O3 support to a higher degree than the smaller nanoparticles and that the distribution of projected particle sizes consequently broadens by the appearance of an asymmetric tail toward the larger particle sizes. A comparison with computer simulations based on a simple mean-field model for the Ostwald ripening process indicates that the observed change in the particle size distribution can be accounted for by wetting of the Al2O3 support by the larger Pd nanoparticles.

  3. 3D TEM reconstruction and segmentation process of laminar bio-nanocomposites

    SciTech Connect

    Iturrondobeitia, M. Okariz, A.; Fernandez-Martinez, R.; Jimbert, P.; Guraya, T.; Ibarretxe, J.

    2015-03-30

    The microstructure of laminar bio-nanocomposites (Poly (lactic acid)(PLA)/clay) depends on the amount of clay platelet opening after integration with the polymer matrix and determines the final properties of the material. Transmission electron microscopy (TEM) technique is the only one that can provide a direct observation of the layer dispersion and the degree of exfoliation. However, the orientation of the clay platelets, which affects the final properties, is practically immeasurable from a single 2D TEM image. This issue can be overcome using transmission electron tomography (ET), a technique that allows the complete 3D characterization of the structure, including the measurement of the orientation of clay platelets, their morphology and their 3D distribution. ET involves a 3D reconstruction of the study volume and a subsequent segmentation of the study object. Currently, accurate segmentation is performed manually, which is inefficient and tedious. The aim of this work is to propose an objective/automated segmentation methodology process of a 3D TEM tomography reconstruction. In this method the segmentation threshold is optimized by minimizing the variation of the dimensions of the segmented objects and matching the segmented V{sub clay} (%) and the actual one. The method is first validated using a fictitious set of objects, and then applied on a nanocomposite.

  4. In Situ and Ex Situ TEM Study of Lithiation Behaviours of Porous Silicon Nanostructures

    NASA Astrophysics Data System (ADS)

    Shen, Chenfei; Ge, Mingyuan; Luo, Langli; Fang, Xin; Liu, Yihang; Zhang, Anyi; Rong, Jiepeng; Wang, Chongmin; Zhou, Chongwu

    2016-08-01

    In this work, we study the lithiation behaviours of both porous silicon (Si) nanoparticles and porous Si nanowires by in situ and ex situ transmission electron microscopy (TEM) and compare them with solid Si nanoparticles and nanowires. The in situ TEM observation reveals that the critical fracture diameter of porous Si particles reaches up to 1.52 μm, which is much larger than the previously reported 150 nm for crystalline Si nanoparticles and 870 nm for amorphous Si nanoparticles. After full lithiation, solid Si nanoparticles and nanowires transform to crystalline Li15Si4 phase while porous Si nanoparticles and nanowires transform to amorphous LixSi phase, which is due to the effect of domain size on the stability of Li15Si4 as revealed by the first-principle molecular dynamic simulation. Ex situ TEM characterization is conducted to further investigate the structural evolution of porous and solid Si nanoparticles during the cycling process, which confirms that the porous Si nanoparticles exhibit better capability to suppress pore evolution than solid Si nanoparticles. The investigation of structural evolution and phase transition of porous Si nanoparticles and nanowires during the lithiation process reveal that they are more desirable as lithium-ion battery anode materials than solid Si nanoparticles and nanowires.

  5. In Situ and Ex Situ TEM Study of Lithiation Behaviours of Porous Silicon Nanostructures.

    PubMed

    Shen, Chenfei; Ge, Mingyuan; Luo, Langli; Fang, Xin; Liu, Yihang; Zhang, Anyi; Rong, Jiepeng; Wang, Chongmin; Zhou, Chongwu

    2016-08-30

    In this work, we study the lithiation behaviours of both porous silicon (Si) nanoparticles and porous Si nanowires by in situ and ex situ transmission electron microscopy (TEM) and compare them with solid Si nanoparticles and nanowires. The in situ TEM observation reveals that the critical fracture diameter of porous Si particles reaches up to 1.52 μm, which is much larger than the previously reported 150 nm for crystalline Si nanoparticles and 870 nm for amorphous Si nanoparticles. After full lithiation, solid Si nanoparticles and nanowires transform to crystalline Li15Si4 phase while porous Si nanoparticles and nanowires transform to amorphous LixSi phase, which is due to the effect of domain size on the stability of Li15Si4 as revealed by the first-principle molecular dynamic simulation. Ex situ TEM characterization is conducted to further investigate the structural evolution of porous and solid Si nanoparticles during the cycling process, which confirms that the porous Si nanoparticles exhibit better capability to suppress pore evolution than solid Si nanoparticles. The investigation of structural evolution and phase transition of porous Si nanoparticles and nanowires during the lithiation process reveal that they are more desirable as lithium-ion battery anode materials than solid Si nanoparticles and nanowires.

  6. In Situ and Ex Situ TEM Study of Lithiation Behaviours of Porous Silicon Nanostructures

    PubMed Central

    Shen, Chenfei; Ge, Mingyuan; Luo, Langli; Fang, Xin; Liu, Yihang; Zhang, Anyi; Rong, Jiepeng; Wang, Chongmin; Zhou, Chongwu

    2016-01-01

    In this work, we study the lithiation behaviours of both porous silicon (Si) nanoparticles and porous Si nanowires by in situ and ex situ transmission electron microscopy (TEM) and compare them with solid Si nanoparticles and nanowires. The in situ TEM observation reveals that the critical fracture diameter of porous Si particles reaches up to 1.52 μm, which is much larger than the previously reported 150 nm for crystalline Si nanoparticles and 870 nm for amorphous Si nanoparticles. After full lithiation, solid Si nanoparticles and nanowires transform to crystalline Li15Si4 phase while porous Si nanoparticles and nanowires transform to amorphous LixSi phase, which is due to the effect of domain size on the stability of Li15Si4 as revealed by the first-principle molecular dynamic simulation. Ex situ TEM characterization is conducted to further investigate the structural evolution of porous and solid Si nanoparticles during the cycling process, which confirms that the porous Si nanoparticles exhibit better capability to suppress pore evolution than solid Si nanoparticles. The investigation of structural evolution and phase transition of porous Si nanoparticles and nanowires during the lithiation process reveal that they are more desirable as lithium-ion battery anode materials than solid Si nanoparticles and nanowires. PMID:27571919

  7. Differential Dependence on N-Glycosylation of Anthrax Toxin Receptors CMG2 and TEM8

    PubMed Central

    Friebe, Sarah; Deuquet, Julie; van der Goot, F. Gisou

    2015-01-01

    ANTXR 1 and 2, also known as TEM8 and CMG2, are two type I membrane proteins, which have been extensively studied for their role as anthrax toxin receptors, but with a still elusive physiological function. Here we have analyzed the importance of N-glycosylation on folding, trafficking and ligand binding of these closely related proteins. We find that TEM8 has a stringent dependence on N-glycosylation. The presence of at least one glycan on each of its two extracellular domains, the vWA and Ig-like domains, is indeed necessary for efficient trafficking to the cell surface. In the absence of any N-linked glycans, TEM8 fails to fold correctly and is recognized by the ER quality control machinery. Expression of N-glycosylation mutants reveals that CMG2 is less vulnerable to sugar loss. The absence of N-linked glycans in one of the extracellular domains indeed has little impact on folding, trafficking or receptor function of the wild type protein expressed in tissue culture cells. N-glycans do, however, seem required in primary fibroblasts from human patients. Here, the presence of N-linked sugars increases the tolerance to mutations in cmg2 causing the rare genetic disease Hyaline Fibromatosis Syndrome. It thus appears that CMG2 glycosylation provides a buffer towards genetic variation by promoting folding of the protein in the ER lumen. PMID:25781883

  8. In Situ and Ex Situ TEM Study of Lithiation Behaviours of Porous Silicon Nanostructures.

    PubMed

    Shen, Chenfei; Ge, Mingyuan; Luo, Langli; Fang, Xin; Liu, Yihang; Zhang, Anyi; Rong, Jiepeng; Wang, Chongmin; Zhou, Chongwu

    2016-01-01

    In this work, we study the lithiation behaviours of both porous silicon (Si) nanoparticles and porous Si nanowires by in situ and ex situ transmission electron microscopy (TEM) and compare them with solid Si nanoparticles and nanowires. The in situ TEM observation reveals that the critical fracture diameter of porous Si particles reaches up to 1.52 μm, which is much larger than the previously reported 150 nm for crystalline Si nanoparticles and 870 nm for amorphous Si nanoparticles. After full lithiation, solid Si nanoparticles and nanowires transform to crystalline Li15Si4 phase while porous Si nanoparticles and nanowires transform to amorphous LixSi phase, which is due to the effect of domain size on the stability of Li15Si4 as revealed by the first-principle molecular dynamic simulation. Ex situ TEM characterization is conducted to further investigate the structural evolution of porous and solid Si nanoparticles during the cycling process, which confirms that the porous Si nanoparticles exhibit better capability to suppress pore evolution than solid Si nanoparticles. The investigation of structural evolution and phase transition of porous Si nanoparticles and nanowires during the lithiation process reveal that they are more desirable as lithium-ion battery anode materials than solid Si nanoparticles and nanowires. PMID:27571919

  9. The Morgagnian and Brunescens cataract morphology studied with with SEM and TEM.

    PubMed

    Jongebloed, W L; Kalicharan, D; Los, L I; Worst, J G

    1993-01-01

    The Morgagnian cataract lenses--pre-fixed with GA for SEM & TEM and post-fixed with tannic-acid-arginine-OsO4 for SEM and OsO4/K4Fe(CN)6 for TEM after staining with Ur-acetate/Pb-citrate--showed areas in the cortex with radial instead of concentric running lens fibres, degeneration of lens fibres with vacuoles and defected "ball & socket" connections. The presence of oval/spherical bodies of 0.5-20 microns was acknowledged, the largest of them having a golf-ball appearance and originating from the cytoplasm of the degenerating lens fibres; the smallest of them with an approximate size of 0.2-0.5 micron seemed to be formed by budding off from the microvilli of the furrowed lens epithelium. The Brunescens cataract lenses showed at low magnification no difference between lens fibres from the cortical area and the nucleus. The disintegration process of the lens fibres was observable as degradation of the ball & socket system and the existence of holes in the lens fibre body and emerging of spherical bodies from the cytoplasm. The globular structures seemed to be covered with a thin coating and were partly filled with a low density membranous-like material. In TEM-sections of the cataractous lens aterial vacuoles were visible consisting of a large number of smaller globules with a contents of low contrast low density membranous-like material, comparable with the globular structures seen in SEM.

  10. Novel Transrotational Solid State Order Discovered by TEM in Crystallizing Amorphous Films

    NASA Astrophysics Data System (ADS)

    Kolosov, Vladimir

    Exotic thin crystals with unexpected transrotational microstructures have been discovered by transmission electron microscopy (TEM) for crystal growth in thin (10-100 nm) amorphous films of different chemical nature (oxides, chalcogenides, metals and alloys) prepared by various methods. Primarily we use our TEM bend contour technique. The unusual phenomenon can be traced in situ in TEM column: dislocation independent regular internal bending of crystal lattice planes in a growing crystal. Such transrotation (unit cell trans lation is complicated by small rotationrealized round an axis lying in the film plane) can result in strong regular lattice orientation gradients (up to 300 degrees per micrometer) of different geometries: cylindrical, ellipsoidal, toroidal, saddle, etc. Transrotation is increasing as the film gets thinner. Transrotational crystal resembles ideal single crystal enclosed in a curved space. Transrotational micro crystals have been eventually recognized by other authors in some vital thin film materials, i.e. PCMs for memory, silicides, SrTiO3. Atomic model and possible mechanisms of the phenomenon are discussed. New transrotational nanocrystalline model of amorphous state is also proposed Support of RF Ministry of Education and Science is acknowledged.

  11. Validation of the gyrokinetic model in ITG and TEM dominated L-mode plasmas

    NASA Astrophysics Data System (ADS)

    Howard, N. T.; White, A. E.; Reinke, M. L.; Greenwald, M.; Holland, C.; Candy, J.; Walk, J. R.

    2013-12-01

    A rigorous validation of the gyrokinetic model was performed in both ion temperature gradient (ITG) and trapped electron mode (TEM) dominated Alcator C-Mod plasmas at (normalized midplane minor radius) r/a = 0.5 and 0.8. Analysis focuses on two L-mode discharges operated with 1.2 and 3.5 MW of ion cyclotron resonance heating. In depth investigation into the experimental uncertainties and simulation sensitivities in these discharges allows for a stringent test of the gyrokinetic model implemented by the GYRO code (Candy and Waltz 2003 J. Comput. Phys. 186 545) in both the centre of the stiff gradient region (r/a = 0.5) and the middle of the region often associated with the transport ‘shortfall’(r/a = 0.8). To identify the nature of the plasma turbulence and to ensure a robust evaluation of the model's ability to reproduce experiment, the sensitivity of the simulation results to experimental uncertainty in turbulence drive and suppression terms were determined at both radial locations. When significant TEM activity is present, nonlinear gyrokinetic simulations are found to reproduce both electron and ion experimental heat fluxes within their diagnosed uncertainties. In contrast, in the absence of TEM, electron heat fluxes are robustly under predicted by low-k, gyrokinetic simulation.

  12. Constraints on the Thermal History of Martian Meteorites ALH84001 and MIL03346 by Single Crystal XRD, Electron Microprobe and Mössbauer Analyses of Ortho- and Clinopyroxene

    NASA Astrophysics Data System (ADS)

    Domeneghetti, M. C.; Fioretti, A. M.; Cámara, F.; Carraro, A.; McCammon, C.; Tazzoli, V.

    2007-07-01

    Constraints on the thermal history of meteorites can be established by estimating the Fe2+-Mg order degree in their pyroxene using single-crystal XRD. We present here the data obtained on martian meteorites ALH84001 and MIL03346.

  13. The importance of XRD analysis in provenance and palaeoenvironmental studies of the Piedras de Afilar Formation, Neoproterozoic of Uruguay

    NASA Astrophysics Data System (ADS)

    Pamoukaghlian, K.; Poiré, D. G.; Gaucher, C.; Uriz, N.; Cingolani, C.; Frigeiro, P.

    2009-04-01

    The Piedras de Afilar Formation crops out in the southeast part of Uruguay, forming part of the Tandilia Terrane (sensu Bossi et al. 2005). Pamoukaghlian et al. (2006) and Gaucher et al. (2008) have published δ13C, δ18O and U/Pb SHRIMP results, which indicate a Neoproterozoic age for this formation. The palaeoenvironment has been defined as a shallow marine platform based on the presence of interference ripples, hummocky and mega-hummocky cross-stratification. X-ray diffraction (XRD) analyses help to better constrain the palaeoenvironment: the presence of chlorite/smectite found in black shales, suggest a reducing environment, and abundant illite indicates a cold to temperate climate. Provenance studies have been undertaken that utilise a combination of detailed palaeocurrent measurements, petrographic descriptions, XRD analyses, and geochemical isotopic analyses, including U/Pb SHRIMP determinations. Mineral compositional diagrams for sandstones suggest a stable cratonic provenance. Palaeocurrents are mainly from the NNE, indicating a provenance from the cratonic areas of the Tandilia Terrane. The illite crystal index indicates diagenetic to low-metamorphic conditions for the sequence; this is important to confirm that the identified minerals are authigenic. Clay minerals identified by XRD analysis of sandstones from the siliciclastic member are illite (80 - 90%), kaolinite (5 - 10%), and chlorite (5 - 10%). This is consistent with a provenance from the cratonic areas (quartz-feldspar dominated rock types). Isotopic analyses have been undertaken to provide better constraints on the tectonic setting. U/Pb SHRIMP ages for the youngest zircons are 990 Ma (Gaucher et al. 2008), and the basal granite (Granito de la Paz) is 2056 ± 11 Ma (Hartmann et al. 2001), suggesting a provenance from the Archaean basement for the Piedras de Afilar Formation, like its counterparts in the Rio de la Plata Craton. References Bossi, J., Piñeyro, D., Cingolani, C. (2005). El l

  14. A complex mutant of TEM-1 beta-lactamase with mutations encountered in both IRT-4 and extended-spectrum TEM-15, produced by an Escherichia coli clinical isolate.

    PubMed Central

    Sirot, D; Recule, C; Chaibi, E B; Bret, L; Croize, J; Chanal-Claris, C; Labia, R; Sirot, J

    1997-01-01

    Escherichia coli GR102 was isolated from feces of a leukemic patient. It expressed different levels of resistance to amoxicillin or ticarcillin plus clavulanate and to the various cephalosporins tested. The double-disk synergy test was weakly positive. Production of a beta-lactamase with a pI of 5.6 was transferred to E. coli HB101 by conjugation. The nucleotide sequence was determined by direct sequencing of the amplification products obtained by PCR performed with TEM gene primers. This enzyme differed from TEM-1 (blaT-1B gene) by four amino acid substitutions: Met-->Leu-69, Glu-->Lys-104, Gly-->Ser-238 and Asn-->Asp-276. The amino acid susbstitutions Leu-69 and Asp-276 are known to be responsible for inhibitor resistance of the IRT-4 mutant, as are Lys-104 and Ser-238 substitutions for hydrolytic activity of the extended-spectrum beta-lactamases TEM-15, TEM-4, and TEM-3. These combined mutations led to a mutant enzyme which conferred a level of resistance to coamoxiclav (MIC, 64 microg/ml) much lower than that conferred by IRT-4 (MIC, 2,048 microg/ml) but higher than that conferred by TEM-15 or TEM-1 (MIC, 16 microg/ml). In addition, the MIC of ceftazidime for E. coli transconjugant GR202 (1 microg/ml) was lower than that for E. coli TEM-15 (16 microg/ml) and higher than that for E. coli IRT-4 or TEM-1 (0.06 microg/ml). The MICs observed for this TEM-type enzyme were related to the kinetic constants Km and k(cat) and the 50% inhibitory concentration, which were intermediate between those observed for IRT-4 and TEM-15. In conclusion, this new type of complex mutant derived from TEM-1 (CMT-1) is able to confer resistance at a very low level to inhibitors and at a low level to extended-spectrum cephalosporins. CMT-1 received the designation TEM-50. PMID:9174192

  15. Weathering and hydrothermal alteration of basalts in Iceland: mineralogy from VNIR, TIR, XRD, and implications for Mars

    NASA Astrophysics Data System (ADS)

    Ehlmann, B. L.; Mustard, J. F.; Bish, D. L.

    2009-12-01

    thomsonite, basalts with silica/quartz-bearing veins, basalts bearing celadonite, and basalts partially altered to montmorillonite, Fe/Mg smectite, or mixed smectite-chlorite. Analyses included: (1) measurement of reflectance spectra of the whole rock by the ASD; (2) measurement of VNIR and TIR spectra in RELAB of particle-size separates (<25um and <125um) derived from the bulk rock and from precipitated minerals extracted from the vesicles; (3) measurement of X-ray diffraction (XRD) patterns, including quantitative XRD; and (4) electron microprobe chemical analyses. These data emulate orbital data from CRISM, OMEGA, and TES, which detect the infrared active components, linked to in-situ data on whole rock modal mineralogy such as will be measured by the ChemMin instrument on the MSL rover.

  16. Soot Precursor Material: Visualization Via Simultaneous LIF-LII and Characterization Via TEM

    NASA Technical Reports Server (NTRS)

    VanderWal, Randall L.

    1996-01-01

    Simultaneous combined laser-induced fluorescence and laser-induced incandescence (LIF-LII) images are presented for both a normal and inverse diffusion flame. The excitation wavelength dependence distinguishes the LIF and LII signals in images from the normal diffusion flame while the temporal decay distinguishes the signals in images of the inverse diffusion flame. Each flame presents a minimum in the combined LIF-LII intensity in a region separating the fuel pyrolysis and soot containing regions. Opacity, geometric in definition, and extent of crystallinity measured through both bright and dark field Transmission Electron Microscopy (TEM) characterizes the thermophoretically sampled material from within this minimal LIF-LII intensity region. TEM analysis reveals rather different soot processes occurring within the normal and inverse diffusion flame. In the normal diffusion flame, rapid chemical and physical coalescence of PAHs results in initial formation of soot precursor particles that are highly crystalline and evolve toward fully formed soot. In the inverse diffusion flame, rapid coalescence of pyrolysis products occurs, producing tarlike, globular structures equivalent in size to fully formed soot aggregates but with markedly less crystallinity than normal-appearing soot. These different material properties are interpreted as reflecting different relative rates of chemical and physical coalescence of fuel pyrolysis products versus carbonization. Significantly, these TEM images support qualitative photophysical arguments suggesting that, in general, this 'dark' region observed in the LIF-LII images demarcates a transitional region in which a fundamental change in the material the material chemical/physical properties occurs between solid carbonaceous soot and condensed or gaseous molecular growth material.

  17. Direct observation of ferroelectric domain switching in varying electric field regimes using in situ TEM.

    PubMed

    Winkler, C R; Damodaran, A R; Karthik, J; Martin, L W; Taheri, M L

    2012-11-01

    In situ Transmission Electron Microscopy (TEM) techniques can potentially fill in gaps in the current understanding interfacial phenomena in complex oxides. Select multiferroic oxide materials, such as BiFeO(3) (BFO), exhibit ferroelectric and magnetic order, and the two order parameters are coupled through a quantum-mechanical exchange interaction. The magneto-electric coupling in BFO allows control of the ferroelectric and magnetic domain structures via applied electric fields. Because of these unique properties, BFO and other magneto-electric multiferroics constitute a promising class of materials for incorporation into devices such as high-density ferroelectric and magnetoresistive memories, spin valves, and magnetic field sensors. The magneto-electric coupling in BFO is mediated by volatile ferroelastically switched domains that make it difficult to incorporate this material into devices. To facilitate device integration, an understanding of the microstructural factors that affect ferroelastic relaxation and ferroelectric domain switching must be developed. In this article, a method of viewing ferroelectric (and ferroelastic) domain dynamics using in situ biasing in TEM is presented. The evolution of ferroelastically switched ferroelectric domains in BFO thin films during many switching cycles is investigated. Evidence of partial domain nucleation, propagation, and switching even at applied electric fields below the estimated coercive field is revealed. Our observations indicate that the occurrence of ferroelastic relaxation in switched domains and the stability of these domains is influenced the applied field as well as the BFO microstructure. These biasing experiments provide a real time view of the complex dynamics of domain switching and complement scanning probe techniques. Quantitative information about domain switching under bias in ferroelectric and multiferroic materials can be extracted from in situ TEM to provide a predictive tool for future device

  18. Behaviour of TEM metal grids during in-situ heating experiments.

    PubMed

    Zhang, Zaoli; Su, Dangsheng

    2009-05-01

    The stability of Ni, Cu, Mo and Au transmission electron microscope (TEM) grids coated with ultra-thin amorphous carbon (alpha-C) or silicon monoxide film is examined by in-situ heating up to a temperature in the range 500-850 degrees C in a transmission electron microscope. It is demonstrated that some grids can generate nano-particles either due to the surface diffusion of metal atoms on amorphous film or due to the metal evaporation/redeposition. The emergence of nano-particles can complicate experimental observations, particularly in in-situ heating studies of dynamic behaviours of nano-materials in TEM. The most widely used Cu grid covered with amorphous carbon is unstable, and numerous Cu nano-particles start to form once the heating temperature reaches 600 degrees C. In the case of Ni grid covered with alpha-C film, a large number of Ni nano-crystals occur immediately when the temperature approaches 600 degrees C, accompanied by the graphitization of amorphous carbon. In contrast, both Mo and Au grids covered with alpha-C film exhibit good stability at elevated temperature, for instance, up to 680 and 850 degrees C for Mo and Au, respectively, and any other metal nano-particles are detected. Cu grid covered Si monoxide thin film is stable up to 550 degrees C, but Si nano-crystals appear under intensive electron beam. The generated nano-particles are well characterized by spectroscopic techniques (EDXS/EELS) and high-resolution TEM. The mechanism of nano-particle formation is addressed based on the interactions between the metal grid and the amorphous carbon film and on the sublimation of metal.

  19. Geological Hypothesis Testing and Investigations of Coupling with Transient Electromagnetics (TEM)

    NASA Astrophysics Data System (ADS)

    Adams, A. C.; Moeller, M. M.; Snyder, E.; Workman, E. J.; Urquhart, S.; Bedrosian, P.; Pellerin, L.

    2014-12-01

    Transient electromagnetic (TEM) data were acquired in Borrego Canyon within the Santo Domingo Basin of the Rio Grande Rift, central New Mexico, during the 2014 Summer of Applied Geophysical Experience (SAGE) field program. TEM surveys were carried out in several regions both to investigate geologic structure and to illustrate the effects of coupling to anthropogenic structures. To determine an optimal survey configuration, 50, 100 and 200 m square transmitter loops were deployed; estimates of depth-of-investigation and logistical considerations determined that 50 m loops were sufficient for production-style measurements. A resistive (100s of ohm-m) layer was identified at a depth of 25-75 m at several locations, and interpreted as dismembered parts of one or more concealed volcanic flows, an interpretation consistent with Tertiary volcanic flows that cap the Santa Anna Mesa immediately to the south. TEM soundings were also made across an inferred fault to investigate whether fault offset is accompanied by lateral changes in electrical resistivity. Soundings within several hundred meters of the inferred fault strand were identical, indicating no resistivity contrast across the fault, and possibly an absence of recent activity. An old windmill and water tank, long-abandoned, offered an excellent laboratory to study the effect of coupling to metallic anthropogenic structures. The character of the measured data strongly suggests the water tank is in electrical contact with the earth (galvanic coupling), and an induced response was persistent to more than 1 second after current turn-off. Coupling effects could be identified at least 150 meters from the tank. Understanding the mechanism behind such coupling and the ability to identify coupled data are critical skills, as one-dimensional modeling of data is affected by such coupling producing artificial conductive layers at depth.

  20. Microscopic imaging of resin-bonded dentin using Cryo-FIB/TEM system

    NASA Astrophysics Data System (ADS)

    Bakhsh, Turki A.

    2015-03-01

    Background and Objective: Introduction of focused ion beam (FIB) for transmission electron microscopy (TEM) preparation had enhanced the understanding of materials' interaction at nanoscale. However, this technique generates localized heat that may possibly have some effect on organic/vital structures during preparation of biological tissues. Therefore, the aim of this study was to investigate the effect of milling with Cryogenic-FIB on imaging the ultra-morphological features of dentin-resin interface bonded in a tooth and compare the findings to a room-temperature FIB prepared specimens. Methods: After cylindrical dentin cavities (3 mm diameter × 1.5 mm depth) were prepared on the occlusal surfaces of extracted, non-carious human premolar teeth, they were restored with Filtek P90 (Silorane) restorative system (3M ESPE, USA). To investigate the ultra-morphological features of resin-dentin interface, the bonded specimens were divided into 2 groups based on the preparation technique; (1) FIB preparation at room-temperature (RT), and (2) FIB preparation with cryogenic cooling (Cy). Later, each group was examined under TEM. Results: The obtained sections in RT group showed blurred scattered needle-like crystals above the resin-impregnated dentin. However, the orientation of these crisscross needle-like crystals and the ultramorphological features of the underlying dentin were more vivid and distinct in Cy group. Conclusion: Within the limitation of this in-vitro study, it could be concluded that combining FIB with cryogenic cooling had preserved the biological organic features of dentin due to minimized beam damage. The presented cryogenic technique should be considered in future FIB/TEM studies involving biological substrates. This research was supported by King Abdulaziz University.

  1. First application of time-domain electromagnetic technology (TEM) for permafrost mapping on the Arctic shelf.

    NASA Astrophysics Data System (ADS)

    Koshurnikov, A.; Gunar, A.; Tumskoy, V. E.; Shakhova, N. E.; Semiletov, I. P.; Valuyskiy, S.

    2015-12-01

    Different geophysical methods are used to study and map submarine permafrost on the Arctic Shelf. Due to specific features of submarine permafrost, none of geophysical methods can provide conclusive data when gas-charged sediments and taliks occur within permafrost. Experimental data show that electrical properties of frozen grounds change significantly. For example, depending on ground lithology and wetness, electrical resistivity can increase up to 103 times upon freezing. Thus, electromagnetic methods could be considered more informative and valuable tool for characterizing subsea permafrost. Investigation of submarine permafrost on the shallow Arctic Shelf requires modifications of electromagnetic methods to cover specific needs of working from the fast ice. Winter expeditions devoted to subsea permafrost investigations were performed in March-April of 2012-2015 in the near-shore area of the Laptev Sea. TEM was applied to predict permafrost down to 1 km depth. TEM systems are advantageous when many stations are required, because many short deployments can be performed in a single survey. Working from the fast ice allowed collection of few tens of stations to cover the entire polygon. Interpretation of data collected in 2012 allowed to predict position of the permafrost table near-shore near Muostakh Island, which was validated by followed up permafrost drilling. Surveys performed in 2013-2015 also confirmed good agreement between electromagnetic data and observational data obtained by drilling. Accuracy of the methods reached 3.5%. Note, that in March-April of 2014 and 2015, we used the modified TEM which allows obtaining continuous subsea permafrost table profiles.

  2. High Spatial Resolution Study of Microbe-Carbonate-Silicate Interfaces by FIB and TEM

    NASA Astrophysics Data System (ADS)

    Benzerara, K.; Menguy, N.; Guyot, F.; Vanni, C.; Gillet, P.

    2003-12-01

    High resolution transmission electron microscopy (HRTEM), chemical micro-analysis (EDX) and electron energy loss spectroscopy (EELS) are among the most powerful analytical techniques for studying microbe-mineral interactions, allowing to observe the microbe-mineral interface at almost the angstrom scale, to evidence transformations of the mineral structure and chemical alterations at the nanometer scale. However, the samples must be very thin and only a small area can be investigated. A key limitation for using this technique is thus to prepare natural geomicrobiological samples which combine hard minerals, preventing use of ultramicrotomy, with soft organic matter inadequate to ion milling procedures. Additionaly the areas of interest are usually restricted to few micrometer large areas which have to be selected from macroscopic samples. In this study we present two procedures : micromanipulation and FIB (Focused Ion Beam) which allow the study of microbe-mineral interfaces with TEM. The micromanipulation procedure has been presented in Benzerara et al (2003, PNAS). We have evidenced nannobacteria-like objects at the surface of the Tatahouine orthopyroxenite meteorite fallen in the tunisian desert in 1931. SEM observations suggest a complex interaction pattern between the nannobacteria-like objects, the pyroxene and microorganisms which have colonized the surface of the meteorite during its seventy years of residence on Earth. The TEM study on the very same area shows that the nannobacteria-like rods are actually well-crystallized nanometric calcite single crystals surrounded by an amorphous layer of carbonate composition. Those morphologies and structures are unusual for calcite single crystals. We discuss these observations in regard to the criteria of biogenicity i.e. biosignatures. Moreover, we examine the implications for carbonate production associated to silicate bio-weathering under aridic conditions. This work is relevant both to astrobiological and

  3. Transposition of the gene encoding a TEM-12 extended-spectrum beta-lactamase.

    PubMed Central

    Heritage, J; Hawkey, P M; Todd, N; Lewis, I J

    1992-01-01

    An isolate of Klebsiella oxytoca from the blood culture of a child with leukemia was found to produce two beta-lactamases, at least one of which conferred resistance to ceftazidime. Genes encoding both enzymes were located on a single self-transmissible 100-kb plasmid, pOZ201. This plasmid was introduced into Escherichia coli UB5201 (pACYC184), and the gene encoding one beta-lactamase was transposed onto plasmid pACYC184 by exploiting a gene dosage effect. The transposable gene was found to encode a TEM-12 enzyme as determined by nucleotide sequencing. This gene was subsequently transposed onto plasmid pUB307. The transposable element encoding the TEM-12 enzyme has been designated Tn841. Both plasmids pACYC184::Tn841 and pUB307::Tn841 were shown to encode a beta-lactamase with the same isoelectric point and substrate profile as the TEM-12 beta-lactamase. Transposon Tn841, at approximately 7 kb, is larger than TnA (4.8 kb) and transposes at a lower frequency. Although it produced a resolvase which can complement the resolvase of Tn3, its transposase function was not able to complement the transposition of a TnA element which lacked transposase. The occurrence of a gene encoding an extended-spectrum beta-lactamase on a transposable element in a clinically significant bacterium is potentially a cause for concern for the spread of resistance to the extended-spectrum cephalosporins. PMID:1329636

  4. A Survey of Jet Aircraft PM by TEM in APEX III

    NASA Technical Reports Server (NTRS)

    VanderWal, Randy L.; Bryg, Victoria M.

    2014-01-01

    Based upon field testing during the NASA led APEX III campaign conducted in November 2005 at the NASA Glenn Research Center in coordination with Continental Airlines and Cleveland Hopkins International Airport. This paper reports observations of particulate emissions collected from a suite of jet engine aircraft to assess differences and similarities in soot macro- micro- and nanostructure using transmission electron microscopy (TEM). Aggregates are compact, primary particle sizes varied and nanostructure mixed. Comparisons are made to more familiar laboratory flame-generated soot as a well-studied point of reference. Results are interpreted in terms of turbulence interacting with the different stages of particle formation and growth.

  5. In Situ Laser Synthesis of Si Nanowires in the Dynamic TEM

    SciTech Connect

    Taheri, M; Reed, B; LaGrange, T; Browning, N

    2007-12-05

    Nanowires (NWs) are a crucial component in today's nanoscale devices and are vital to the further development of nanotechnology. To achieve reliable growth of NWs and uniform electronic properties, the specific mechanisms that control the structural development of NWs and the correlation between NWs and their nucleation and growth processes must be examined. Because imaging is not possible in Chemical Vapor Deposition (CVD) chambers, in situ transmission electron microscope (TEM) based growth methods provide a method for characterizing NW evolution. In this paper, we describe a new method of in situ synthesis and imaging of NWs using laser-assisted growth inside a TEM. The vapor-liquid solid (VLS) growth mechanism (Figure 1), first described by Wagner and co-workers, is a widely accepted description of how many 1D nanostructures are formed. VLS and similar models have been applied to such methods as hybrid pulsed-laser ablation/chemical vapor deposition (PLA/CVD) and laser assisted NW growth at elevated temperatures, in which a pulsed laser ablates a target with gas flowing through the reaction chamber held at elevated temperature. These methods have successfully produced semiconductor and conducting oxide NWs with size control determined by the catalyst droplet diameter. The VLS description of NW growth is a widely accepted model, but the exact role of vapor species and its interaction with the catalyst particle is not fully understood. For example, NW growth has been observed to occur far below predicted eutectic temperatures, which suggests that alternative mechanisms such as solid-liquid-solid growth (SLS) may play a role. Many NW fabrication techniques preclude direct in situ characterization of the growth process. Because of this need for direct observation during growth, TEM-based NW growth methods have become increasingly popular. Though progress has been made in the study of the VLS mechanism of NW growth using in situ TEM, conventional in situ growth

  6. In-Situ TEM-STM Observations of SWCNT Ropes/Tubular Transformations

    NASA Technical Reports Server (NTRS)

    Sola, F.; Lebron-Colon, M.; Ferreira, P. J.; Fonseca, L. F.; Meador, M. A.; Marin, C.

    2010-01-01

    Single-walled carbon nanotubes (SWCNTs) prepared by the HiPco process were purified using a modified gas phase purification technique. A TEM-STM holder was used to study the morphological changes of SWCNT ropes as a function of applied voltage. Kink formation, buckling behavior, tubular transformation and eventual breakdown of the system were observed. The tubular formation was attributed to a transformation from SWCNT ropes to multi-walled carbon nanotube (MWCNT) structures. It is likely mediated by the patching and tearing mechanism which is promoted primarily by the mobile vacancies generated due to current-induced heating and, to some extent, by electron irradiation.

  7. A survey of jet aircraft PM by TEM in APEX III

    NASA Astrophysics Data System (ADS)

    Huang, Chung-Hsuan; Bryg, Victoria M.; Vander Wal, Randy L.

    2016-09-01

    Results are reported for sampling non-volatile particulate matter from field tests during the NASA led APEX III campaign. This paper reports observations of particulate emissions collected from a suite of jet engine aircraft to assess differences and similarities in soot macro- micro- and nanostructure using TEM. Aggregates are compact, primary particle sizes varied and nanostructure is mixed. Comparisons are made to soot from a laboratory flame as a well-studied reference. Results are interpreted in terms of turbulence interacting with the different stages of particle formation and growth with implications for atmospheric processing and climate impact.

  8. Thermophysical ESEM and TEM Characterization of Carbon Fibers CTE, Spectroscopy and Roughness Studies at High Temperatures

    NASA Technical Reports Server (NTRS)

    Ochoa, Ozden O.

    2004-01-01

    Accurate determination of the transverse properties of carbon fibers is important for assessment and prediction of local material as well as global structural response of composite components. However the measurements are extremely difficult due to the very small diameters of the fibers (few microns only) and must be conducted within a microscope. In this work, environmental scanning electron microscope (ESEM) and transmission electron microscope (TEM) are used to determine the transverse coefficient of thermal expansion of different carbon fibers as a function of temperature.

  9. Structural investigations of {beta}-CaAlF{sub 5} by coupling powder XRD, NMR, EPR and spectroscopic parameter calculations

    SciTech Connect

    Body, M. . E-mail: monique.body@univ-lemans.fr; Silly, G.; Legein, C.; Buzare, J.-Y.; Calvayrac, F.; Blaha, P.

    2005-12-15

    {beta}-CaAlF{sub 5} was synthesized by solid-state reaction. The precise structure was refined from X-ray powder diffraction data in the monoclinic space group P2{sub 1}/c with lattice constants a=5.3361A, b=9.8298A, c=7.3271A, and {beta}=109.91{sup o} (Z=4). The structure exhibits isolated chains of AlF{sub 6}{sup 3-} octahedra sharing opposite corners.{sup 19}F and {sup 27}Al solid state NMR spectra were recorded using MAS and SATRAS techniques. An EPR spectrum was recorded for {beta}-CaAlF{sub 5}:Cr{sup 3+}. The experimental spectra were simulated in order to extract the NMR and EPR parameter values. Five fluorine sites and one low symmetry aluminium site were found in agreement with the refined structure. These parameters were calculated using empirical and ab-initio methods. The agreement obtained between the calculated {sup 19}F chemical shift values, {sup 27}Al quadrupolar parameters, Cr{sup 3+} EPR fine structure parameters and the experimental results demonstrates the complementarity of XRD, magnetic resonance experiments and theoretical methodologies.

  10. Synthesis and characterization of low-OH-fluor-chlorapatite: A single-crystal XRD and NMR spectroscopic study

    SciTech Connect

    McCubbin, Francis M; Mason, Harris E; Park, Hyunsoo; Phillips, Brian L; Parise, John B; Nekvasil, Hanna; Lindsley, Donald H

    2008-12-12

    Los-OH apatite of the compositional range Ca{sub 4.99-5.06}(PO{sub 4}){sub 2.98-3.00}F{sub 0.51-0.48}Cl{sub 0.38-0.36}OH{sub 0.14-0.12} was synthesized and characterized structurally by synchrotron-based single-crystal X-ray diffraction (XRD), and multiple nuclear magnetic resonance (NMR) spectroscopic techniques. the average structure is hexagonal with space group P6{sub 3}/m. The presence of scattering in the single-crystal diffraction data set, which is incommensurate within the average hexagonal structure, suggests the presence of localized short-range monoclinic domains. Complex lineshapes in the {sup 31}P and {sup 19}F MAS NMR spectra are also consistent with the presence of an incommensurate phase. No evidence was detected for splitting of the Ca2 site into two distinct sites (as had been previously reported for hexagonal ternary apatities). Structure refinement and {sup 19}F{l_brace}{sup 35}Cl{r_brace} TRAPDOR NMR experiments verified intercolumnal neighboring of F and Cl atoms (inter-column distance of 2.62 {angstrom}) within this low-OH{sup -} apatite suggesting that long-range neighboring of F and Cl within the apatite anion channels is feasible.

  11. Investigation of the electrocatalysis for oxygen reduction reaction by Pt and binary Pt alloys: an XRD, XAS and electrochemical study

    SciTech Connect

    Mukerjee, S.; McBreen, J.; Srinivasan, S.

    1995-12-31

    Electrocatalysis for the oxygen reduction reaction (ORR) on five binary Pt alloy electrocatalysts (PtCr/C, PtMn/C, PtFe/C, PtCo/C and PtNi/C) supported on carbon have been investigated. The electrochemical characteristics for ORR in a proton conducting fuel cell environment has been correlated with the electronic and structural parameters determined under in situ conditions using XANES and EXAFS technique respectively. Results indicate that all the alloys possess higher Pt 5d band vacancies as compared to Pt/C. There is also evidence of lattice contraction in the alloys (supported by XRD results). Further, the Pt/C shows increase in Pt 5 d band vacancies during potential transitions from 0.54 to 0.84 V vs. RHE, which has been ration@ on the basis of OH type adsorption. In contrast to this, the alloys do not exhibit such an enhancement. Detailed EXAFS analysis supports the presence of OH species on Pt/C and its relative absence in the alloys. Correlation of the electrochemical results with bond distances and d-band vacancies show a volcano type behavior with the PtCr/C on top of the curve.

  12. Structural studies with the use of XRD and Mössbauer spectroscopy of new high Manganese steels

    NASA Astrophysics Data System (ADS)

    Jablonska, Magdalena Barbara

    2014-04-01

    New high-strength austenitic and austenitic-ferritic manganese steels represent a significant potential in applications for structural components in the automotive and railway industry due to the excellent combination of high mechanical properties and good plasticity. They belong to the group of steels called AHSS (Advanced High Strength Steels) and UHSS (Ultra High Strength Steels). Application of this combination of properties allows a reduction in the weight of vehicles by the use of reduced cross-section components, and thus to reduce fuel consumption. The development and implementation of industrial production of such interesting and promising steel and its use as construction material requires an improvement of their casting properties and susceptibility to deformation in plastic working conditions. In this work, XRD, Transmission Mössbauer Spectroscopy and Conversion Electron Mössbauer Spectroscopy were employed in a study of the new high-manganese steels with a austenite and austenite-ferrite structure. The influence of the plastic deformation parameters on the changes in the structure, distribution of ferrite and disclosure of the presence of carbides was determined. The analysis of phase transformations in various times using CEMS method made possible to reveal their fine details.

  13. XRD analysis of undoped and Fe doped TiO{sub 2} nanoparticles by Williamson Hall method

    SciTech Connect

    Bharti, Bandna; Barman, P. B.; Kumar, Rajesh

    2015-08-28

    Undoped and Fe doped titanium dioxide (TiO{sub 2}) nanoparticles were synthesized by sol-gel method at room temperature. The synthesized samples were annealed at 500°C. For structural analysis, the prepared samples were characterized by X-ray diffraction (XRD). The crystallite size of TiO{sub 2} and Fe doped TiO{sub 2} nanoparticles were calculated by Scherer’s formula, and was found to be 15 nm and 11 nm, respectively. Reduction in crystallite size of TiO{sub 2} with Fe doping was observed. The anatase phase of Fe-doped TiO{sub 2} nanoparticles was also confirmed by X-ray diffraction. By using Williamson-Hall method, lattice strain and crystallite size were also calculated. Williamson–Hall plot indicates the presence of compressive strain for TiO{sub 2} and tensile strain for Fe-TiO{sub 2} nanoparticles annealed at 500°C.

  14. Shades of green in 15th century paintings: combined microanalysis of the materials using synchrotron radiation XRD, FTIR and XRF

    NASA Astrophysics Data System (ADS)

    Salvadó, Nati; Butí, Salvador; Cotte, Marine; Cinque, Gianfelice; Pradell, Trinitat

    2013-04-01

    A representative selection of green paintings from fifteenth century Catalonia and the Crown of Aragon are analyzed by a combination of synchrotron radiation microanalytical techniques including FTIR, XRD, and XRF. The green pigments themselves are found to be a mixture of copper acetates/basic copper acetates and basic copper chlorides. Nevertheless, a broader range of green shades were obtained by mixing the green pigment with yellow, white, and blue pigments and applied forming a sequence of micrometric layers. Besides the nature of the pigments themselves, degradation and reaction products, such as carboxylates, formates and oxalates were also identified. Some of the copper based compounds, such as the basic copper chloride, may be either part of the original pigment or a weathering product. The high resolution, high brilliance, and small footprint of synchrotron radiation proved to be essential for the analysis of those submillimetric paint layers made of a large variety of compounds heterogeneous in nature and distribution and present in extremely low concentrations.

  15. Drill Core Mineral Analysis by Means of the Hyperspectral Imaging Spectrometer HySpex, XRD and Asd in Proximity of the MÝTINA Maar, Czech Republic

    NASA Astrophysics Data System (ADS)

    Koerting, F.; Rogass, C.; Kaempf, H.; Lubitz, C.; Harms, U.; Schudack, M.; Kokaly, R.; Mielke, C.; Boesche, N.; Altenberger, U.

    2015-12-01

    Imaging spectroscopy is increasingly used for surface mapping. Therefore different expert systems are being utilized to identify surface cover materials. Those expert systems mainly rely on the spectral comparison between unknown and library spectra, but their performances were only limited qualified. This study aims on the comparative analysis of drill core samples from the recently discovered maar system in the Czech Republic. Drill core samples from the surrounding area of the Mýtina maar were analyzed by X-Ray diffraction (XRD) and the hyperspectral spectrometer HySpex. Additionally, soil samples were measured in-situ by the ASD FieldSpec4 and in the laboratory by the HySpex VNIR/SWIR spectrometer system. The data was then analyzed by the MICA-algorithm and the results were compared to the results of the XRD -analysis. The XRD-analysis served here as validation basis. The results of the hyperspectral and the XRD analyses were used to densify a volcanic map that also integrates in-situ soil measurements in the surrounding area of Mýtina. The comparison of the XRD- and solaroptical remote sensing results showed a good correlation of qualified minerals if the soil organic carbon content was significantly low. Contrary to XRD, smectites and muscovites were also straightforward identified that underlines the overall performance of the approach to identify minerals. Basically, in this work an operable approach is proposed that enables the fast, repeatable and detailed analysis of drill cores, drill core samples and soil samples and, hence, provides a higher performance than state-of-the-art XRD-analyses.

  16. Identification of small molecules that inhibit the interaction of TEM8 with anthrax protective antigen using a FRET assay.

    PubMed

    Cryan, Lorna M; Habeshian, Kaiane A; Caldwell, Thomas P; Morris, Meredith T; Ackroyd, P Christine; Christensen, Kenneth A; Rogers, Michael S

    2013-07-01

    Tumor marker endothelial 8 (TEM8) is a receptor for the protective antigen (PA) component of anthrax toxin. TEM8 is upregulated on endothelial cells lining the blood vessels within tumors, compared with normal blood vessels. A number of studies have demonstrated a pivotal role for TEM8 in developmental and tumor angiogenesis. We have also shown that targeting the anthrax receptors with a mutated form of PA inhibits angiogenesis and tumor formation in vivo. Here we describe the development and testing of a high-throughput fluorescence resonance energy transfer assay to identify molecules that strongly inhibit the interaction of PA and TEM8. The assay we describe is sensitive and robust, with a Z' value of 0.8. A preliminary screen of 2310 known bioactive library compounds identified ebselen and thimerosal as inhibitors of the TEM8-PA interaction. These molecules each contain a cysteine-reactive transition metal, and complementary studies indicate that their inhibition of interaction is due to modification of a cysteine residue in the TEM8 extracellular domain. This is the first demonstration of a high-throughput screening assay that identifies inhibitors of TEM8, with potential application for antianthrax and antiangiogenic diseases.

  17. Nano-Structural Elucidation in Carbon Black Loaded NR Vulcanizate by 3D-TEM and In Situ WAXD Measurements

    SciTech Connect

    Ikeda,Y.; Kato, A.; Shimanuki, J.; Kohjiya, S.; Tosaka, M.; Poompradub, S.; Toki, S.; Hsiao, B.

    2007-01-01

    Three dimensional (3D) visualization of nanometer structure of carbon black dispersion in rubbery matrix has successfully been studied and reported in this paper. Use of 3D-TEM, which is computerized tomography combined with transmission electron microscopy (TEM), enabled us to reconstruct 3D images of carbon black aggregates in natural rubber (NR) matrix. The TEM measurements were conducted by a bright-field method on thin samples without any electron staining. The sample was subject to uni-axial tilting (+65 degree to -65 degree with 2 degree increment) in the sample chamber, and 66 TEM images were taken on each sample. These TEM images were used for computerized tomography to reconstruct the 3D image. This technique is designated as 3D-TEM. The nano-structural features observed by 3D-TEM were in conformity with the electron-conductivity results, and the percolation behavior was recognized. These results were further supplemented by in situ wide-angle X-ray diffraction (WAXD), i.e., simultaneous WAXD and tensile measurements on the sample to observe the strain-induced crystallization in NR vulcanizate. Upon tensile elongation, the crystallization was clearly observed in WAXD in the presence of carbon black, and it contributed to the tensile properties. In order to understand the performances of filled NR vulcanizates, it surely is necessary to know the structural states of the mixed nano-filler and the crystallites produced upon elongation.

  18. CMT-Type β-Lactamase TEM-125, an Emerging Problem for Extended-Spectrum β-Lactamase Detection†

    PubMed Central

    Robin, Frédéric; Delmas, Julien; Archambaud, Maryse; Schweitzer, Cédric; Chanal, Catherine; Bonnet, Richard

    2006-01-01

    The clinical strain Escherichia coli TO799 was resistant to penicillin-clavulanate combinations and ceftazidime and was not reproducibly detected as an extended-spectrum β-lactamase (ESBL) according to the standards of the Clinical Laboratory Standards Institute (CLSI; formerly NCCLS) and the national guidelines of the French Society for Microbiology (Comité de l'Antibiogramme de la Société Française de Microbiologie). A novel β-lactamase, designated TEM-125, was responsible for this phenotype. TEM-125 harbors a complex association of mutations previously described in the ESBL TEM-12 and in the inhibitor-resistant β-lactamase TEM-39. TEM-125 is the first complex mutant TEM to present hydrolytic activity against ceftazidime (kcat, 3.7 s−1) together with a high level of resistance to clavulanate (50% inhibitory concentration, 13.6 μM). The discovery of such an ESBL, which is difficult to detect by the usual ESBL detection methods, confirms the emergence of a complex mutant TEM subgroup and highlights the need to evaluate detection methods so as to avoid possible therapeutic failures. PMID:16801418

  19. EBSD and TEM Characterization of High Burn-up Mixed Oxide Fuel

    SciTech Connect

    Teague, Melissa C.; Gorman, Brian P.; Miller, Brandon D.; King, Jeffrey

    2014-01-01

    Understanding and studying the irradiation behavior of high burn-up oxide fuel is critical to licensing of future fast breeder reactors. Advancements in experimental techniques and equipment are allowing for new insights into previously irradiated samples. In this work dual column focused ion beam (FIB)/scanning electron microscope (SEM) was utilized to prepared transmission electron microscope samples from mixed oxide fuel with a burn-up of 6.7% FIMA. Utilizing the FIB/SEM for preparation resulted in samples with a dose rate of <0.5 mRem/h compared to approximately 1.1 R/h for a traditionally prepared TEM sample. The TEM analysis showed that the sample taken from the cooler rim region of the fuel pellet had approximately 2.5x higher dislocation density than that of the sample taken from the mid-radius due to the lower irradiation temperature of the rim. The dual column FIB/SEM was additionally used to prepared and serially slice approximately 25 um cubes. High quality electron back scatter diffraction (EBSD) were collected from the face at each step, showing, for the first time, the ability to obtain EBSD data from high activity irradiated fuel.

  20. Performance of low-voltage STEM/TEM with delta corrector and cold field emission gun.

    PubMed

    Sasaki, Takeo; Sawada, Hidetaka; Hosokawa, Fumio; Kohno, Yuji; Tomita, Takeshi; Kaneyama, Toshikatsu; Kondo, Yukihito; Kimoto, Koji; Sato, Yuta; Suenaga, Kazu

    2010-08-01

    To reduce radiation damage caused by the electron beam and to obtain high-contrast images of specimens, we have developed a highly stabilized transmission electron microscope equipped with a cold field emission gun and spherical aberration correctors for image- and probe-forming systems, which operates at lower acceleration voltages than conventional transmission electron microscopes. A delta-type aberration corrector is designed to simultaneously compensate for third-order spherical aberration and fifth-order 6-fold astigmatism. Both were successfully compensated in both scanning transmission electron microscopy (STEM) and transmission electron microscopy (TEM) modes in the range 30-60 kV. The Fourier transforms of raw high-angle annular dark field (HAADF) images of a Si[110] sample revealed spots corresponding to lattice spacings of 111 and 96 pm at 30 and 60 kV, respectively, and those of raw TEM images of an amorphous Ge film with gold particles showed spots corresponding to spacings of 91 and 79 pm at 30 and 60 kV, respectively. Er@C(82)-doped single-walled carbon nanotubes, which are carbon-based samples, were successfully observed by HAADF-STEM imaging with an atomic-level resolution.

  1. Inversion of arbitrary segmented loop source TEM data over a layered earth

    NASA Astrophysics Data System (ADS)

    Li, Hai; Xue, Guo-qiang; Zhao, pan; Zhou, Nan-nan; Zhong, Hua-sen

    2016-05-01

    The loop source TEM method has been widely used in the detection of a mined out area in China. In the cases that the laying of traditional rectangle or square transmitting loop is limited due to the presence of obstacle on the path of the loop, the changing of the shape of the transmitting loop to bypass the obstacle is a labor saving solution. A numeric integration scheme is proposed to calculate the response and Jacobian of the segmented loop source from that of an electric dipole source. The comparison of forward response between the segmented loop and square loop shows the effect of loop geometry on the decay curves. In order to interpret the data from an irregular source loop, this paper presents an inversion scheme that incorporate the effect of loop geometry. The proposed inversion scheme is validated on the synthetic data, and then applied to the field data. The result reveals that the developed inversion scheme is capable of interpreting the segmented loop source TEM field data.

  2. TEM study of shock metamorphism in quartz from the Sedan nuclear test site

    NASA Astrophysics Data System (ADS)

    Cordier, P.; Gratz, A. J.

    1995-01-01

    Nuclear explosions represent a useful simulation of meteorite impacts. Stressed of tens of gigapascals are produced during detonation and stress pulses can last 0.1 ms or longer, which is 3-4 orders of magnitude longer than laboratory experiments. Samples studied here were taken from the ejecta of the Sedan nuclear test site and consist of a coarse-grained granodiorite containing quartz, plagioclase, K-feldspar, cordierite and hornblende. Schocked quartz grains were selected optically in thin section and studied by Transmission Electron Microscopy (TEM). TEM reveals the presence of planar deformation features (PDFs), which consist of multiple sets of planar amorphous lamellae with the crystallographic orientations (1 0 - 1 3), (1 0 - 1 2), and rarely (1 0 - 1 1). Some lamellae exhibit a substructure which consist of amorphous sublamellae organized 'en echelon'. No high-pressure phases were detected along the transformation lamellae. Some lamellae show evidence of beginning recrystallization, which probably occurred during cooling of the hot ejecta. The shock-induced defects present at the Sedan site are very similar to those seen in laboratory shock recovery experiments and also to those present at meteorite impact craters (e.g., Meteor Crater or Ries Crater). This suggests that shock-induced amorphization in quartz is not strongly dependant on shock pulse duration.

  3. Quantitative electrochemical measurements using in situ ec-S/TEM devices.

    PubMed

    Unocic, Raymond R; Sacci, Robert L; Brown, Gilbert M; Veith, Gabriel M; Dudney, Nancy J; More, Karren L; Walden, Franklin S; Gardiner, Daniel S; Damiano, John; Nackashi, David P

    2014-04-01

    Insight into dynamic electrochemical processes can be obtained with in situ electrochemical-scanning/transmission electron microscopy (ec-S/TEM), a technique that utilizes microfluidic electrochemical cells to characterize electrochemical processes with S/TEM imaging, diffraction, or spectroscopy. The microfluidic electrochemical cell is composed of microfabricated devices with glassy carbon and platinum microband electrodes in a three-electrode cell configuration. To establish the validity of this method for quantitative in situ electrochemistry research, cyclic voltammetry (CV), choronoamperometry (CA), and electrochemical impedance spectroscopy (EIS) were performed using a standard one electron transfer redox couple [Fe(CN)6]3-/4--based electrolyte. Established relationships of the electrode geometry and microfluidic conditions were fitted with CV and chronoamperometic measurements of analyte diffusion coefficients and were found to agree with well-accepted values that are on the order of 10-5 cm2/s. Influence of the electron beam on electrochemical measurements was found to be negligible during CV scans where the current profile varied only within a few nA with the electron beam on and off, which is well within the hysteresis between multiple CV scans. The combination of experimental results provides a validation that quantitative electrochemistry experiments can be performed with these small-scale microfluidic electrochemical cells provided that accurate geometrical electrode configurations, diffusion boundary layers, and microfluidic conditions are accounted for.

  4. TEM and SIMS Analysis of (100), (110), and (111) Single Crystal Niobium

    SciTech Connect

    Batchelor, A. D.; Stevie, F. A.; Leonard, D. N.; Russell, P. E.; Griffis, D. P.; Myneni, G. R.

    2007-08-09

    Single crystal niobium specimens of (100), (110) and (111) crystal orientations have been analyzed using TEM and SIMS. The TEM specimens were prepared using Focused Ion Beam (FIB) and show niobium oxide thicknesses ranging from 4.9 to 8.3 nm for the three specimens after buffer chemical polishing. The oxide layers appear uniform and no significant sub-oxide region was noted. SIMS analysis was made for all three orientations on hydrogen, carbon, and oxygen before and after heat treatments at 90, 600, and 1250 deg. C. Hydrogen is at a high level between the oxide layer and niobium, but at a relatively low level in the oxide. No high oxygen concentration region was noted in the niobium below the oxide. C contamination on the surface is detected mainly at the surface. Analysis after heat treatments showed some decrease in hydrogen after the 600 deg. C heat treatment, and significant oxidation of the niobium after the 1250 deg. C heat treatment.

  5. Double-helical ultrastructure of polycationic dendronized polymers determined by single-particle Cryo-TEM.

    PubMed

    Böttcher, Christoph; Schade, Boris; Ecker, Christof; Rabe, Jürgen P; Shu, Lijin; Schlüter, A Dieter

    2005-05-01

    The ultrastructure of cationic dendronized polymers (denpols) of third and fourth generations (PG3 and PG4) in water was determined by using single-particle cryo-transmission electron microscopy (cryo-TEM). At concentrations in the region of 50 mg L(-1), networks of double-stranded fibers were revealed that exhibit well-defined diameters of 5.9 nm+/-0.4 nm for PG3 and 7.4 nm+/-0.4 nm for PG4. The structure varies with progression along the fibers, and includes a double helix with a pitch of 7.0+/-0.4 nm for PG3 and 9.0+/-0.4 nm for PG4. The formation of the double strands is attributed to the hydrophobic effect and limited crowding in the dendron shell of the third and fourth generation denpols investigated. From solutions of lower concentrations (around 10 mg L(-1)), isolated molecular fibers were adsorbed onto high-energy surfaces and examined by performing scanning force microscopy (SFM) on mica, and after staining, TEM on glow-discharged carbon films. In both cases, characteristic undulations of single strands were observed, which are attributed largely to the adsorption process. PMID:15736148

  6. Structural changes in collagen fibrils across a mineralized interface revealed by cryo-TEM.

    PubMed

    Quan, Bryan D; Sone, Eli D

    2015-08-01

    The structure of the mineralized collagen fibril, which is the basic building block of mineralized connective tissues, is critical to its function. We use cryo-TEM to study collagen structure at a well-defined hard-soft tissue interface, across which collagen fibrils are continuous, in order to evaluate changes to collagen upon mineralization. To establish a basis for the analysis of collagen banding, we compared cryo-TEM images of rat-tail tendon collagen to a model based on the X-ray structure. While there is close correspondence of periodicity, differences in band intensity indicate fibril regions with high density but lacking order, providing new insight into collagen fibrillar structure. Across a mineralized interface, we show that mineralization results in an axial contraction of the fibril, concomitant with lateral expansion, and that this contraction occurs only in the more flexible gap region of the fibril. Nevertheless, the major features of the banding pattern are not significantly changed, indicating that the axial arrangement of molecules remains largely intact. These results suggest a mechanism by which collagen fibrils are able to accommodate large amounts of mineral without significant disruption of their molecular packing, leading to synergy of mechanical properties.

  7. Alpha to Omega Phase Change in Zr under Shock and Static Pressures: A TEM Study.

    NASA Astrophysics Data System (ADS)

    Jyoti, G.; Dey, G. K.; Joshi, K. D.; Tiwari, R.; Gupta, Satish C.; Banerjee, S.; Sikka, S. K.

    2001-06-01

    To compare the mode of formation of ω phase from the α phase in Zr under dynamic and static high pressures, we have carried out a TEM study on Zr samples partially transformed to ω phase under the two conditions. In the present paper, we present this comparative TEM study on Zr. Comparison of the selected area diffraction patterns shows the identical orientation relationship between the α and the ω phases for the two cases. The micrographs for the two cases, however, show considerably different morphology. The shock transformed sample displays the formation of large plates of ω structure from the α structure, whereas the statically transformed sample shows ω grains of irregular shape and sizes. This implies that although the orientation relations between the α and the ω phase i.e the relation between the end states are identical, it does not necessarily imply that the mode of formation of the ω phase is the same under the two conditions. The high resolution electron microscopy results especially pertaining to the coherency of the atomic planes on the (α/ω) interface for the static and dynamically transformed sample will be presented.

  8. High-resolution methane emission estimates using the InTEM inversion system

    NASA Astrophysics Data System (ADS)

    Connors, S.; Manning, A.; Robinson, A. D.; Riddick, S. N.; Forster, G.; Oram, D.; O'Doherty, S.; Harris, N. R. P.

    2014-12-01

    There is a growing need for comparisons between emission estimates produced using bottom-up and top-down techniques at high spatial resolution. In response to this, an inversion approach, InTEM, was adapted to estimate methane emissions for a region in the South East of the UK (~100 x 150 km). We present results covering a 2-year period (July 2012 - July 2014) in which atmospheric methane concentrations were recorded at 1 - 2 minute time-steps at four locations within the region of interest. Precise measurements were obtained using gas chromatography with flame ionisation detection (GC-FID) for all sites except one, which used a PICARRO Cavity Ring-Down Spectrometer (CRDS). These observations, along with the UK Met Office's Lagrangian particle dispersion model (NAME) were used within InTEM to produce the methane emission fields. Emission estimates were produced at varying spatial resolutions, for annual and seasonal time frames . We present results indicating the optimum number of observation sites required for this region, and how this can affect our uncertainty estimates. These results are compared with the UK National Atmospheric Emissions Inventory (NAEI) which is compiled using bottom-up methods and available at 1x1 km resolution. To our knowledge, no inversion technique has been implemented on such a fine spatial resolution. This is a pilot project which, given proof of concept, could be scaled up as an alternative method for producing national scale emission inventories.

  9. Chromatic Aberration Correction for Atomic Resolution TEM Imaging from 20 to 80 kV.

    PubMed

    Linck, Martin; Hartel, Peter; Uhlemann, Stephan; Kahl, Frank; Müller, Heiko; Zach, Joachim; Haider, Max; Niestadt, Marcel; Bischoff, Maarten; Biskupek, Johannes; Lee, Zhongbo; Lehnert, Tibor; Börrnert, Felix; Rose, Harald; Kaiser, Ute

    2016-08-12

    Atomic resolution in transmission electron microscopy of thin and light-atom materials requires a rigorous reduction of the beam energy to reduce knockon damage. However, at the same time, the chromatic aberration deteriorates the resolution of the TEM image dramatically. Within the framework of the SALVE project, we introduce a newly developed C_{c}/C_{s} corrector that is capable of correcting both the chromatic and the spherical aberration in the range of accelerating voltages from 20 to 80 kV. The corrector allows correcting axial aberrations up to fifth order as well as the dominating off-axial aberrations. Over the entire voltage range, optimum phase-contrast imaging conditions for weak signals from light atoms can be adjusted for an optical aperture of at least 55 mrad. The information transfer within this aperture is no longer limited by chromatic aberrations. We demonstrate the performance of the microscope using the examples of 30 kV phase-contrast TEM images of graphene and molybdenum disulfide, showing unprecedented contrast and resolution that matches image calculations. PMID:27563976

  10. Characterization of mineral particles in winter fog of Beijing analyzed by TEM and SEM.

    PubMed

    Li, Weijun; Shao, Longyi

    2010-02-01

    Aerosol samples were collected during winter fog and nonfog episodes in Beijing. Transmission electron microscopy (TEM) and scanning electron microscopy (SEM) were applied to study morphologies, sizes, and compositions of aerosol particles. TEM observation indicates that most mineral particles collected in fog episode are scavenged in fog droplets. Number-size distributions of mineral particles collected in fog and nonfog episodes show two main peaks at the ranges of 0.1-0.3 and 1-2.5 microm, respectively. Based on their major compositions, mineral particles mainly include Si-rich, Ca-rich, and S-rich. Average S/Ca ratio of mineral particles collected in fog episode is 6.11, being eight times higher than that in nonfog episodes. Development mechanism of individual mineral particles in fog droplets is proposed. It is suggested that mineral particles with abundant alkaline components (e.g., "Ca-rich" particles) occurred in air should alleviate acidic degree of fog and contribute to complexity of fog droplets in Beijing.

  11. Chromatic Aberration Correction for Atomic Resolution TEM Imaging from 20 to 80 kV

    NASA Astrophysics Data System (ADS)

    Linck, Martin; Hartel, Peter; Uhlemann, Stephan; Kahl, Frank; Müller, Heiko; Zach, Joachim; Haider, Max.; Niestadt, Marcel; Bischoff, Maarten; Biskupek, Johannes; Lee, Zhongbo; Lehnert, Tibor; Börrnert, Felix; Rose, Harald; Kaiser, Ute

    2016-08-01

    Atomic resolution in transmission electron microscopy of thin and light-atom materials requires a rigorous reduction of the beam energy to reduce knockon damage. However, at the same time, the chromatic aberration deteriorates the resolution of the TEM image dramatically. Within the framework of the SALVE project, we introduce a newly developed Cc/Cs corrector that is capable of correcting both the chromatic and the spherical aberration in the range of accelerating voltages from 20 to 80 kV. The corrector allows correcting axial aberrations up to fifth order as well as the dominating off-axial aberrations. Over the entire voltage range, optimum phase-contrast imaging conditions for weak signals from light atoms can be adjusted for an optical aperture of at least 55 mrad. The information transfer within this aperture is no longer limited by chromatic aberrations. We demonstrate the performance of the microscope using the examples of 30 kV phase-contrast TEM images of graphene and molybdenum disulfide, showing unprecedented contrast and resolution that matches image calculations.

  12. TEM studies of laterally overgrown GaN layers grown on non-polarsubstrates

    SciTech Connect

    Liliental-Weber, Z.; Ni, X.; Morkoc, H.

    2006-01-05

    Transmission electron microscopy (TEM) was used to study pendeo-epitaxial GaN layers grown on polar and non-polar 4H SiC substrates. The structural quality of the overgrown layers was evaluated using a number of TEM methods. Growth of pendeo-epitaxial layers on polar substrates leads to better structural quality of the overgrown areas, however edge-on dislocations are found at the meeting fronts of two wings. Some misorientation between the 'seed' area and wing area was detected by Convergent Beam Electron Diffraction. Growth of pendeo-epitaxial layers on non-polar substrates is more difficult. Two wings on the opposite site of the seed area grow in two different polar directions with different growth rates. Most dislocations in a wing grown with Ga polarity are 10 times wider than wings grown with N-polarity making coalescence of these layers difficult. Most dislocations in a wing grown with Ga polarity bend in a direction parallel to the substrate, but some of them also propagate to the sample surface. Stacking faults formed on the c-plane and prismatic plane occasionally were found. Some misorientation between the wings and seed was detected using Large Angle Convergent Beam Diffraction.

  13. Deformation mechanisms of a 20Mn TWIP steel investigated by in situ neutron diffraction and TEM

    SciTech Connect

    Shen, Yongfeng; Wang, Y. D.; Liu, Xiaopeng; Sun, Xin; Peng, R. Lin; Zhang, S. Y.; Zuo, Liang; Liaw, Peter K.

    2013-07-25

    The deformation mechanisms and associated microstructure changes during tensile loading of an annealed twinning-induced plasticity (TWIP) steel with the chemical composition of Fe–20Mn–3Si–3Al–0.045C (wt.%) were systematically investigated using in situ time-of-flight (TOF) neutron diffraction in combination with postmortem transmission electron microscopy (TEM). The initial microstructure of the investigated alloy consists of equiaxed austenitic grains with the initial α´-phase of ~7% in volume. In addition to dislocation slip, twinning and two kinds of martensitic transformations from the austenite to α´- and epsilon martensites were observed as the main deformation modes during the tensile deformation. In situ neutron diffraction provides a powerful tool to establish the deformation mode map for elucidating the role of different deformation modes in different strain regions. The critical stress is 520 MPa for the martensitic transformation from the austenite to α´-martensite, whereas a higher stress (>600 MPa) is required for actuating the deformation twin and/or the martensitic transformation from -martensite. Both epsilon- and α´-martensites act as the hard phases whereas mechanical twinning contributes to both strength and ductility of the studied steel. TEM observations confirmed that the twinning process was facilitated by the parent grains orientated with <111> or <110> parallel to the loading direction. The nucleation and growth of twins are attributed to the pole and self-generation formation mechanisms, as well as the stair-rod cross-slip mechanism.

  14. Methods for TEM analysis of NIST's single-walled carbon nanotube Standard Reference Material

    NASA Astrophysics Data System (ADS)

    Mansfield, Elisabeth; Geiss, Roy; Fagan, Jeffrey A.

    2009-08-01

    The National Institute of Standards and Technology (NIST) will soon release a series of single-walled carbon nanotube (SWCNT) reference materials (RMs) to provide users with a well-characterized material for their applications. The SWCNT reference material will be introduced as a series of three types of material: (1) raw soot characterized for composition, which will be certified as a Standard Reference Material, (2) purified (greater than 90 % SWCNT by weight) bucky paper and (3) dispersed, length-sorted populations characterized by length. The instrumental characterization of NIST's SWCNT reference materials is extensive, and this paper aims to provide researchers with dispersion preparation methods for TEM (transmission electron microscopy) analysis of the SWCNT raw soot. A selection of dispersing solvents, including organic solvents, aqueous surfactants and DNA dispersions, were prepared and examined by TEM. Recommendations for sample preparation of the SWCNT SRM 2483 to yield images similar to those presented here are given. Examples of images of the length-sorted SWCNT reference material are also shown. These results illustrate the importance of optimal dispersion to enable imaging of SWCNT characteristics.

  15. Determination of the initial oxidation behavior of Zircaloy-4 by in-situ TEM

    NASA Astrophysics Data System (ADS)

    Harlow, Wayne; Ghassemi, Hessam; Taheri, Mitra L.

    2016-06-01

    The corrosion behavior of Zircaloy-4 (Zry-4), specifically by oxidation, is a problem of great importance as this material is critical for current nuclear reactor cladding. The early formation behavior and structure of the oxide layer during oxidation was studied using in-situ TEM techniques that allowed for Zry-4 to be monitored during corrosion. These environmental exposure experiments were coupled with precession electron diffraction to identify and quantify the phases present in the samples before and after the oxidation. Following short-term, high temperature oxidation, the dominant phase was revealed to be monoclinic ZrO2 in a columnar structure. These samples oxidized in-situ contained structures that correlated well with bulk Zry-4 subjected to autoclave treatment, which were used for comparison and validation of this technique. By using in-situ TEM the effect of microstructure features, such as grain boundaries, on oxidation behavior of an alloy can be studied. The technique presented herein holds the potential to be applied any alloy system to study these effects.

  16. Applying compressive sensing to TEM video: A substantial frame rate increase on any camera

    SciTech Connect

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

    2015-08-13

    One of the main limitations of imaging at high spatial and temporal resolution during in-situ transmission electron microscopy (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 0.1 ms, the cameras are expensive and must replace existing detectors. In this paper, we examine the use of coded aperture compressive sensing (CS) methods to increase the frame rate 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 CS inversion. Here we describe the background of CS and statistical methods in depth and simulate the frame rates and efficiencies for in-situ TEM experiments. Depending on the resolution and signal/noise of the image, it should be possible to increase the speed of any camera by more than an order of magnitude using this approach.

  17. Applying compressive sensing to TEM video: A substantial frame rate increase on any camera

    DOE PAGESBeta

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

    2015-08-13

    One of the main limitations of imaging at high spatial and temporal resolution during in-situ transmission electron microscopy (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 0.1 ms, the cameras are expensive and must replace existing detectors. In this paper, we examine the use of coded aperture compressive sensing (CS) methods to increase the frame rate of any camera with simple, low-cost hardware modifications. The coded aperture approach allows multiple sub-frames to be coded and integratedmore » into a single camera frame during the acquisition process, and then extracted upon readout using statistical CS inversion. Here we describe the background of CS and statistical methods in depth and simulate the frame rates and efficiencies for in-situ TEM experiments. Depending on the resolution and signal/noise of the image, it should be possible to increase the speed of any camera by more than an order of magnitude using this approach.« less

  18. Advantages and limitations of OM, SEM, TEM and AFM in the study of ancient decorated pottery

    NASA Astrophysics Data System (ADS)

    Arenas-Alatorre, J.; Silva-Velazquez, Y.; Alva Medina, A.; Rivera, M.

    2010-03-01

    This paper presents results from the study of two fragments of pre-Hispanic pottery, decorated with red pigment, using Optical Microscopy (OM), Scanning Electron Microscopy (SEM), High Resolution Transmission Electron Microscopy (HRTEM), Atomic Force Microscopy (AFM) and Magnetic Force Microscopy (MFM). Capabilities and limitations of these techniques in the analysis of archaeological material are highlighted with special emphasis on TEM, AFM and MFM due to their contribution in the study of the pigment layer at micro and nano scale. The analyzed samples come from the archaeological sites of El Tajin and Xochicalco, both in Mexico. Results of conventional TEM and HRTEM analysis of the red pigment showed nanometric Fe2O3 particles in both samples but different particle shape and size distributions: specimen from El Tajin presented irregular particles between 50-100 nm while that from Xochicalco exhibited semispherical shapes in the 3-25 nm range. AFM images showed the topography of the pigments, which are related to the texture of their surface and thus to the production process. Finally, MFM showed different contrast regions suggesting the presence of ferromagnetic elements forming clusters and domain orientations on the color layer.

  19. Characterizing the Phyllosilicate Component of the Sheepbed Mudstone in Gale Crater, Mars Using Laboratory XRD and EGA

    NASA Technical Reports Server (NTRS)

    Rampe, E. B.; Morris, R. V.; Ming, D. W.; Archer, P. D.; Bish, D. L.; Chipera, S. J.; Vaniman, D. T.; Blake, D. F.; Bristow, T. F.; Sutter, B.; Farmer, J. D.; Downs, R. T.; Leveille, R.; Achilles, C. A.; Crisp, J. A.; Des Marais, D. J.; Morookian, J. M.; Morrison, S. M.; Sarrazin, P. C.; Spanovich, N.; Treiman, A. H.; Yen, A. S.

    2014-01-01

    The Curiosity rover investigated the mineralogy of the Sheepbed mudstone member of the Yellowknife Bay formation in Gale crater. Data from the Chemistry and Mineralogy (CheMin) X-ray diffractometer (XRD) helped identify phyllosilicates in the two drilled samples, John Klein and Cumberland. These patterns showed peaks at low angles, consistent with (001) peaks in 2:1 swelling phyllosilicates [1]. Evolved gas analyses (EGA) by the Sample Analysis at Mars (SAM) instrument of these samples confirmed the presence of phyllosilicates through the release of H2O at high temperatures, consistent with dehydroxylation of octahedral OH in phyllosilicates [2]. CheMin data for the phyllosilicates at John Klein and Cumberland show that they are structurally similar in that their (02l) peaks are near 22.5 deg 2theta, suggesting both samples contain trioctahedral 2:1 phyllosilicates [1]. However, the positions of the (001) peaks differ: the phyllosilicate at John Klein has its (001) peak at 10 Angstroms, whereas the phyllosilicate at Cumberland has an (001) peak at 14 Angstroms. Such differences in (001) dspacings can be ascribed to the type of cation in the interlayer site [3]. For example, large monovalent cations (e.g., K(+)) have low hydration energies and readily lose their H2O of hydration, whereas small divalent cations (e.g., Mg(2+)) have high energies of hydration and retain H2O in the phyllosilicate interlayers [3,4]. The goal of this study is to determine whether differences in the interlayer cation composition can explain the CheMin data from John Klein and Cumberland and to use this knowledge to better understand phyllosilicate formation mechanisms.

  20. A combined study by XRD, FTIR, TG and HRTEM on the structure of delaminated Fe-intercalated/pillared clay.

    PubMed

    Yuan, Peng; Annabi-Bergaya, Faïza; Tao, Qi; Fan, Mingde; Liu, Zongwen; Zhu, Jianxi; He, Hongping; Chen, Tianhu

    2008-08-01

    Fe-PILC samples were synthesized by the reaction between Na(+)- and/or Ca(2+)-montmorillonite (Mt) and base-hydrolyzed solutions of Fe(III) nitrate. Different from the known usual microporous pillared structure, a meso-microporous delaminated structure containing intercalated or pillared fragments was found in the respective resulting Fe-intercalated or -pillared clays. XRD patterns of Na(+)-Mt-based Fe-intercalated/pillared clays show one large d-spacing above 6.4 nm corresponding to the mesoporous delaminated part, whereas another d-spacing of ca. 1.5 nm was indicative of the microporous pillared part. Fe-intercalated/pillared clays based on Ca(2+)-Mt lead to similar results, but with a d-spacing less than 6 nm and a second low intense d-spacing less than 1.5 nm. In the delaminated Fe-intercalated clays, NO(-)(3) anions were retained even after thorough washing process. They play as counterions to neutralize the positive-charged iron aggregates in the delaminated structure, and can be exchanged by heteropolyanions as [PW(12)O(40)](3-). The delaminated Fe-pillared clays show good thermal stability at 500 degrees C and exhibit at this temperature dramatically higher specific surface area and porosity than the starting montmorillonites. However, calcination at a higher temperature leads to the formation of nanocrystalline hematite. Air-drying after ethanol extraction (EAD) method has an advantage over air-drying (AD) method in preserving the delaminated structure. PMID:18502444

  1. Bone matrix calcification during embryonic and postembryonic rat calvarial development assessed by SEM-EDX spectroscopy, XRD, and FTIR spectroscopy.

    PubMed

    Henmi, Akiko; Okata, Hiroshi; Anada, Takahisa; Yoshinari, Mariko; Mikami, Yasuto; Suzuki, Osamu; Sasano, Yasuyuki

    2016-01-01

    Bone mineral is constituted of biological hydroxyapatite crystals. In developing bone, the mineral crystal matures and the Ca/P ratio increases. However, how an increase in the Ca/P ratio is involved in maturation of the crystal is not known. The relationships among organic components and mineral changes are also unclear. The study was designed to investigate the process of calcification during rat calvarial bone development. Calcification was evaluated by analyzing the atomic distribution and concentration of Ca, P, and C with scanning electron microscopy (SEM)-energy-dispersive X-ray (EDX) spectroscopy and changes in the crystal structure with X-ray diffraction (XRD) and Fourier transform infrared (FTIR) spectroscopy. Histological analysis showed that rat calvarial bone formation started around embryonic day 16. The areas of Ca and P expanded, matching the region of the developing bone matrix, whereas the area of C became localized around bone. X-ray diffraction and FTIR analysis showed that the amorphous-like structure of the minerals at embryonic day 16 gradually transformed into poorly crystalline hydroxyapatite, whereas the proportion of mineral to protein increased until postnatal week 6. FTIR analysis also showed that crystallization of hydroxyapatite started around embryonic day 20, by which time SEM-EDX spectroscopy showed that the Ca/P ratio had increased and the C/Ca and C/P ratios had decreased significantly. The study suggests that the Ca/P molar ratio increases and the proportion of organic components such as proteins of the bone matrix decreases during the early stage of calcification, whereas crystal maturation continues throughout embryonic and postembryonic bone development.

  2. Transformation of meta-stable calcium silicate hydrates to tobermorite: reaction kinetics and molecular structure from XRD and NMR spectroscopy.

    PubMed

    Houston, Jacqueline R; Maxwell, Robert S; Carroll, Susan A

    2009-01-01

    Understanding the integrity of well-bore systems that are lined with Portland-based cements is critical to the successful storage of sequestered CO2 in gas and oil reservoirs. As a first step, we investigate reaction rates and mechanistic pathways for cement mineral growth in the absence of CO2 by coupling water chemistry with XRD and NMR spectroscopic data. We find that semi-crystalline calcium (alumino-)silicate hydrate (Al-CSH) forms as a precursor solid to the cement mineral tobermorite. Rate constants for tobermorite growth were found to be k = 0.6 (+/- 0.1) x 10(-5) s(-1) for a solution:solid of 10:1 and 1.6 (+/- 0.8) x 10(-4) s(-1) for a solution:solid of 5:1 (batch mode; T = 150 degrees C). This data indicates that reaction rates for tobermorite growth are faster when the solution volume is reduced by half, suggesting that rates are dependent on solution saturation and that the Gibbs free energy is the reaction driver. However, calculated solution saturation indexes for Al-CSH and tobermorite differ by less than one log unit, which is within the measured uncertainty. Based on this data, we consider both heterogeneous nucleation as the thermodynamic driver and internal restructuring as possible mechanistic pathways for growth. We also use NMR spectroscopy to characterize the site symmetry and bonding environment of Al and Si in a reacted tobermorite sample. We find two [4]Al coordination structures at delta iso = 59.9 ppm and 66.3 ppm with quadrupolar product parameters (PQ) of 0.21 MHz and 0.10 MHz (+/- 0.08) from 27Al 3Q-MAS NMR and speculate on the Al occupancy of framework sites by probing the protonation environment of Al metal centers using 27Al{1H}CP-MAS NMR. PMID:19144195

  3. Using TEM for sounding conductive and deep groundwater in Mars analog environments: Comparing two field studies

    NASA Astrophysics Data System (ADS)

    Jernsletten, J. A.

    2005-11-01

    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, using a 16 Hz sounding frequency, which is sensitive to slightly salty groundwater. Prominent features in the data are the ~500 m depth of investigation and the ~120 m depth to the water table, confirmed by data from four USGS test wells sur-rounding the field area. Note also the conductive (~20-40 Ωm) clay-rich soil above the water table. 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 conduc-tive 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. 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 show con-ductive highs at ~15 m depth below Station 50 (Line 15) and Station 30 (Line 14), interpreted as subsurface water flow under mine tailings matching surface flows seen coming out from under the tailings, and shown on maps. Both of the interpretations from Rio Tinto data (Line 4, and Lines 15 & 14) were confirmed by preliminary results from the MARTE ground truth drilling campaign carried out in September and October 2003. Drill Site 1 was moved ~50 m based on recommendations built on data from Line 15 and Line 14 of the Fast-Turnoff TEM survey.

  4. Optical and TEM study of shock metamorphism from the Sedan test site

    NASA Astrophysics Data System (ADS)

    Gratz, A. J.

    Thus far, detailed petrologic studies of shock metamorphism have been performed on samples recovered from laboratory experiments and on a few natural impactites. The loading history of these samples is quite different: In particular, laboratory experiments spend only a short time (less than 1 microsec) at peak pressure, whereas natural impactites may have stress pulses from 0.1 - 1 ms. On the other hand, laboratory experiments have known stress histories; natural impactites do not. Natural samples are also subjected to thousands or millions of years of postshock annealing and/or weathering. A useful intermediate case is that of nuclear detonation. Stress pulses for these events can reach 0.1 ms or higher, and samples are obtained in pristine condition. All three types of loading produce stresses of hundreds of kilobars. Samples studied were taken from the Sedan nulcear test site, and consist of a coarse-grained granodiorite containing quartz, K-feldspar, cordierite, and hornblende. Samples were studied optically in this section, then were thinned with an ion mill and studied by transmission electron microscopy (TEM). Optically, quartz and K-feldspar displayed numerous sets of planar deformation features (PDF's) identical to the nondecorated PDF's seen in laboratory samples and many natural impactites. TEM study showed that the PDF's in quartz and feldspar corresponded to densely packed wide transformation lamellae identical to those described in laboratory studies. The transformation lamellae in both minerals were amorphous, with no sign of high-pressure phases. In the case of K-feldspar only, narrow sublamellae extended outward from some wide lamellae. Quartz, which was more abundant and studied more extensively, contained no shock-induced dislocations. Some planar features were also seen in cordierite, but could not be identified due to rapid beam damage. No shock defects were seen in hornblende in TEM. The shock-induced defects present at the Sedan site are very

  5. Shallow geothermal exploration using SkyTEM data: the VIGOR experiment

    NASA Astrophysics Data System (ADS)

    Santilano, Alessandro; Manzella, Adele; Viezzoli, Andrea; Menghini, Antonio; Donato, Assunta; Montanari, Domenico; Maggi, Sabino; Rizzo, Enzo

    2013-04-01

    Within the "VIGOR" project, aimed at assessing the geothermal potential of four regions in southern Italy, helicopter geophysical electromagnetic (SkyTEM) data have been acquired, modeled and interpreted. The SkyTEM system provides, after data acquisition, analysis, processing and modeling, a distribution volume of electrical resistivity, spanning an investigation depth from ground surface of few hundred meters, depending on resistivity condition. Results were used also to characterize the main geological units outcropping in the region and extend the investigation at depth. Resistivity is an important physical parameter for geothermal investigation, since it proved to be very effective in mapping anomalies due to hydrothermal fluid circulation, which usually has high salt content and produces clayey alteration minerals. Besides, resistivity data may help in characterizing hydrogeological or tectonic features. The attempt is also to define relations between resistivity distribution, lithological units and thermal conductivity. The geophysical survey was carried out in Sicily, Italy, in late 2011, covering two areas. SkyTEM data have been acquired in a series of flight lines and were then processed and inverted. In the "Termini" area the flight line spacing had 150 m separation. In the "Western Sicily" area two different line spacing were used: the 1 km spacing was used for the regional mapping, whereas for infill areas, around the main hydrothermal springs, the flight lines had 100 m spacing. After acquisition, data were analysed and processed. Inversions were then carried out using the quasi 3-D Spatially Constrained Inversion (SCI). The obtained resistivity volume has then been the base for a detailed lithological and geothermal interpretation. Lithological and geological maps were used to constrain surface condition and to understand the resistivity ranges of the different lithological units. On the base of resistivity values, lithological units were combined to

  6. Characterization of nanoscale local lattice strains in silicon CMOS devices by TEM/CBED

    NASA Astrophysics Data System (ADS)

    Huang, Jiang

    Strained-Si technology has become one of the leading approaches to further improve the performance of the metal-oxide-semiconductor field effect transistors (MOSFETs) as traditional device scaling faces its physical limitation. In particular, mechanical strain induced in the Si channel region is used to increase the carrier mobility and the transistor drive current. To be able to understand and engineer the local lattice strain incorporated in the nanoscale device region, a strain measurement technique with high spatial resolution and high sensitivity is essential. Currently, transmission electron microscope (TEM)/convergent beam electron diffraction (CBED) is the only method to measure local changes in lattice parameters due to strain in advanced CMOS devices, because this technique provides nanometer spatial resolution and strain sensitivity on the order of 10-4. In this study, a novel experimental methodology is developed to measure the strain effectively and efficiently. Site-specific TEM samples are prepared by focused ion beam (FIB) with controlled thickness. Zone axes such as <230>, <340>, <560> and <910> are evaluated for obtaining CBED patterns. The specimen-tilt projection and dynamical effects related to the zone axis are discussed. CBED pattern simulation and matching procedures are explained to extract the strain tensors. The accuracy of the strain measurement depends on the clarity of the CBED pattern, which can be improved by using an energy-filter or sample cooling stage. The direct strain measurements are performed in sub-100 nm CMOS devices with either structure-induced or process-induced strains. It is found that the compressive strains are induced when the shallow trench structure (STI) is filled with isolation films. The compressive strains on the order of 10 -3 are observed under the gate region in a Si <110> PMOS transistor with a 37 nm gate length. One-dimensional quantitative strain-mapping is demonstrated using the nanometer probe. The

  7. Optical and TEM study of shock metamorphism from the Sedan test site

    NASA Technical Reports Server (NTRS)

    Gratz, A. J.

    1992-01-01

    Thus far, detailed petrologic studies of shock metamorphism have been performed on samples recovered from laboratory experiments and on a few natural impactites. The loading history of these samples is quite different: In particular, laboratory experiments spend only a short time (less than 1 microsec) at peak pressure, whereas natural impactites may have stress pulses from 0.1 - 1 ms. On the other hand, laboratory experiments have known stress histories; natural impactites do not. Natural samples are also subjected to thousands or millions of years of postshock annealing and/or weathering. A useful intermediate case is that of nuclear detonation. Stress pulses for these events can reach 0.1 ms or higher, and samples are obtained in pristine condition. All three types of loading produce stresses of hundreds of kilobars. Samples studied were taken from the Sedan nulcear test site, and consist of a coarse-grained granodiorite containing quartz, K-feldspar, cordierite, and hornblende. Samples were studied optically in this section, then were thinned with an ion mill and studied by transmission electron microscopy (TEM). Optically, quartz and K-feldspar displayed numerous sets of planar deformation features (PDF's) identical to the nondecorated PDF's seen in laboratory samples and many natural impactites. TEM study showed that the PDF's in quartz and feldspar corresponded to densely packed wide transformation lamellae identical to those described in laboratory studies. The transformation lamellae in both minerals were amorphous, with no sign of high-pressure phases. In the case of K-feldspar only, narrow sublamellae extended outward from some wide lamellae. Quartz, which was more abundant and studied more extensively, contained no shock-induced dislocations. Some planar features were also seen in cordierite, but could not be identified due to rapid beam damage. No shock defects were seen in hornblende in TEM. The shock-induced defects present at the Sedan site are very

  8. In situ TEM investigations of mineral growth through oriented attachment of nanoparticles

    NASA Astrophysics Data System (ADS)

    Li, D.; Nielsen, M.; Lee, J. R.; Frandsen, C.; Banfield, J. F.; Kisailus, D.; De Yoreo, J.

    2012-12-01

    The growth of crystals through aggregation and coalescence of nanoparticles is now recognized as a widespread phenomenon in biomineral, biomimetic and natural systems, and during synthetic production of nanoparticles and nanowires. The resulting crystals often exhibit complex forms ranging from quasi-one-dimensional chains to 3D hierarchical and self-similar superstructures. Yet the final structure typically diffracts as a single crystal, implying that the primary particles aligned during growth. When coalignment is accompanied by coalescence, this growth process is often referred to as oriented attachment (OA). OA is now recognized as an important mechanism of crystal growth in many materials in the environment. However, the pathway by which OA occurs has not been established. Although the preservation of primary particle morphology and formation of twins and stacking faults at particle-particle boundaries strongly suggest a sequence of whole particle alignment followed by interface elimination, atom-by-atom reorientation via dislocation and grain-boundary migration after attachment are another potential mechanism. If indeed the primary particles align before attachment, the dynamics of that process and the forces that drive it have yet to be revealed. To achieve this understanding we are investigating crystal nucleation and oriented attachment in a number of systems, such as iron oxides and oxyhydroxide as well as titanium dioxide, through in situ and ex situ TEM. We performed high-resolution TEM using a fluid cell to directly observe oriented attachment of iron oxyhydroxide nanoparticles. The particles undergo continuous rotation and interaction until they find a perfect lattice match. A sudden jump to contact then occurs over less than 1 nanometer, followed by lateral atom-by-atom addition initiated at the contact point. Interface elimination proceeds at a rate consistent with the curvature dependence of the Gibbs free energy. Measured translational and

  9. In situ TEM visualization of superior nanomechanical flexibility of shear-exfoliated phosphorene

    NASA Astrophysics Data System (ADS)

    Xu, Feng; Ma, Hongyu; Lei, Shuangying; Sun, Jun; Chen, Jing; Ge, Binghui; Zhu, Yimei; Sun, Litao

    2016-07-01

    Recently discovered atomically thin black phosphorus (called phosphorene) holds great promise for applications in flexible nanoelectronic devices. Experimentally identifying and characterizing nanomechanical properties of phosphorene are challenging, but also potentially rewarding. This work combines for the first time in situ transmission electron microscopy (TEM) imaging and an in situ micro-manipulation system to directly visualize the nanomechanical behaviour of individual phosphorene nanoflakes. We demonstrate that the phosphorene nanoflakes can be easily bent, scrolled, and stretched, showing remarkable mechanical flexibility rather than fracturing. An out-of-plane plate-like bending mechanism and in-plane tensile strain of up to 34% were observed. Moreover, a facile liquid-phase shear exfoliation route has been developed to produce such mono-layer and few-layer phosphorene nanoflakes in organic solvents using only a household kitchen blender. The effects of surface tensions of the applied solvents on the ratio of average length and thickness (L/T) of the nanoflakes were studied systematically. The results reported here will pave the way for potential industrial-scale applications of flexible phosphorene nanoelectronic devices.Recently discovered atomically thin black phosphorus (called phosphorene) holds great promise for applications in flexible nanoelectronic devices. Experimentally identifying and characterizing nanomechanical properties of phosphorene are challenging, but also potentially rewarding. This work combines for the first time in situ transmission electron microscopy (TEM) imaging and an in situ micro-manipulation system to directly visualize the nanomechanical behaviour of individual phosphorene nanoflakes. We demonstrate that the phosphorene nanoflakes can be easily bent, scrolled, and stretched, showing remarkable mechanical flexibility rather than fracturing. An out-of-plane plate-like bending mechanism and in-plane tensile strain of up to

  10. Quasi-TEM electromagnetic modes of a plasma waveguide with a nonsimply connected cross section in an external magnetic field

    SciTech Connect

    Kartashov, I. N. Kuzelev, M. V.

    2014-12-15

    Electromagnetic modes of a plasma waveguide with a nonsimply connected cross section in an external magnetic field are investigated. The existence of quasi-TEM modes in a finite-strength magnetic field is demonstrated. It is shown that, in the limits of infinitely strong and zero magnetic fields, this mode transforms into a true TEM mode. The possibility of excitation of such modes by an electron beam in the regime of the anomalous Doppler effect is analyzed.

  11. TEM Study of Precipitation in a NiAl-3Ti-0.5Hf Single-Crystal Alloy

    NASA Technical Reports Server (NTRS)

    Garg, A.; Noebe, R. D.; Howe, J. M.; Wilson, A. W.; Levit, V.

    1996-01-01

    Samples for transmission electron microscopy (TEM) were prepared from 3 mm diameter cylinders electro-discharge machined from the heat-treated ingots. Slices sectioned from the cylinders were mechanically ground and electrochemically thinned in a twinjet Tenupol-3 polisher. Microstructural and energy-dispersive X-ray spectroscopy (EDXS) studies were conducted in a Philips 400T TEM equipped with a double tilt goniometer and a KEVEX Si/Li X-ray detector.

  12. In situ TEM investigation of microstructural behavior of superplastic Al–Mg–Sc alloy

    SciTech Connect

    Dám, Karel; Lejček, Pavel; Michalcová, Alena

    2013-02-15

    Dynamic changes in microstructure of the superplastic ultrafine-grained Al–3Mg–0.2Sc (wt.%) alloy refined by equal-channel angular pressing (ECAP). were observed by in situ transmission electron microscopy at temperatures up to 300 °C (annealing and tensile deformation) in order to simulate the initial stages of superplastic testing. It was found that the microstructure changes significantly during the preheating before the superplastic deformation, which was accompanied by decreased microhardness. During the deformation at 300 °C, high dislocation activity as well as motion of low-angle grain boundaries was observed while high-angle grain boundaries did not move due to the presence of scandium in the alloy. - Highlights: ► We performed in situ TEM annealing and straining on superplastic Al–Mg–Sc alloy. ► We simulated the conditions of early stages of superplastic testing. ► Significant changes in microstructure occur during preheating before deformation.

  13. A Rapid Method for Viral Particle Detection in Viral-Induced Gastroenteritis: A TEM Study

    NASA Astrophysics Data System (ADS)

    Hicks, M. John; Barrish, James P.; Hayes, Elizabeth S.; Leer, Laurie C.; Estes, Mary K.; Cubitt, W. D.

    1995-10-01

    Infectious gastroenteritis is a common cause of hospitalization in the pediatric population. The most frequent cause of gastroenteritis is viral in origin. The purpose of this study was to compare a rapid modified negative-staining TEM method with the conventional pseudoreplica technique in detection of viral particles in fecal samples from children with viral gastroenteritis. The modified negative-staining method resulted in a significantly higher (2.5 ± 0.5, p = 0.02) viral rating score than that for the conventional pseudoreplica technique (1.7 ± 0.4). In addition, the preparation time for the negative-staining method was approximately one fifth that for the conventional pseudoreplica technique. Rapid diagnosis of viral gastroenteritis may be made by ultrastructural detection of viral particles in fecal samples using the negative staining technique.

  14. A TEM Investigation of the Fine-Grained Matrix of the Martian Basaltic Breccia NWA 7034

    NASA Technical Reports Server (NTRS)

    Muttik, N.; Keller, L. P.; Agee, C. B.; McCubbin, F. M.; Santos, A. R.; Rahman, Z.

    2014-01-01

    The martian basaltic breccia NWA 7034 is characterized by fine-grained groundmass containing several different types of mineral grains and lithologic clasts. The matrix composition closely resembles Martian crustal rock and soil composition measured by recent rover and orbiter missions. The first results of NWA 7034 suggest that the brecciation of this martian meteorite may have formed due to eruptive volcanic processes; however, impact related brecciation processes have been proposed for paired meteorites NWA 7533 and NWA 7475]. Due to the very fine grain size of matrix, its textural details are difficult to resolve by optical and microprobe observations. In order to examine the potential nature of brecciation, transmission electron microscopy (TEM) studies combined with focused ion-beam technique (FIB) has been undertaken. Here we present the preliminary observations of fine-grained groundmass of NWA 7034 from different matrix areas by describing its textural and mineralogical variations and micro-structural characteristics.

  15. Laser Based In Situ Techniques: Novel Methods for Generating Extreme Conditions in TEM Samples

    SciTech Connect

    Taheri, M; Lagrange, T; Reed, B; Armstrong, M; Campbell, G; DeHope, W; Kim, J; King, W; Masiel, D; Browning, N

    2008-02-25

    The Dynamic Transmission Electron Microscope (DTEM) is introduced as a novel tool for in situ processing of materials. Examples of various types of dynamic studies outline the advantages and differences of laser-based heating in the DTEM in comparison to conventional (resistive) heating in situ TEM methods. We demonstrate various unique capabilities of the drive laser, namely, in situ processing of nanoscale materials, rapid and high temperature phase transformations, and controlled thermal activation of materials. These experiments would otherwise be impossible without the use of the DTEM drive laser. Thus, the potential of the DTEM to as a new technique to process and characterize the growth of a myriad of micro and nanostructures is demonstrated.

  16. A Microanalytical (TEM) Study of Fine-grained Chondrule Rims in NWA 5717

    NASA Technical Reports Server (NTRS)

    Bigolski, J. N.; Frank, D. R.; Zolensky, Michael E.; Weisberg, M. K.; Ebel, D. S.; Rahman, Z.

    2013-01-01

    Northwest Africa (NWA) 5717 is a highly primitive ordinary chondrite of petrologic type 3.05 with ubiquitous fine-grained chondrule rims [1, 2]. Rims appear around approximately 60% of chondrules and are comprised of micron-sized mineral and lithic fragments and microchondrules that are embdedded in an FeO-rich submicron groundmass that compositionally resembles fayalitic olivine. Some rim clasts appear overprinted with FeO-rich material, suggesting secondary alteration that postdates rim formation. Here we present a microanalytical (TEM) study of the submicron component (i.e. the groundmass) of the rims in order to determine the crystal structures and compositions of their constituent phases and decipher the accretion and alteration history recorded in rims.

  17. Nanoribbons from conjugated macromolecules on amorphous substrates observed by SFM and TEM

    NASA Astrophysics Data System (ADS)

    Samori, Paolo; Sikharulidze, Irakli; Francke, Viola; Müllen, Klaus; Rabe, Jürgen P.

    1999-03-01

    Micrometre long nanoribbons have been grown from solutions of functionalized poly( para-phenyleneethynylene)s (PPE)s on noncrystalline insulating substrates including glass and carbon coated copper grids. Tapping mode scanning force microscopy (SFM) and transmission electron microscopy (TEM) revealed that these nanostructures possess a molecular cross section with a typical thickness of 2-3 molecular layers and a width which reflects the distribution of macromolecular lengths. The ribbons are therefore quite similar to the ones found on the crystalline mica substrate except that they are not oriented within the surface plane. This indicates that the growth of these architectures from solution is mainly governed by intermolecular interactions between the π-conjugated macromolecules. The possibility to self-assemble these nanoribbons also on amorphous silica opens a prospect for their application as molecular nanowires bridging gold nanoelectrodes grown on oxidized silicon wafers.

  18. Image processing enhancement of high-resolution TEM micrographs of nanometer-size metal particles

    NASA Technical Reports Server (NTRS)

    Artal, P.; Avalos-Borja, M.; Soria, F.; Poppa, H.; Heinemann, K.

    1989-01-01

    The high-resolution TEM detectability of lattice fringes from metal particles supported on substrates is impeded by the substrate itself. Single value decomposition (SVD) and Fourier filtering (FFT) methods were applied to standard high resolution micrographs to enhance lattice resolution from particles as well as from crystalline substrates. SVD produced good results for one direction of fringes, and it can be implemented as a real-time process. Fourier methods are independent of azimuthal directions and allow separation of particle lattice planes from those pertaining to the substrate, which makes it feasible to detect possible substrate distortions produced by the supported particle. This method, on the other hand, is more elaborate, requires more computer time than SVD and is, therefore, less likely to be used in real-time image processing applications.

  19. A FIB/TEM Study of a Complex Wark-Lovering Rim on a Vigarano CAI

    NASA Technical Reports Server (NTRS)

    Keller, L. P.; Needham, A. W.; Messenger, S.

    2013-01-01

    Wark-Lovering (WL) rims are thin multilayered mineral sequences that surround most Ca, Al-rich inclusions (CAIs). Several processes have been proposed for WL rim formation, including condensation, flash-heating or reaction with a nebular reservoir, or combinations of these [e.g. 1-7], but no consensus exists. Our previous coordinated transmission electron microscope (TEM) and NanoSIMS O isotopic measurements showed that a WL rim experienced flash heating events in a nebular environment with planetary O isotopic composition, distinct from the (16)O-rich formation environment [6]. Our efforts have focused on CAIs from the CV(sub red) chondrites, especially Vigarano, because these have escaped much of the parent body alteration effects that are common in CAIs from CV(sub ox) group.

  20. A TEM Study of Creep Deformation Mechanisms in Allvac 718Plus

    SciTech Connect

    Unocic, Raymond R; Unocic, Kinga A; Hayes, Robert; Daehn, Glenn; Mills, Michael J.

    2010-01-01

    A preliminary study on the evolution of creep deformation substructure in Ni-base superalloy Allvac 718Plus has been performed. Specimens crept at 620 MPa and at temperatures ranging from 690-732 C were examined utilizing diffraction contrast TEM characterization techniques. Creep was interrupted at 1-2.5% strain in order to study the deformation substructure following a limited amount of deformation. The dominant deformation modes at each of the test temperatures were highly planar in nature and involved shearing of the matrix and precipitates on {111} glide planes. In addition, paired a/2<110> dislocations were evident which suggest an antiphase boundary shearing mechanism. Creep induced microtwinning was also observed at the highest creep temperature which was created by identical a/6<112> Shockley partial dislocations that shear the matrix and precipitates on consecutive close packed {111} glide planes.

  1. In situ TEM imaging of CaCO₃ nucleation reveals coexistence of direct and indirect pathways.

    PubMed

    Nielsen, Michael H; Aloni, Shaul; De Yoreo, James J

    2014-09-01

    Mechanisms of nucleation from electrolyte solutions have been debated for more than a century. Recent discoveries of amorphous precursors and evidence for cluster aggregation and liquid-liquid separation contradict common assumptions of classical nucleation theory. Using in situ transmission electron microscopy (TEM) to explore calcium carbonate (CaCO3) nucleation in a cell that enables reagent mixing, we demonstrate that multiple nucleation pathways are simultaneously operative, including formation both directly from solution and indirectly through transformation of amorphous and crystalline precursors. However, an amorphous-to-calcite transformation is not observed. The behavior of amorphous calcium carbonate upon dissolution suggests that it encompasses a spectrum of structures, including liquids and solids. These observations of competing direct and indirect pathways are consistent with classical predictions, whereas the behavior of amorphous particles hints at an underlying commonality among recently proposed precursor-based mechanisms. PMID:25190792

  2. Quantitative TEM analysis of precipitation and grain boundary segregation in neutron irradiated EUROFER 97

    NASA Astrophysics Data System (ADS)

    Dethloff, Christian; Gaganidze, Ermile; Aktaa, Jarir

    2014-11-01

    Characterization of irradiation induced microstructural defects is essential for assessing the applicability of structural steels like the Reduced Activation Ferritic/Martensitic steel EUROFER 97 in upcoming fusion reactors. In this work Transmission Electron Microscopy (TEM) is used to analyze the types and structure of precipitates, and the evolution of their size distributions and densities caused by neutron irradiation to a dose of 32 displacements per atom (dpa) at 330-340 °C in the irradiation experiment ARBOR 1. A significant growth of MX and M23C6 type precipitates is observed after neutron irradiation, while the precipitate density remains unchanged. Hardening caused by MX and M23C6 precipitate growth is assessed by applying the Dispersed Barrier Hardening (DBH) model, and shown to be of minor importance when compared to other irradiation effects like dislocation loop formation. Additionally, grain boundary segregation of chromium induced by neutron irradiation was investigated and detected in irradiated specimens.

  3. Materials science applications of a 120 kV FEG TEM/STEM: Triskaidekaphilia

    SciTech Connect

    Bentley, J.; Fisher, A.T.; Kenik, E.A.; Wang, Z.L.

    1991-01-01

    The introduction by several manufacturers of 200kV transmission electron microscopes (TEM) equipped with field emission guns affords the opportunity to assess their potential impact on materials science by examining applications of similar 100-120kV instruments that have been in use for more than a decade. This summary is based on results from a Philips EM400T/FEG configured as an analytical electron microscope (AEM) with a 6,585 scanning transmission (STEM) unit, EDAX 9100/70 or 9900 energy dispersive X-ray spectroscopy (EDS) systems, and Gatan 607 serial- or 666 parallel-detection electron energy-loss spectrometers (EELS). Examples in four areas that illustrate applications that are impossible or so difficult as to be impracticable with conventional thermionic electron guns are described.

  4. In situ TEM/SEM electronic/mechanical characterization of nano material with MEMS chip

    NASA Astrophysics Data System (ADS)

    Yuelin, Wang; Tie, Li; Xiao, Zhang; Hongjiang, Zeng; Qinhua, Jin

    2014-08-01

    Our investigation of in situ observations on electronic and mechanical properties of nano materials using a scanning electron microscope (SEM) and a transmission electron microscope (TEM) with the help of traditional micro-electro-mechanical system (MEMS) technology has been reviewed. Thanks to the stability, continuity and controllability of the loading force from the electrostatic actuator and the sensitivity of the sensor beam, a MEMS tensile testing chip for accurate tensile testing in the nano scale is obtained. Based on the MEMS chips, the scale effect of Young's modulus in silicon has been studied and confirmed directly in a tensile experiment using a transmission electron microscope. Employing the nanomanipulation technology and FIB technology, Cu and SiC nanowires have been integrated into the tensile testing device and their mechanical, electronic properties under different stress have been achieved, simultaneously. All these will aid in better understanding the nano effects and contribute to the designation and application in nano devices.

  5. Use of an ultrasonic/sonic driller/corer to obtain sample powder for chemin, a combined XRD/XRF instrument.

    SciTech Connect

    Chipera, S. J.; Bish, D. L.; Vaniman, D. T.; Sherrit, S.; Bar-Cohen, Yoseph; Blake, D.

    2003-01-01

    One of the technical issues that must be addressed before landing an XRD,iXRF spectrometer on an extraterrestrial body is how best to obtain a representative sample powder for analysis. For XRD powder diffraction analyses, it is beneficial to have a powder that is extremely fine grained to reduce preferred orientation effects and to provide a statistically significant number of crystallites to the Xray beam. Although a 2 dimensional detector as used in the CHEMIN instrument will produce good results with poorly prepared powders, the quality of the data will improve with the quality of the sample powder.

  6. Transmission Kikuchi diffraction and transmission electron forescatter imaging of electropolished and FIB manufactured TEM specimens

    SciTech Connect

    Zieliński, W. Płociński, T.; Kurzydłowski, K.J.

    2015-06-15

    We present a study of the efficiency of the utility of scanning electron microscope (SEM)-based transmission methods for characterizing grain structure in thinned bulk metals. Foils of type 316 stainless steel were prepared by two methods commonly used for transmission electron microscopy — double-jet electropolishing and focused ion beam milling. A customized holder allowed positioning of the foils in a configuration appropriate for both transmission electron forward scatter diffraction, and for transmission imaging by the use of a forescatter detector with two diodes. We found that both crystallographic orientation maps and dark-field transmitted images could be obtained for specimens prepared by either method. However, for both methods, preparation-induced artifacts may affect the quality or accuracy of transmission SEM data, especially those acquired by the use of transmission Kikuchi diffraction. Generally, the quality of orientation data was better for specimens prepared by electropolishing, due to the absence of ion-induced damage. - Highlights: • The transmission imaging and diffraction techniques are emerging in scanning electron microscopy (SEM) as promising new field of materials characterization. • The manuscript titled: “Transmission Kikuchi Diffraction and Transmission Electron Forescatter Imaging of Electropolished and FIB Manufactured TEM Specimens” documents how different specimen thinning procedures can effect efficiency of transmission Kikuchi diffraction and transmission electron forescatter imaging. • The abilities to make precision crystallographic orientation maps and dark-field images in transmission was studied on electropolished versus focus ion beam manufactured TEM specimens. • Depending on the need, electropolished and focused ion beam technique may produce suitable specimens for transmission imaging and diffraction in SEM.

  7. Nano-scale Petrography of Permian-Basin Halite by TEM

    NASA Astrophysics Data System (ADS)

    Nemer, M. B.; Powers, D. W.; Ismail, A. E.

    2009-12-01

    Halite from the upper Permian Salado Formation of the Permian basin has been extensively studied over the last century. Few researchers, however, have looked at these units at the nano-scale. This is partially due to the difficulty of preparing soft-ionic-crystal samples for TEM studies, and because of the inherent artifacts created in the sectioning and imaging process. We have ultramicrotomed and imaged halite from the Salado in a 200kV TEM. An interesting find is the presence of a ≈ 30 nm transition zone of crystal surrounding some (but not all) fluid inclusions in primary halite (chevron crystal). The transition-zone crystal appears to be oriented differently than the bulk halite crystal away from the transition zone. The thickness of the transition zone does not seem to be sensitive to the dimensions of the inclusion which rules out pressure-temperature changes in solubility in such a small volume. The cause of these transition zones is unknown. Several interesting petrofabrics can also be seen in the primary halite. Fluid-inclusion-banded halite contains bands of very small (< 100 nm) fluid inclusions. Some inclusions appear to have trails of smaller drops, as if due to a drop-breakup event. This is curious because we don’t expect breakup events in a primary crystal. A “myrmekite” like texture has been observed that contains a series of indentations and spurs along the bedding plane. A turbulent fabric has been observed which contains small eddy-like structures . At this time, we are not able to interpret these fabrics with confidence or determine which are real and which are artifacts. This work is considered preliminary and should not be cited, as some samples were not collected under the Waste Isolation Pilot Plant (WIPP) Quality Assurance (QA) program. This work will be repeated in the future with full WIPP QA.

  8. Carbon investigation of two Stardust particles: A TEM, NanoSIMS, and XANES study

    SciTech Connect

    Matrajt, G.; Ito, M; Wirick, S; Messenger, S; Brownlee, D; Joswiak, D; Flynn, G; Sandford, S; Snead, C; Westphal, A

    2008-01-01

    In this work we present the results of a systematic search for cometary organics in 14 Stardust particles (particles from comet 81P/Wild 2, captured by NASA's Stardust mission) by TEM and multidisciplinary studies (XANES and NanoSIMS) of Febo and Ada, two of the organic-bearing particles identified. The combination of the three analytical techniques has established the presence of organic, cometary C in both particles. Using energy-filtered and high-resolution imaging it was shown that the C is amorphous and rare, given that it is found in grains =200 nm in size that are not abundant throughout the particles. The XANES maps and spectra of the carbonaceous areas identified with the TEM have shown that the carbonaceous material is organic due to the presence of carbonyl (C=O) functional groups and the overlapping of C and N on the same grains. In addition, several different C-XANES spectra were obtained from the same particle, suggesting that there is diversity in the types of carbonaceous phases present in these particles, as well as a heterogeneous distribution of the carbonaceous phases within these particles. The C-XANES spectra obtained are different from C-XANES spectra of carbonaceous chondrites and IDPs. In the particle Febo we found five spots showing a pronounced enrichment in the isotope {sup 15}N ({sigma}{sup 15} ffffrom 420 to 639 {+-} 20 to 70%, 1S) that were clearly associated with the C-rich regions. The carbonaceous material has approximately solar C and D/H isotopic compositions, and the bulk O isotopic composition was found to be S{sup 17} O=-18 {+-} 13% and {sigma}{sup 18} O=-37 {+-}12% (aS).

  9. Design of high-brightness TEM00-mode solar-pumped laser for renewable material processing

    NASA Astrophysics Data System (ADS)

    Liang, D.; Almeida, J.

    2014-08-01

    The conversion of sunlight into laser light by direct solar pumping is of ever-increasing importance because broadband, temporally constant, sunlight is converted into laser light, which can be a source of narrowband, collimated, rapidly pulsed, radiation with the possibility of obtaining extremely high brightness and intensity. Nonlinear processes, such as harmonic generation, might be used to obtain broad wavelength coverage, including the ultraviolet wavelengths, where the solar flux is very weak. The direct excitation of large lasers by sunlight offers the prospect of a drastic reduction in the cost of coherent optical radiation for high average power materials processing. This renewable laser has a large potential for many applications such as high-temperature materials processing, renewable magnesium-hydrogen energy cycle and so on. We propose here a scalable TEM00 mode solar laser pumping scheme, which is composed of four firststage 1.13 m diameter Fresnel lenses with its respective folding mirrors mounted on a two-axis automatic solar tracker. Concentrated solar power at the four focal spots of these Fresnel lenses are focused individually along a common 3.5 mm diameter, 70 mm length Nd:YAG rod via four pairs of second-stage fused-silica spherical lenses and third-stage 2D-CPCs (Compound Parabolic Concentrator), sitting just above the laser rod which is also double-pass pumped by four V-shaped pumping cavities. Distilled water cools both the rod and the concentrators. 15.4 W TEM00 solar laser power is numerically calculated, corresponding to 6.7 times enhancement in laser beam brightness.

  10. TEM Study of Aerosol Particles in Brown Haze Episodes over Northern China in Spring 2007

    NASA Astrophysics Data System (ADS)

    Li, W.; Shao, L.; Buseck, P. R.

    2008-12-01

    Airborne aerosol collections were performed in eight brown haze episodes from 31 May to 21 June 2007 in Beijing, China. Morphologies, compositions, and mixing states of individual aerosol particles having different sizes were obtained using transmission electron microscopy (TEM). Aerosol particle types less than 2 μ m in diameter include mineral dust, fly ash, soot, organic material, and K-rich, S-rich, and metal particles (Fe- and Zn-rich). Mineral dust particles dominate in the range of 2 to 10 μ m. In addition to finding contributions from vehicle emissions and soil dust in Beijing, TEM results from the study provide new insights into sources such as agricultural biomass burning, industrial activities, and waste incineration. These sources can contribute not only great amounts of K-rich and metal particles but also reactive gases such as NH3, NOx, SO2, and VOCs to the haze. More than 80% of the analyzed aerosol particles are internally mixed. K- and S-rich particles tend to be coagulated with fly ash, soot, metal, and fine-grained mineral dust particles. Organic materials can act as inclusions in the K- and S-rich particles and their coatings. Over 90% of the analyzed internally mixed mineral particles are covered with Ca-, Mg-, or Na-rich coatings, and only 8% are associated with K- or S-rich coatings. The compositions of Ca-, Mg-, and Na-rich coatings suggest that they are possibly nitrates mixed with minor sulfates and chlorides. Calcium sulfate particles with diameters from 10 to 500 nm were also detected within Ca(NO3)2 and Mg(NO3)2 coatings. These results indicate that mineral dust particles in the brown haze episodes participated in heterogeneous reactions in the atmosphere with one or more of SO2, NO2, HCl, and HNO3. The development of coatings altered some mineral dust particles from hydrophobic to hydrophilic.

  11. Crystal polymer interaction with new injectable bone substitute; SEM and Hr TEM study.

    PubMed

    Daculsi, G; Rohanizadeh, R; Weiss, P; Bouler, J M

    2000-04-01

    A composite constituted of calcium phosphate (CaP) granules and a hydrophilic polymer as a carrier (hydroxy-propyl-methyl cellulose, HPMC) was developed to be an injectable bone substitute (IBS, CNRS patent). IBS is a composite and not an ionic cement. The composite obtained is ready to use and sterile. Chemical interactions between organic and inorganic components appeared during the association of the two. The interactions of the CaP and the polymer have been studied using scanning electron microscopy (SEM), electron microprobe (EDX), and high-resolution transmission electron microscopy (HrTEM) SEM revealed a degradation of the granules into smaller particles while EDX was unable to show significant changes in the Ca/P ratio during aging of the composite. With Hr TEM, however, we observed hydrolysis (process of dissolution and precipitation) from the surface to about 13 nm into the HA crystals and occasional dissolution with precipitation of beta-TCP crystals. In HA, the first zone of interaction consisted of a single layer of small globular crystals of 2 to 3 nm in diameter. Numerous lattice patterns in all three axes could be observed. Under the globular crystals zone, the inter-reticular distances of the single crystals appeared enlarged by 1.2% (from 0.817 to 0.827 nm). The enlargement seems to correspond to diffusion of HPO(4) into the crystal lattice. In beta-TCP crystals, dissolution was observed to be several nanometers deep, but globular surface precipitation rarely was observed. With time or after steam sterilization, no changes were observed. These data demonstrate the strong interactions of the hydrophylic polymer with calcium phosphate, but only in the first several nanometers of thickness.

  12. High-resolution methane emission estimates using surface measurements and the InTEM inversion system.

    NASA Astrophysics Data System (ADS)

    Connors, Sarah; Manning, Alistair; Robinson, Andrew; Riddick, Stuart; Forster, Grant; Oram, Dave; O'Doherty, Simon; Harris, Neil

    2015-04-01

    High quality GHG emission estimates will be required to successfully tackle climate change. There is a growing need for comparisons between emission estimates produced using bottom-up and top-down techniques at high spatial resolution. Here, a top-down inversion approach combining multi-year atmospheric measurements and an inversion model, InTEM, was used to estimate methane emissions for a region in the South East of the UK (~100 x 150 km). We present results covering a 2-year period (July 2012 - July 2014) in which atmospheric methane concentrations were recorded at 1 - 2 minute time-steps at four locations within the region of interest. Precise measurements were obtained using gas chromatography with flame ionisation detection (GC-FID) for all sites except one, which used a PICARRO Cavity Ring-Down Spectrometer (CRDS). These observations, along with the UK Met Office's Lagrangian particle dispersion model, NAME, were used within InTEM to produce the methane emission fields. We present results from both Bayesian and non-prior based inversion analysis at varying spatial resolutions, for annual, seasonal and monthly time frames. These results are compared with the UK National Atmospheric Emissions Inventory (NAEI) which is compiled using bottom-up methods and available at 1x1 km resolution. A thorough assessment of uncertainty is incorporated into this technique which is represented in the results. This project is part of the UK GAUGE campaign which aims to produce robust estimates of the UK GHG budget using new and existing measurement networks (e.g. the UK DECC GHG network) and modelling activities at a range of scales.

  13. Monitoring the Stability of Perfluorocarbon Nanoemulsions by Cryo-TEM Image Analysis and Dynamic Light Scattering

    PubMed Central

    Grapentin, Christoph; Barnert, Sabine; Schubert, Rolf

    2015-01-01

    Perfluorocarbon nanoemulsions (PFC-NE) are disperse systems consisting of nanoscale liquid perfluorocarbon droplets stabilized by an emulsifier, usually phospholipids. Perfluorocarbons are chemically inert and non-toxic substances that are exhaled after in vivo administration. The manufacture of PFC-NE can be done in large scales by means of high pressure homogenization or microfluidization. Originally investigated as oxygen carriers for cases of severe blood loss, their application nowadays is more focused on using them as marker agents in 19F Magnetic Resonance Imaging (19F MRI). 19F is scarce in organisms and thus PFC-NE are a promising tool for highly specific and non-invasive imaging of inflammation via 19F MRI. Neutrophils, monocytes and macrophages phagocytize PFC-NE and subsequently migrate to inflamed tissues. This technique has proven feasibility in numerous disease models in mice, rabbits and mini pigs. The translation to clinical trials in human needs the development of a stable nanoemulsion whose droplet size is well characterized over a long storage time. Usually dynamic light scattering (DLS) is applied as the standard method for determining particle sizes in the nanometer range. Our study uses a second method, analysis of transmission electron microscopy images of cryo-fixed samples (Cryo-TEM), to evaluate stability of PFC-NE in comparison to DLS. Four nanoemulsions of different composition are observed for one year. The results indicate that DLS alone cannot reveal the changes in particle size, but can even mislead to a positive estimation of stability. The combination with Cryo-TEM images gives more insight in the particulate evolution, both techniques supporting one another. The study is one further step in the development of analytical tools for the evaluation of a clinically applicable perfluorooctylbromide nanoemulsion. PMID:26098661

  14. Coupling spindle position with mitotic exit in budding yeast: The multifaceted role of the small GTPase Tem1

    PubMed Central

    Scarfone, Ilaria; Piatti, Simonetta

    2015-01-01

    The budding yeast S. cerevisiae divides asymmetrically and is an excellent model system for asymmetric cell division. As for other asymmetrically dividing cells, proper spindle positioning along the mother-daughter polarity axis is crucial for balanced chromosome segregation. Thus, a surveillance mechanism named Spindle Position Checkpoint (SPOC) inhibits mitotic exit and cytokinesis until the mitotic spindle is properly oriented, thereby preventing the generation of cells with aberrant ploidies. The small GTPase Tem1 is required to trigger a Hippo-like protein kinase cascade, named Mitotic Exit Network (MEN), that is essential for mitotic exit and cytokinesis but also contributes to correct spindle alignment in metaphase. Importantly, Tem1 is the target of the SPOC, which relies on the activity of the GTPase-activating complex (GAP) Bub2-Bfa1 to keep Tem1 in the GDP-bound inactive form. Tem1 forms a hetero-trimeric complex with Bub2-Bfa1 at spindle poles (SPBs) that accumulates asymmetrically on the bud-directed spindle pole during mitosis when the spindle is properly positioned. In contrast, the complex remains symmetrically localized on both poles of misaligned spindles. We have recently shown that Tem1 residence at SPBs depends on its nucleotide state and, importantly, asymmetry of the Bub2-Bfa1-Tem1 complex does not promote mitotic exit but rather controls spindle positioning. PMID:26507466

  15. Quantitative In Situ TEM Studies of Small-Scale Plasticity in Irradiated and Unirradiated Metals

    NASA Astrophysics Data System (ADS)

    Chisholm, Claire

    In this work, unirradiated and irradiated model body centered cubic (BCC) and face centered cubic (FCC) materials are investigated using advanced electron microscopy techniques to quantitatively measure local stresses and strains around defects, with the overarching goal of obtaining a fundamental understanding of defect physics. Quantitative in-situ transmission electron microscopy (TEM) tensile tests are performed with Molybdenum-alloy nano-fibers, functioning as a model BCC structural material. Local true stress and strain around an active Frank-Read type dislocation source are obtained using quantitative load-displacement data and digital image correlation. A mixed Frank-Read dislocation source, b=a/2[-1-11](112) with a line direction 20° from a screw orientation and length 177 nm, is observed to begin operating at a measured local stress of 1.38 GPa. The measured local true stress values compare very well to estimated stresses using dislocation radius of curvature, and a line-tension model of a large bow-out configuration, with differences of only ˜1%. The degree to which the local true stresses can be measured is highly promising. However, the ultimate failure mode of these fibers, sudden strain softening after dislocation starvation and exhaustion, cannot be captured at the typical camera frame rate of 30 frames per second. Thus, fibers are mechanically tested while under observation with the Gatan K2-IS direct electron detector camera, where the frame rate is an order of magnitude larger at 400 fps. Though the increase in frame rate adds to the overall understanding of the sudden failure, by definitively showing that the nano-fibers break rather than strain soften, the failure mechanism still operates too quickly to be observed. In the final investigation of this BCC model structural alloy, the mechanical behavior of heavily dislocated, but unirradiated, and He1+ and Ni 2+ irradiated nano-fibers are compared. Remarkable similarities are found in the

  16. Sol-gel route of synthesis of nanoparticles of MgFe 2O 4 and XRD, FTIR and VSM study

    NASA Astrophysics Data System (ADS)

    Pradeep, A.; Priyadharsini, P.; Chandrasekaran, G.

    Nanoparticles of MgFe 2O 4 are synthesized using sol-gel autocombustion method. Structural studies are carried out using X-ray diffraction (XRD). The XRD pattern of MgFe 2O 4 provides information about single-phase formation of spinel structure with cubic symmetry. The grain size and lattice constant are obtained using XRD data. The cation distribution is also proposed theoretically. The change in site preference of cations in nano-MgFe 2O 4 is compared with its bulk counterpart. The structural morphology of the nanoparticles is studied using Scanning Electron Microscopy (SEM). Formation of spinel structure is conformed using Fourier transform infrared spectroscopy (FTIR), which also lends support for the cation distribution proposed using XRD data. The effect of nanoregime on parameters such as bond length, vibration frequency and force constant are discussed with the help of FTIR data. The M- H loop of MgFe 2O 4 has been traced using the Vibrating Sample Magnetometer (VSM) and magnetic parameters such as saturation magnetization ( MS), coercivity ( HC) and retentivity ( MR) are obtained from VSM data.

  17. Correlated NanoSIMS, TEM, and XANES Studies of Presolar Grains

    NASA Astrophysics Data System (ADS)

    Groopman, Evan Edward

    The objective of this thesis is to describe the correlated study of individual presolar grains via Nano-scale Secondary Ion Mass Spectrometry (NanoSIMS), Transmission Electron Microscopy (TEM), and Scanning Transmission X-ray Microscopy (STXM) utilizing X-ray Absorption Near Edge Structure (XANES), with a focus on connecting these correlated laboratory studies to astrophysical phenomena. The correlated isotopic, chemical, and microstructural studies of individual presolar grains provide the most detailed description of their formation environments, and help to inform astrophysical models and observations of stellar objects. As a part of this thesis I have developed and improved upon laboratory techniques for micromanipulating presolar grains and embedding them in resin for ultramicrotomy after NanoSIMS analyses and prior to TEM characterization. The new methods have yielded a 100% success rate and allow for the specific correlation of microstructural and isotopic properties of individual grains. Knowing these properties allows for inferences to be made regarding the condensation sequences and the origins of the stellar material that condensed to form these grains. NanoSIMS studies of ultramicrotomed sections of presolar graphite grains have revealed complex isotopic heterogeneities that appear to be primary products of the grains' formation environments and not secondary processing during the grains' lifetimes. Correlated excesses in 15N and 18O were identified as being carried by TiC subgrains within presolar graphite grains from supernovae (SNe). These spatially-correlated isotopic anomalies pinpoint the origin of the material that formed these grains: the inner He/C zone. Complex microstructures and isotopic heterogeneities also provide evidence for mixing in globular SN ejecta, which is corroborated by models and telescopic observations. In addition to these significant isotopic discoveries, I have also observed the first reported nanocrystalline core

  18. Multi-scale characterization by FIB-SEM/TEM/3DAP.

    PubMed

    Ohkubo, T; Sepehri-Amin, H; Sasaki, T T; Hono, K

    2014-11-01

    In order to improve properties of functional materials, it is important to understand the relation between the structure and the properties since the structure has large effect to the properties. This can be done by using multi-scale microstructure analysis from macro-scale to nano and atomic scale. Scanning electron microscope (SEM) equipped with focused ion beam (FIB), transmission electron microscope (TEM) and 3D atom probe (3DAP) are complementary analysis tools making it possible to know the structure and the chemistry from micron to atomic resolution. SEM gives us overall microstructural and chemical information by various kinds of detectors such as secondary electron, backscattered electron, EDS and EBSD detectors. Also, it is possible to analyze 3D structure and chemistry via FIB serial sectioning. In addition, using TEM we can focus on desired region to get more complementary information from HRTEM/STEM/Lorentz images, SAED/NBD patterns and EDS/EELS to see the detail micro or nano-structure and chemistry. Especially, combination of probe Cs corrector and split EDS detectors with large detector size enable us to analyze the atomic scale elemental distribution. Furthermore, if the specimen has a complicated 3D nanostructure, or we need to analyze light elements such as hydrogen, lithium or boron, 3DAP can be used as the only technique which can visualize and analyze distribution of all constituent atoms of our materials within a few hundreds nm area. Hence, site-specific sample preparation using FIB/SEM is necessary to get desired information from region of interest. Therefore, this complementary analysis combination works very well to understand the detail of materials.In this presentation, we will show the analysis results obtained from some of functional materials by Carl Zeiss CrossBeam 1540EsB FIB/SEM, FEI Tecnai G(2) F30, Titan G2 80-200 TEMs and locally build laser assisted 3DAP. As the one of the example, result of multi-scale characterization for

  19. XRD measurement of mean thickness, thickness distribution and strain for illite and illite-smectite crystallites by the Bertaut-Warren-Averbach technique

    USGS Publications Warehouse

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

    1998-01-01

    A modified version of the Bertaut-Warren-Averbach (BWA) technique (Bertaut 1949, 1950; Warren and Averbach 1950) has been developed to measure coherent scattering domain (CSD) sizes and strains in minerals by analysis of X-ray diffraction (XRD) data. This method is used to measure CSD thickness distributions for calculated and experimental XRD patterns of illites and illite-smectites (I-S). The method almost exactly recovers CSD thickness distributions for calculated illite XRD patterns. Natural I-S samples contain swelling layers that lead to nonperiodic structures in the c* direction and to XRD peaks that are broadened and made asymmetric by mixed layering. Therefore, these peaks cannot be analyzed by the BWA method. These difficulties are overcome by K-saturation and heating prior to X-ray analysis in order to form 10-A?? periodic structures. BWA analysis yields the thickness distribution of mixed-layer crystals (coherently diffracting stacks of fundamental illite particles). For most I-S samples, CSD thickness distributions can be approximated by lognormal functions. Mixed-layer crystal mean thickness and expandability then can be used to calculate fundamental illite particle mean thickness. Analyses of the dehydrated, K-saturated samples indicate that basal XRD reflections are broadened by symmetrical strain that may be related to local variations in smectite interlayers caused by dehydration, and that the standard deviation of the strain increases regularly with expandability. The 001 and 002 reflections are affected only slightly by this strain and therefore are suited for CSD thickness analysis. Mean mixed-layer crystal thicknesses for dehydrated I-S measured by the BWA method are very close to those measured by an integral peak width method.

  20. He Transport and Fate of Tempered Martensitic Steels: Summary of Recent TEM Observations

    SciTech Connect

    Edwards, Danny J.; Kurtz, Richard J.; Odette, G Robert; Yamamoto, Takuya

    2010-02-26

    As an extension of prior work [1-4], we summarize recent observations made on a He-implanted tempered martensitic steel (TMS), F82H mod 3, irradiated in the HFIR, in both as-tempered (AT) and cold-worked (CW) conditions. A novel implantation technique was used to uniformly inject He into 3-mm diameter TEM discs to depths ranging from ≈ 5-8 µm. The He is generated by two-step transmutation reactions in Ni contained in a NiAl coating layer adjacent to paired 3 mm TEM discs. NiAl layers from 1 to 4 μm thick produced He/dpa ratios between 5 and 40 appm/dpa. The irradiations were at temperatures of 300, 400 and 500°C from 3.9 to 9 dpa and 90 to 380 appm He. Electron transparent samples were prepared by a cross-sectional thinning technique that allowed investigating microstructural evolution over a range of implantation depths. Irradiation of the AT alloy to 9 dpa at 500°C and 380 appm He resulted in relatively large, faceted cavities, that are likely voids, along with a much higher density of smaller He bubbles. The cavities were most often aligned in pearl necklace like strings, presumably due to their formation on pre-existing dislocations. A finer distribution of cavities was also present on precipitate interfaces, lath and grain boundaries. Nine dpa irradiations that produced 190 appm He resulted in a somewhat more random distribution and lower density of smaller matrix cavities; but lower He levels had a less noticeable effect on bubbles in the lath and precipitate boundaries. Corresponding irradiations of the CW F82H produced a larger number of smaller cavities. Irradiation of the AT alloy to 3.9 dpa and 90 ppm He at 400°C produced a similar cavity population to that observed at 500°C at 190 appm He, while the corresponding cavities at 500°C are slightly larger and more numerous at 380 appm He. The cavity strings were less obvious for the 400°C irradiations, and the bubble distribution appeared to be more random. No cavities were observed in the case of

  1. Shell structure of natural rubber particles: evidence of chemical stratification by electrokinetics and cryo-TEM.

    PubMed

    Rochette, Christophe N; Crassous, Jérôme J; Drechsler, Markus; Gaboriaud, Fabien; Eloy, Marie; de Gaudemaris, Benoît; Duval, Jérôme F L

    2013-11-26

    The interfacial structure of natural rubber (NR) colloids is investigated by means of cryogenic transmission electron microscopy (cryo-TEM) and electrokinetics over a broad range of KNO3 electrolyte concentrations (4-300 mM) and pH values (1-8). The asymptotic plateau value reached by NR electrophoretic mobility (μ) in the thin double layer limit supports the presence of a soft (ion- and water-permeable) polyelectrolytic type of layer located at the periphery of the NR particles. This property is confirmed by the analysis of the electron density profile obtained from cryo-TEM that evidences a ∼2-4 nm thick corona surrounding the NR polyisoprene core. The dependence of μ on pH and salt concentration is further marked by a dramatic decrease of the point of zero electrophoretic mobility (PZM) from 3.6 to 0.8 with increasing electrolyte concentration in the range 4-300 mM. Using a recent theory for electrohydrodynamics of soft multilayered particles, this "anomalous" dependence of the PZM on electrolyte concentration is shown to be consistent with a radial organization of anionic and cationic groups across the peripheral NR structure. The NR electrokinetic response in the pH range 1-8 is indeed found to be equivalent to that of particles surrounded by a positively charged ∼3.5 nm thick layer (mean dissociation pK ∼ 4.2) supporting a thin and negatively charged outermost layer (0.6 nm in thickness, pK ∼ 0.7). Altogether, the strong dependence of the PZM on electrolyte concentration suggests that the electrostatic properties of the outer peripheral region of the NR shell are mediated by lipidic residues protruding from a shell containing a significant amount of protein-like charges. This proposed NR shell interfacial structure questions previously reported NR representations according to which the shell consists of either a fully mixed lipid-protein layer, or a layer of phospholipids residing exclusively beneath an outer proteic film. PMID:24152085

  2. Shell structure of natural rubber particles: evidence of chemical stratification by electrokinetics and cryo-TEM.

    PubMed

    Rochette, Christophe N; Crassous, Jérôme J; Drechsler, Markus; Gaboriaud, Fabien; Eloy, Marie; de Gaudemaris, Benoît; Duval, Jérôme F L

    2013-11-26

    The interfacial structure of natural rubber (NR) colloids is investigated by means of cryogenic transmission electron microscopy (cryo-TEM) and electrokinetics over a broad range of KNO3 electrolyte concentrations (4-300 mM) and pH values (1-8). The asymptotic plateau value reached by NR electrophoretic mobility (μ) in the thin double layer limit supports the presence of a soft (ion- and water-permeable) polyelectrolytic type of layer located at the periphery of the NR particles. This property is confirmed by the analysis of the electron density profile obtained from cryo-TEM that evidences a ∼2-4 nm thick corona surrounding the NR polyisoprene core. The dependence of μ on pH and salt concentration is further marked by a dramatic decrease of the point of zero electrophoretic mobility (PZM) from 3.6 to 0.8 with increasing electrolyte concentration in the range 4-300 mM. Using a recent theory for electrohydrodynamics of soft multilayered particles, this "anomalous" dependence of the PZM on electrolyte concentration is shown to be consistent with a radial organization of anionic and cationic groups across the peripheral NR structure. The NR electrokinetic response in the pH range 1-8 is indeed found to be equivalent to that of particles surrounded by a positively charged ∼3.5 nm thick layer (mean dissociation pK ∼ 4.2) supporting a thin and negatively charged outermost layer (0.6 nm in thickness, pK ∼ 0.7). Altogether, the strong dependence of the PZM on electrolyte concentration suggests that the electrostatic properties of the outer peripheral region of the NR shell are mediated by lipidic residues protruding from a shell containing a significant amount of protein-like charges. This proposed NR shell interfacial structure questions previously reported NR representations according to which the shell consists of either a fully mixed lipid-protein layer, or a layer of phospholipids residing exclusively beneath an outer proteic film.

  3. Cryo-TEM of morphology and kinetics of self-assembled nanostructures

    NASA Astrophysics Data System (ADS)

    Dong, Jingshan

    Cryogenic Transmission Electron Microscopy (Cryo-TEM) is applied to study various structures in solutions and suspensions from micron to nanometer scale. By vitrifying the liquid samples at different moments, sequential stages of a dynamic process can be frozen and the structures occurring from about 30 sec to over 10 min can be imaged. Therefore a picture of how the structures evolve with time in the liquid systems can be established. This method has been proven to be a powerful technique in studying the morphology and kinetics of self-assembled nanostructures. Such a pseudo-in-situ technique is used to "watch" the crystallization process of silver stearate (AgSt) from sodium stearate (NaSt) dispersions. AgSt crystal is produced from a reaction of NaSt and silver nitrate. The reaction, as a AgSt crystallization process, starts from AgSt micelles, which aggregate and grow into hexagonal shaped crystals of about 10 microns. If silver bromide (AgBr) grains are present, the micelles do not prefer to aggregate, but rather deposit on the surface of the AgBr crystalline grains. Variation of the carboxylate chain length does not affect the crystallization process very much, although the morphology of both the reactant and the product is changed. Nanostructure transition in sodium lauryl ether sulfate (SLES) solutions is investigated as well. A micellar network structure can form if equal molar calcium chloride is added to 3 wt% SLES solution. The network can be broken into wormlike micelle segments such as spheres and rods by sonication. After about 10 min, these broken pieces can reassemble and reform the network through wormlike micelle growth and connection. Also by using Cryo-TEM, 100-200 nm casein micelles are observed at 1 wt% casein solution, but aggregated submicelles cannot be distinguished. However, individual submicelles of about 30 nm are indeed captured in a 0.03 wt% solution. By adding acid or EDTA, the casein micelles can be disrupted into small particles

  4. Experimental Space Weathering: A coordinated LIBS, TEM, VIS and NIR/MIR study

    NASA Astrophysics Data System (ADS)

    Stojic, Aleksandra N.; Pavlov, Sergey; Markus, Kathrin; Morlok, Andreas; Wirth, Richard; Weber, Iris; Schreiber, Anja; Hiesinger, Harald; Sohn, Martin; Huebers, Heinz-Wilhelm

    2016-04-01

    We conducted pulsed infrared laser irradiation experiments, in order to simulate space weathering triggered modifications of planetary surfaces not protected by an enveloping atmosphere [1,2], e.g., Mercury. Our work is embedded in the framework of the BepiColombo space mission to Mercury [3]. The MErcury Radiometer and Thermal Infrared Spectrometer (MERTIS), an onboard spectrometer will deliver surface data in the range of 7 - 14 μm once it reaches orbit in 2024 [4]. Space weathering effects known from other Solar System bodies are likely to be very prominent on Mercury due to its proximity to the Sun, the lack of a protective atmosphere and its weak magnetic field [5]. Space weathering effects, e.g., implantation of solar wind in regolith material, sputtering and (micro) meteorite impacts modify the planetary surface and thus, therefrom obtained spectral data in the VIS/NIR range considerably (e.g., reddening and darkening of spectra) [6-9]. We expect modifications induced by space weathering, known from the VIS/NIR range also to show in the mid infrared range, probably by amorphisation or similar still unknown effects [2,10]. Our approach is therefore threefold: a) alter analog material artificially by pulsed laser experiments, b) investigate altered analog material spectrally (VIS/NIR and MIR range) and c) conduct transmission electron microscopy (TEM) studies on selected weathered grains to better understand the nanostratigraphy developed by irradiation and its impact on the resulting infrared spectra. Here, we report on results obtained from the first set of experiments. Characteristic upper mantle minerals were taken as analog material, Mg-rich olivine and pyroxene, were ground into a powder (< 160 μm), slightly compressed into pellets and subsequently irradiated under high vacuum conditions (˜ 10-6 mbar) with a pulsed (˜ 8ns) infrared laser at a fluence of ˜ 2 Jcm-2. From the irradiated pellet surfaces, VIS/NIR and MIR spectra were obtained and

  5. Experimental Space Weathering: A coordinated LIBS, TEM, VIS and NIR/MIR study

    NASA Astrophysics Data System (ADS)

    Stojic, Aleksandra N.; Pavlov, Sergey; Markus, Kathrin; Morlok, Andreas; Wirth, Richard; Weber, Iris; Schreiber, Anja; Hiesinger, Harald; Sohn, Martin; Huebers, Heinz-Wilhelm

    2016-04-01

    We conducted pulsed infrared laser irradiation experiments, in order to simulate space weathering triggered modifications of planetary surfaces not protected by an enveloping atmosphere [1,2], e.g., Mercury. Our work is embedded in the framework of the BepiColombo space mission to Mercury [3]. The MErcury Radiometer and Thermal Infrared Spectrometer (MERTIS), an onboard spectrometer will deliver surface data in the range of 7 - 14 μm once it reaches orbit in 2024 [4]. Space weathering effects known from other Solar System bodies are likely to be very prominent on Mercury due to its proximity to the Sun, the lack of a protective atmosphere and its weak magnetic field [5]. Space weathering effects, e.g., implantation of solar wind in regolith material, sputtering and (micro) meteorite impacts modify the planetary surface and thus, therefrom obtained spectral data in the VIS/NIR range considerably (e.g., reddening and darkening of spectra) [6‑9]. We expect modifications induced by space weathering, known from the VIS/NIR range also to show in the mid infrared range, probably by amorphisation or similar still unknown effects [2,10]. Our approach is therefore threefold: a) alter analog material artificially by pulsed laser experiments, b) investigate altered analog material spectrally (VIS/NIR and MIR range) and c) conduct transmission electron microscopy (TEM) studies on selected weathered grains to better understand the nanostratigraphy developed by irradiation and its impact on the resulting infrared spectra. Here, we report on results obtained from the first set of experiments. Characteristic upper mantle minerals were taken as analog material, Mg-rich olivine and pyroxene, were ground into a powder (< 160 μm), slightly compressed into pellets and subsequently irradiated under high vacuum conditions (˜ 10‑6 mbar) with a pulsed (˜ 8ns) infrared laser at a fluence of ˜ 2 Jcm‑2. From the irradiated pellet surfaces, VIS/NIR and MIR spectra were obtained and

  6. TEM Cell Testing of Cable Noise Reduction Techniques From 2 MHz to 200 MHz - Part 1

    NASA Technical Reports Server (NTRS)

    Bradley, Arthur T.; Evans, William C.; Reed, Joshua L.; Shimp, Samuel K.; Fitzpatrick, Fred D.

    2008-01-01

    This paper presents empirical results of cable noise reduction techniques as demonstrated in a TEM cell operating with radiated fields from 2 - 200 MHz. It is the first part of a two-paper series. This first paper discusses cable types and shield connections. In the second paper, the effects of load and source resistances and chassis connections are examined. For each topic, well established theories are compared to data from a real-world physical system. Finally, recommendations for minimizing cable susceptibility (and thus cable emissions) are presented. There are numerous papers and textbooks that present theoretical analyses of cable noise reduction techniques. However, empirical data is often targeted to low frequencies (e.g. <50 KHz) or high frequencies (>100 MHz). Additionally, a comprehensive study showing the relative effects of various noise reduction techniques is needed. These include the use of dedicated return wires, twisted wiring, cable shielding, shield connections, changing load or source impedances, and implementing load- or source-to-chassis isolation. We have created an experimental setup that emulates a real-world electrical system, while still allowing us to independently vary a host of parameters. The goal of the experiment was to determine the relative effectiveness of various noise reduction techniques when the cable is in the presence of radiated emissions from 2 MHz to 200 MHz. The electronic system (Fig. 1) consisted of two Hammond shielded electrical enclosures, one containing the source resistance, and the other containing the load resistance. The boxes were mounted on a large aluminium plate acting as the chassis. Cables connecting the two boxes measured 81 cm in length and were attached to the boxes using standard D38999 military-style connectors. The test setup is shown in Fig. 2. Electromagnetic fields were created using an HP8657B signal generator, MiniCircuits ZHL-42W-SMA amplifier, and an EMCO 5103 TEM cell. Measurements were

  7. Synthesis, TEM characterization and thermal behaviour of LiNiSi2O6 pyroxene

    NASA Astrophysics Data System (ADS)

    Tribaudino, Mario; Bromiley, Geoffrey; Ohashi, Haruo; Nestola, Fabrizio

    2009-10-01

    A pyroxene with composition LiNiSi2O6 was synthesized at T = 1,473 K and P = 2.0 GPa; the cell parameters at T = 298 K are a = 9.4169(6) Å, b = 8.4465(7) Å, c = 5.2464(3) Å, β = 110.534(6)°, V = 390.78(3) Å3. TEM examination of the LiNiSi2O6 pyroxene showed the presence of h + k odd reflections indicative of a primitive lattice, and of antiphase domains obtained by dark field imaging of the h + k odd reflections. A HT in situ investigation was performed by examining TEM selected area diffraction patterns collected at high temperature and synchrotron radiation powder diffraction. In HTTEM the LiNiSi2O6 was examined together with LiCrSi2O6 pyroxene. In LiCrSi2O6 the h + k odd critical reflections disappear at about 340 K; they are sharp up to the transition temperature and do not change their shape until they disappear. In LiNiSi2O6 the h + k odd reflections are present up to sample deterioration at 650 K. A high temperature synchrotron radiation powder diffraction investigation was performed on LiNiSi2O6 between 298 and 773 K. The analysis of critical reflections and of changes in cell parameters shows that the space group is P-centred up to the highest temperature. The comparative analysis of the thermal and spontaneous strain contributions in P21/ c and C2/ c pyroxenes indicates that the high temperature strain in P-LiNiSi2O6 is very similar to that due to thermal strain only in C2/ c spodumene and that a spontaneous strain contribution related to pre-transition features is not apparent in LiNiSi2O6. A different high-temperature behaviour in LiNiSi2O6 with respect to other pyroxenes is suggested, possibly in relation with the presence of Jahn-Teller distortion of the M1 polyhedron centred by low-spin Ni3+.

  8. Detecting single-electron events in TEM using low-cost electronics and a silicon strip sensor.

    PubMed

    Gontard, Lionel C; Moldovan, Grigore; Carmona-Galán, Ricardo; Lin, Chao; Kirkland, Angus I

    2014-04-01

    There is great interest in developing novel position-sensitive direct detectors for transmission electron microscopy (TEM) that do not rely in the conversion of electrons into photons. Direct imaging improves contrast and efficiency and allows the operation of the microscope at lower energies and at lower doses without loss in resolution, which is especially important for studying soft materials and biological samples. We investigate the feasibility of employing a silicon strip detector as an imaging detector for TEM. This device, routinely used in high-energy particle physics, can detect small variations in electric current associated with the impact of a single charged particle. The main advantages of using this type of sensor for direct imaging in TEM are its intrinsic radiation hardness and large detection area. Here, we detail design, simulation, fabrication and tests in a TEM of the front-end electronics developed using low-cost discrete components and discuss the limitations and applications of this technology for TEM. PMID:24401331

  9. Prevalence of β-lactam (blaTEM) and Metronidazole (nim) Resistance Genes in the Oral Cavity of Greek Subjects

    PubMed Central

    Koukos, Georgios; Konstantinidis, Antonios; Tsalikis, Lazaros; Arsenakis, Minas; Slini, Theodora; Sakellari, Dimitra

    2016-01-01

    Objectives: The aim of this study is to investigate the prevalence of blaTEM and nim genes that encode resistance to β-lactams and nitroimidazoles, respectively, in the oral cavity of systemically healthy Greek subjects. Materials and Methodology: After screening 720 potentially eligible subjects, 154 subjects were recruited for the study, including 50 periodontally healthy patients, 52 cases of gingivitis and 52 cases of chronic periodontitis. The clinical parameters were assessed with an automated probe. Various samples were collected from the tongue, first molars and pockets >6mm, and analysed by polymerase chain reaction-amplification of the blaTEM and nim genes, using primers and conditions previously described in the literature. Results: There was a high rate of detection of blaTEM in plaque and tongue samples alike in all periodontal conditions (37% of plaque and 60% of tongue samples, and 71% of participants). The blaTEM gene was detected more frequently in the tongue samples of the periodontally healthy (56%) and chronic periodontitis (62%) groups compared to the plaque samples from the same groups (36% and 29%, respectively; z-test with Bonferroni corrections-tests, P<0.05). The nim gene was not detected in any of the 343 samples analysed. Conclusion: The oral cavity of Greek subjects often harbours blaTEM but not nim genes, and therefore the antimicrobial activity of β-lactams might be compromised. PMID:27099637

  10. Resistance to β-Lactamase Inhibitor Protein Does Not Parallel Resistance to Clavulanic Acid in TEM β-Lactamase Mutants

    PubMed Central

    Schroeder, William A.; Locke, Troy R.; Jensen, Susan E.

    2002-01-01

    In order to compare patterns of resistance to inhibition by clavulanic acid with patterns of resistance to inhibition by a β-lactamase inhibitor protein (BLIP), R164S, R244S, and R164S/R244S mutant forms of TEM β-lactamase were prepared by site-directed mutagenesis. When kinetic parameters were determined for these mutant and wild-type forms of TEM, the single mutants showed properties that were similar to those in the literature but the double mutant showed properties that were very different. The R164S/R244S double mutant form of TEM retained its resistance to inhibition by clavulanic acid (characteristic of the R244S mutation) but lost all its ability to hydrolyze ceftazidime (characteristic of the R164S mutation). While these characteristics are contrary to those previously reported for an R164S/R244S double mutant, this discrepancy resulted from the use of a defective mutant in the earlier study. Both the single and double mutant forms of TEM remained highly sensitive when tested for inhibition by BLIP, showing only slightly increased resistance compared to that of the wild type; this pattern of resistance is quite different from the pattern of clavulanic acid resistance. The slight increases in resistance to inhibition by BLIP seen in the mutants may have been related to the fact that all of the mutations effected changes in the net charge on the TEM protein that could impede interactions with BLIP. PMID:12384366

  11. In situ TEM visualization of superior nanomechanical flexibility of shear-exfoliated phosphorene.

    PubMed

    Xu, Feng; Ma, Hongyu; Lei, Shuangying; Sun, Jun; Chen, Jing; Ge, Binghui; Zhu, Yimei; Sun, Litao

    2016-07-14

    Recently discovered atomically thin black phosphorus (called phosphorene) holds great promise for applications in flexible nanoelectronic devices. Experimentally identifying and characterizing nanomechanical properties of phosphorene are challenging, but also potentially rewarding. This work combines for the first time in situ transmission electron microscopy (TEM) imaging and an in situ micro-manipulation system to directly visualize the nanomechanical behaviour of individual phosphorene nanoflakes. We demonstrate that the phosphorene nanoflakes can be easily bent, scrolled, and stretched, showing remarkable mechanical flexibility rather than fracturing. An out-of-plane plate-like bending mechanism and in-plane tensile strain of up to 34% were observed. Moreover, a facile liquid-phase shear exfoliation route has been developed to produce such mono-layer and few-layer phosphorene nanoflakes in organic solvents using only a household kitchen blender. The effects of surface tensions of the applied solvents on the ratio of average length and thickness (L/T) of the nanoflakes were studied systematically. The results reported here will pave the way for potential industrial-scale applications of flexible phosphorene nanoelectronic devices. PMID:27362430

  12. Analytical TEM examinations of CoPt-TiO2 perpendicular magnetic recording media.

    PubMed

    Risner, Juliet D; Nolan, Thomas P; Bentley, James; Girt, Erol; Harkness, Samuel D; Sinclair, Robert

    2007-04-01

    For this analytical TEM study, nonmagnetic oxygen-rich boundaries were introduced into Co-Pt-alloy perpendicular recording media by cosputtering Co and Pt with TiO2. Increasing the TiO2 content resulted in changes to the microstructure and elemental distribution within grains and boundaries in these films. EFTEM imaging was used to generate composition maps spanning many tens of grains, thereby giving an overall depiction of the changes in elemental distribution occurring with increasing TiO2 content. Comparing EFTEM with spectrum-imaging maps created by high-resolution STEM with EDXS and EELS enabled both corroboration of EFTEM results and quantification of the chemical composition within individual grain boundary areas. The difficulty of interpreting data from EDXS for these extremely thin films is discussed. Increasing the TiO2 content of the media was found to create more uniformly wide Ti- and O-rich grain boundaries as well as Ti- and O-rich regions within grains.

  13. TEM-simulation of amorphous carbon films: influence of supercell packaging.

    PubMed

    Schultrich, H; Schultrich, B

    2001-07-01

    Recent developments in thin film technology allow to prepare deliberately amorphous carbon films with structures widely varying between graphite-like (sp2) and diamond-like (sp3) atomic bonds. This leads to amorphous structures with correspondingly varying densities. By periodically changing deposition conditions, nanometer multilayers may be prepared consisting of carbon layers of different density. Simulation of the electron microscopic imaging allows to differentiate between such real structural details (on the nanometer scale) and artefacts induced by the imaging procedure. But it must be assured that the modeled structure reflects the real one with sufficient accuracy. Thorough comparison of different simulation strategies shows that for the adequate simulation of TEM imaging of amorphous materials, the thickness of the layer with independently distributed atoms has to exceed a certain limit. Then, the statistical scattering of the randomly distributed atoms will be averaged. Otherwise, if the model of the transmission electron microscopy sample is constructed as iteration of thin identical supercells, the superposition of scattering waves with constant phase differences results in enhanced local fluctuations burying the multilayer structure. For thicker packages of supercells with independent random distributions, the effect of statistical atomic arrangements is more and more leveled off. Hence, nanometer structures based on regions with different density will be visible more distinctively in the random background. For carbon, this critical thickness amounts to about 4 nm. This is of special importance for the visualization of nanoscaled heterogeneities like multilayers or nanotube-like inclusions in amorphous matrices. PMID:11419873

  14. Advanced TEM specimen preparation methods for replication of P91 steel

    SciTech Connect

    Mitchell, D.R.G. . E-mail: drm@ansto.gov.au; Sulaiman, S.

    2006-01-15

    A range of advanced transmission electron microscopy specimen preparation methods, based on replication, have been developed for P91 steel. The results obtained have been compared with conventional replication and thin foil methods. The aim has been to obtain complimentary information from thin foil and replica specimens from the same region of interest either sequentially or simultaneously. The effects of various reagents for dissolution of the steel matrix and replica release have been investigated, and chemical methods for removing amorphous iron oxide contaminants from replicas have been identified. A method of region-specific replication is demonstrated whereby regions of thin foils previously characterised by TEM, can be subsequently replicated. This enables the former location of extracted particles, such as on grain/lath/subgrain boundaries etc., to be determined prior to microanalysis. It also permits the identification of artefacts such as stray particles and failed extractions. A second method of thin foil partial replication was developed in which both replica and thin foil are present on the same specimen. At the interface between the two regions, thin foil information such as dislocation interactions with fine scale particles and replica information such as microanalysis of particles within the same grain or lath can be obtained. Double replication of thin foils has also been successfully demonstrated. These methods are applied to a creep resistant martensitic steel (P91), but should be broadly applicable to a wide range of alloy steels.

  15. Metal biosorption capacity of the organic solvent tolerant Pseudomonas fluorescens TEM08.

    PubMed

    Uzel, Atac; Ozdemir, Guven

    2009-01-01

    Many kinds of biomass are being tested as a biosorption material for metal removal from the contaminated waters. In the present study the biosorption capacity of an organic solvent tolerant (OST) bacterium was investigated against Cr(VI) and Ni(II). The OST strain of Pseudomonas fluorescens TEM08 was isolated from an oil contaminated soil sample and grown in normal culture conditions (type I) and in the presence of the cyclohexane (type II). Two types of cells were used in the biosorption experiments to compare the organic solvent effect on the biosorption capacity. The biosorption equilibrium was described by Langmuir and Freundlich adsorption isotherms. The value of Q(0) was higher for type I cells (40.8 for Cr(VI); 12.4 for Ni(II)) then the type II (40.7 for Cr(VI); 11.2 for Ni(II)). The adsorption capacity constants (K(F)) of Freundlich model for type I cells and for type II cells were 10.87 and 8.78 for Ni(II) and 13.60 and 10.99 for Cr(VI), respectively. PMID:18657416

  16. TEM observations on Type III kerogen, with special reference to coal as a source rock

    NASA Astrophysics Data System (ADS)

    Liu, Susie Y.; Taylor, Geoff H.

    Type III kerogen follows the coalification track of vitrinite or a bulk coal. It is often inferred that, because this organic matter is of comparatively low hydrogen and high oxygen content, it cannot be more than a marginal source of petroleum. This is not a correct approach because the actual source material is not the whole coal but only a small fraction. Some, at least, of this small fraction appears likely to be just as rich a source as much of Type I or Type II kerogen. There is no doubt that the liptinite macerals are important source materials. However, with TEM it can be shown that there are additional, and in some cases more significant, sources with varying degrees of thermal reactivity. These include: -in vitrinite, the remains of fungi and bacteria, other fine lipid-rich matter, and suberin; -in vitrinitic and especially in inertinitic coal, algal and algae-like material. Micrinite consists of aggregates of very fine spherical bodies which are formed when hydrocarbons are generated. The presence of such aggregates within the coal texture confirms the generative role of the lipid-rich components and provides an important indication as to whether generation has occurred.

  17. In situ TEM Studies of the Initial Oxidation stage of Cu and Cu Alloy Thin Films

    NASA Astrophysics Data System (ADS)

    Yang, Judith; Kang, Yihong; Luo, Langli; Ciston, James; Stach, Eric; Zhou, Guangwen

    2012-02-01

    The fundamental understanding of oxidation at the nanoscale is important for the environmental stability of coating materials as well as processing of oxide nanostructures. Our previous studies show the epitaxial growth of Cu2O islands during the initial stages of oxidation of Cu thin films, where surface diffusion and strain impact the oxide development and morphologies. The addition of secondary elements changes the oxidation mechanism. If the secondary element is non-oxidizing, such as Au, it will limit the Cu2O island growth due to the depletion of Cu near the oxide islands. When the secondary element is oxidizing, for example Ni, the alloy will show more complex behaviour, where duplex oxide islands were observed. Nucleation density and growth rate of oxide islands are observed under various temperatures and oxygen partial pressures (pO2) as a function of time by in situ ultra high vacuum (UHV)-transmission electron microscopy (TEM). Our initial results of Cu-Ni(001) oxidation is that the oxide epitaxy and morphologies change as function of Ni concentration. For higher spatial resolution, we are examining the atomic scale oxidation by aberration-corrected ETEM with 1å resolution.

  18. TEM Observation of the Ti Interlayer Between SiC Substrates During Diffusion Bonding

    NASA Technical Reports Server (NTRS)

    Tsuda, Hiroshi; Mori, Shigeo; Halbig, Michael C.; Singh, Mori

    2012-01-01

    Diffusion bonding was carried out to join SiC to SiC substrates using titanium interlayers. In this study, 10 m and 20 m thick physical vapor deposited (PVD) Ti surface coatings, and 10 and 20 m thick Ti foils were used. Diffusion bonding was performed at 1250 C for PVD Ti coatings and 1200 C for Ti foil. This study investigates the microstructures of the phases formed during diffusion bonding through TEM and selected-area diffraction analysis of a sample prepared with an FIB, which allows samples to be taken from the reacted area. In all samples, Ti3SiC2, Ti5Si3Cx and TiSi2 phases were identified. In addition, TiC and unknown phases also appeared in the samples in which Ti foils were used as interlayers. Furthermore, Ti3SiC2 phases show high concentration and Ti5Si3Cx formed less when samples were processed at a higher temperature and thinner interlayer samples were used. It appears that the formation of microcracks is caused by the presence of intermediate phase Ti5Si3Cx, which has anisotropic thermal expansion, and by the presence of an unidentified Ti-Si-C ternary phase with relatively low Si content.

  19. TEM investigation on the microstructural evolution of Hastelloy N induced by Ar⁺ ion irradiation.

    PubMed

    Liu, Min; Lu, Yanling; Liu, Renduo; Zhou, Xingtai

    2014-02-01

    Hastelloy N alloy has been selected as the primary structure material for molten salt reactor. In this article, Hastelloy N alloy samples were irradiated to different doses at room temperature using 300 keV Ar(+) ions. The microstructural evolution was investigated by transmission electron microscopy (TEM) and energy-dispersive spectroscopy (EDS). Black dot defects emerged in sample irradiated at low dose (0.4 displacement per atom (dpa)), and they grew up with irradiation doses (0.4-2 dpa). A high density of small dislocation loops (nano meters in size) were observed in the sample irradiated to 4 dpa. When the ion dose increased to 12 dpa, complicated structures with defects (including dislocation lines, larger loops and smaller black dots) were observed. Dislocation networks were detected from high-angle annular dark field (HAADF) images. Larger dislocation loops (size: 30-80 nm) were visible in the sample irradiated to 40 dpa. Irradiation with dose of 120 dpa led to the formation of face-centered cubic nanocrystallites with preferred orientations.

  20. TEM examination of microstructural evolution during processing of 14CrYWTi nanostructured ferritic alloys

    NASA Astrophysics Data System (ADS)

    Kishimoto, H.; Alinger, M. J.; Odette, G. R.; Yamamoto, T.

    2004-08-01

    A transmission electron microscopy (TEM) study was carried out on the co-evolution of the coarser-scale microstructural features in mechanically alloyed (MA) powders and hot isostatic press (HIP) consolidated Fe-14Cr-3W-0 and 0.4Ti-0.25Y 2O 3 nanostructured ferritic alloys (NFAs). The pancake shaped nanoscale grains in the as-MA powders are textured and elongated parallel to the particle surface. Powder annealing results in re-crystallization at 850 °C and grain growth at 1150 °C. The grains also recrystallize and may grow in the alloys HIPed at 850 °C, but appear to retain a polygonized sub-grain structure. The grains are larger and more distinct in the alloys HIPed at 1000 and 1150 °C. However, annealing resulted in bi-modal grain size distribution. Finer grains retained a significant dislocation density and populations of small precipitates with crystal structures distinct form the matrix. The grains and precipitates were much larger in alloys without Ti.

  1. TEM Cell Testing of Cable Noise Reduction Techniques from 2 MHz to 200 MHz -- Part 2

    NASA Technical Reports Server (NTRS)

    Bradley, Arthur T.; Evans, William C.; Reed, Joshua L.; Shimp, Samuel K., III; Fitzpatrick, Fred D.

    2008-01-01

    This paper presents empirical results of cable noise reduction techniques as demonstrated in a TEM cell operating with radiated fields from 2 - 200 MHz. It is the second part of a two-paper series. The first paper discussed cable types and shield connections. In this second paper, the effects of load and source resistances and chassis connections are examined. For each topic, well established theories are compared to data from a real-world physical system. Finally, recommendations for minimizing cable susceptibility (and thus cable emissions) are presented. There are numerous papers and textbooks that present theoretical analyses of cable noise reduction techniques. However, empirical data is often targeted to low frequencies (e.g. <50 KHz) or high frequencies (>100 MHz). Additionally, a comprehensive study showing the relative effects of various noise reduction techniques is needed. These include the use of dedicated return wires, twisted wiring, cable shielding, shield connections, changing load or source impedances, and implementing load- or source-to-chassis isolation. We have created an experimental setup that emulates a real-world electrical system, while still allowing us to independently vary a host of parameters. The goal of the experiment was to determine the relative effectiveness of various noise reduction techniques when the cable is in the presence of radiated emissions from 2 MHz to 200 MHz.

  2. Observation of thermally etched grain boundaries with the FIB/TEM technique

    SciTech Connect

    Palizdar, Y.; San Martin, D.; Ward, M.; Cochrane, R.C.; Brydson, R.; Scott, A.J.

    2013-10-15

    Thermal etching is a method which is able to reveal and characterize grain boundaries, twins or dislocation structures and determine parameters such as grain boundary energies, surface diffusivities or study phase transformations in steels, intermetallics or ceramic materials. This method relies on the preferential transfer of matter away from grain boundaries on a polished sample during heating at high temperatures in an inert/vacuum atmosphere. The evaporation/diffusion of atoms at high temperatures results in the formation of grooves at the intersections of the planes of grain/twin boundaries with the polished surface. This work describes how the combined use of Focussed Ion Beam and Transmission Electron Microscopy can be used to characterize not only the grooves and their profile with the surface, but also the grain boundary line below the groove, this method being complementary to the commonly used scanning probe techniques. - Highlights: • Thermally etched low-carbon steel samples have been characterized by FIB/TEM • Grain boundary (GB) lines below the groove have been characterized in this way • Absence of ghost traces and large θ angle suggests that GB are not stationary but mobile • Observations correlate well with previous works and Mullins' investigations [22].

  3. Using coherent illumination to extend HRTEM resolution: Why we need a FEG-TEM for HREM

    SciTech Connect

    O`Keefe, M.A.

    1992-11-01

    Resolution of a high-resolution transmission electron microscope (HRTEM) has traditionally been defined in terms of its Scherzer resolution limit at optimum defocus. However, even beyond the Scherzer limit, spatial frequencies can be transferred from the specimen to the image, out to the so-called information limit of the electron microscope. The information limit of the HRTEM is determined by the degree of energy spread in the electron beam used to illuminate the sample. Since a HRTEM equipped with a field-emission gun (FEG) will produce an electron beam of high coherence with little energy spread, it can achieve an improved information-limit, and can thus be used to produce through-focus series of images containing information well beyond its nominal (Scherzer) resolution limit. Suitable computer processing of such series of images can produce composite images at resolutions approaching the microscope information limit. For such a FEG-TEM, combined with suitable computer image processing, resolution can approach 1{Angstrom}. 12 refs., 9 figs.

  4. Using coherent illumination to extend HRTEM resolution: Why we need a FEG-TEM for HREM

    SciTech Connect

    O'Keefe, M.A.

    1992-11-01

    Resolution of a high-resolution transmission electron microscope (HRTEM) has traditionally been defined in terms of its Scherzer resolution limit at optimum defocus. However, even beyond the Scherzer limit, spatial frequencies can be transferred from the specimen to the image, out to the so-called information limit of the electron microscope. The information limit of the HRTEM is determined by the degree of energy spread in the electron beam used to illuminate the sample. Since a HRTEM equipped with a field-emission gun (FEG) will produce an electron beam of high coherence with little energy spread, it can achieve an improved information-limit, and can thus be used to produce through-focus series of images containing information well beyond its nominal (Scherzer) resolution limit. Suitable computer processing of such series of images can produce composite images at resolutions approaching the microscope information limit. For such a FEG-TEM, combined with suitable computer image processing, resolution can approach 1[Angstrom]. 12 refs., 9 figs.

  5. TEM observation of bacteria-induced plagioclase dissolution and secondary mineral formation

    NASA Astrophysics Data System (ADS)

    Tamura, T.; Kyono, A.; Nishimiya, Y.

    2015-12-01

    Silicate minerals are the most common minerals in the earth's crust. Bacteria are also distributed throughout the earth's surface environment. The silicate minerals are known to be dissolved by organic acids and polysaccharides known as bacteria metabolites. The metabolic activity of bacteria therefore plays an important role in the interaction between dissolution of the silicate minerals and formation of secondary minerals. However, little is known about the secondary mineral formation process associated with the bacterial metabolism. To clarify the bacterial effect on the mineral dissolution and the secondary mineral formation, we closely investigated the effect of bacterial activity on surface texture modification and chemical composition changes of plagioclase which is the most abundant silicate mineral in the earth's crust. The bacteria were isolated from soil and then added in a suitable medium with several plagioclase fragments (Ab100% and An100%). It was incubated for 10 days. Al and Si concentrations in the medium were measured by ICP-AES to monitor the dissolution of the plagioclase. Secondary mineral formation during the incubation was observed by TEM, EDS and SAED methods. The authors will give the experiment results and discuss the effect of bacterial activity on the plagioclase dissolution and the secondary mineral formation in detail.

  6. In-situ TEM observation of dislocation evolution in Kr-irradiated UO2 single crystal

    SciTech Connect

    Lingfeng He; Mahima Gupta; Clarissa A. Yablinsky; Jian Gan; Marquis A. Kirk; Xian-Ming Bai; Janne Pakarinen; Todd R. Allen

    2013-11-01

    In-situ transmission electron microscopy (TEM) observation of UO2 single crystal irradiated with Kr ions at high temperatures was conducted to understand the dislocation evolution due to high-energy radiation. The dislocation evolution in UO2 single crystal is shown to occur as nucleation and growth of dislocation loops at low-irradiation doses, followed by transformation to extended dislocation segments and networks at high doses, as well as shrinkage and annihilation of some loops and dislocations due to high temperature annealing. Generally the trends of dislocation evolution in UO2 are similar under Kr irradiation at different ion energies and temperatures (150 keV at 600 degrees C and 1 MeV at 800 degrees C) used in this work, although the specific dislocation loop size and density are quite different. Interstitial-type dislocation loops with Burgers vector along <110> were observed in the Kr-irradiated UO2.The irradiated specimens were denuded of dislocation loops near the surface.

  7. An in situ heating TEM analysis method for an interface reaction.

    PubMed

    Tanigaki, Toshiaki; Ito, Katsuji; Nagakubo, Yasuhira; Asakawa, Takayuki; Kanemura, Takashi

    2009-10-01

    In order to analyze the thermal property of nano-sized materials, an in situ observation technique that allows highly sensitive energy dispersive x-ray spectroscopic (EDX) analyses and high-resolution in situ heating observation of precision specimens is required. A method for the in situ observation of the interface reaction using an analytical transmission electron microscopy (TEM) and a specimen-heating holder was developed. The specimen holder used in this study was a direct-heating type having a fine tungsten wire heater. For sensitive analyses including an EDX map of composition changes during the interface reaction, a space toward the EDX detector with a take-off angle of 20 degrees was made in the specimen holder. Samples were prepared by attaching a micro-sample directly to the heater using the focused ion beam (FIB) micro-sampling technique. It was confirmed that the sensitive EDX map and electron diffraction analyses were possible during the reaction, and that the resolution of this technique was of the order of 0.223 nm at 550 degrees C. PMID:19376815

  8. Morphological and Compositional (S)TEM Analysis of Multiple Exciton Generation Solar Cells

    NASA Astrophysics Data System (ADS)

    Wisnivesky-Rocca-Rivarola, F.; Davis, N. J. L. K.; Bohm, M.; Ducati, C.

    2015-10-01

    Quantum confinement of charge carriers in semiconductor nanocrystals produces optical and electronic properties that have the potential to enhance the power conversion efficiency of solar cells. One of these properties is the efficient formation of more than one electron-hole pair from a single absorbed photon, in a process called multiple exciton generation (MEG). In this work we studied the morphology of nanocrystal multilayers of PbSe treated with CdCl2 using complementary imaging and spectroscopy techniques to characterise the chemical composition and morphology of full MEG devices made with PbSe nanorods (NRs). IN the scanning TEM (STEM), plan view images and chemical maps were obtained of the nanocrystal layers, which allowed for the analysis of crystal structure and orientation, as well as size distribution and aspect ratio. These results were complemented by cross-sectional images of full devices, which allowed accessing the structure of each layer that composes the device, including the nanorod packing in the active nanocrystal layer.

  9. Role of pleiotropy during adaptation of TEM-1 β-lactamase to two novel antibiotics

    PubMed Central

    Schenk, Martijn F; Witte, Sariette; Salverda, Merijn L M; Koopmanschap, Bertha; Krug, Joachim; de Visser, J Arjan G M

    2015-01-01

    Pleiotropy is a key feature of the genotype–phenotype map, and its form and extent have many evolutionary implications, including for the dynamics of adaptation and the evolution of specialization. Similarly, pleiotropic effects of antibiotic resistance mutations may affect the evolution of antibiotic resistance in the simultaneous or fluctuating presence of different antibiotics. Here, we study the role of pleiotropy during the in vitro adaptation of the enzyme TEM-1 β-lactamase to two novel antibiotics, cefotaxime (CTX) and ceftazidime (CAZ). We subject replicate lines for four rounds of evolution to selection with CTX and CAZ alone, and in their combined and fluctuating presence. Evolved alleles show positive correlated responses when selecting with single antibiotics. Nevertheless, pleiotropic constraints are apparent from the effects of single mutations and from selected alleles showing smaller correlated than direct responses and smaller responses after simultaneous and fluctuating selection with both than with single antibiotics. We speculate that these constraints result from structural changes in the oxyanion pocket surrounding the active site, where accommodation of CTX and the larger CAZ is balanced against their positioning with respect to the active site. Our findings suggest limited benefits from the combined or fluctuating application of these related cephalosporins for containing antibiotic resistance. PMID:25861383

  10. Coevolutionary Landscape Inference and the Context-Dependence of Mutations in Beta-Lactamase TEM-1

    PubMed Central

    Figliuzzi, Matteo; Jacquier, Hervé; Schug, Alexander; Tenaillon, Oliver; Weigt, Martin

    2016-01-01

    The quantitative characterization of mutational landscapes is a task of outstanding importance in evolutionary and medical biology: It is, for example, of central importance for our understanding of the phenotypic effect of mutations related to disease and antibiotic drug resistance. Here we develop a novel inference scheme for mutational landscapes, which is based on the statistical analysis of large alignments of homologs of the protein of interest. Our method is able to capture epistatic couplings between residues, and therefore to assess the dependence of mutational effects on the sequence context where they appear. Compared with recent large-scale mutagenesis data of the beta-lactamase TEM-1, a protein providing resistance against beta-lactam antibiotics, our method leads to an increase of about 40% in explicative power as compared with approaches neglecting epistasis. We find that the informative sequence context extends to residues at native distances of about 20 Å from the mutated site, reaching thus far beyond residues in direct physical contact. PMID:26446903

  11. Power Line Noise in Transient Electromagnetic (TEM) Data: Identification and Removal in a Practical Field Study.

    NASA Astrophysics Data System (ADS)

    Jernsletten, J. A.

    2004-05-01

    INTRODUCTION: To evaluate the appropriateness of TEM in mapping deep groundwater tables (in Mars analog environmnets), a field study was carried out in the desert ~30 miles SW of Tucson, Arizona. The study was also designed to observe effects of powerline noise on TEM data. The clay-rich soil in the area is quite conductive. The study consisted of 40 in-loop TEM stations, divided into 3 lines, for 4 line-km of data. The survey was carried out by a crew of one person, with square Tx wire loops 100 m on a side, and a ferrite-core magnetic coil Rx antenna in the center of each Tx loop. Maximum useful depth of investigation achieved was ~600 m. TEM DATA: The field area is surrounded by powerlines on all 4 sides: Line 1 has the outside of the first Tx loop under the powerline to the West; Line 2 starts with the powerline to the North passing above just inside its first Tx loop, and ends with the outside of the last station's transmitter loop ~20 m shy of the powerline to the South; finally, Line 3 starts ~50 m East of the powerline to the West, and runs parallel to the powerline to the South along its entire length, at a separation distance of ~70 m. Line 3 was placed largely in an effort to obeserve powerline noise. The decay curve for the first station on Line 1(Line 1/Station 50) is raised above the other curves from Line 1. This is due to the charge (noise) from the adjacent powerline, which is at a distance of ~50 m from the Rx coil. In effect, the transient decay is recorded as being slower than it would be without the presence of the powerline. This also artficially lowers the apparent resistivity, readily observed in Line 1/Station 50 data. These effects are present to a lesser extent (lower magnitude noise) in the data from Line1/Station 150, the second station on Line 1. On the smooth-model inversion cross-section of the data from Line 1, the effects of the powerline noise appears as a pulling up of the low-resistivity water table contact towards the surface

  12. In situ TEM visualization of superior nanomechanical flexibility of shear-exfoliated phosphorene.

    PubMed

    Xu, Feng; Ma, Hongyu; Lei, Shuangying; Sun, Jun; Chen, Jing; Ge, Binghui; Zhu, Yimei; Sun, Litao

    2016-07-14

    Recently discovered atomically thin black phosphorus (called phosphorene) holds great promise for applications in flexible nanoelectronic devices. Experimentally identifying and characterizing nanomechanical properties of phosphorene are challenging, but also potentially rewarding. This work combines for the first time in situ transmission electron microscopy (TEM) imaging and an in situ micro-manipulation system to directly visualize the nanomechanical behaviour of individual phosphorene nanoflakes. We demonstrate that the phosphorene nanoflakes can be easily bent, scrolled, and stretched, showing remarkable mechanical flexibility rather than fracturing. An out-of-plane plate-like bending mechanism and in-plane tensile strain of up to 34% were observed. Moreover, a facile liquid-phase shear exfoliation route has been developed to produce such mono-layer and few-layer phosphorene nanoflakes in organic solvents using only a household kitchen blender. The effects of surface tensions of the applied solvents on the ratio of average length and thickness (L/T) of the nanoflakes were studied systematically. The results reported here will pave the way for potential industrial-scale applications of flexible phosphorene nanoelectronic devices.

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

    SciTech Connect

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

    2014-04-01

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

  14. The Telemedical Rescue Assistance System "TemRas"--development, first results, and impact.

    PubMed

    Büscher, Christian; Elsner, Jesko; Schneiders, Marie-Thérèse; Thelen, Sebastian; Brodziak, Tadeusz; Seidenberg, Peter; Schilberg, Daniel; Tobias, Michael; Jeschke, Sabina

    2014-04-01

    German emergency medical services (EMS) face the challenge of ensuring high-quality emergency care against a background of continuously increasing numbers of emergency missions, resource shortages concomitant with greatly increased arrival times, particularly in rural areas. Because German EMS physicians are at maximum capacity, an immediate response is not always possible, and thus delays in commencing advanced life support measures sometimes occur. In such scenarios, paramedics start the initial treatment until the EMS physician arrives. The delayed availability of a physician can defer the decision process of the paramedics and thus postpone the start of the patient's essential treatment, which is particularly dangerous during the care of cardiovascular emergencies. Therefore, the project Telemedical Rescue Assistance System (TemRas) has developed an innovative concept to improve quality of emergency care. The objective is to introduce so-called tele-EMS physicians providing remote medical support for the emergency team on site by transmitting audio and video data as well as vital signs and 12-lead-ECG from the emergency site to a teleconsultation center. In this article, the development process as well as the first results of the evaluation phase and the impact for further use of telemedicine in EMS are presented. PMID:24445230

  15. Energy-filtering TEM at high magnification: spatial resolution and detection limits.

    PubMed

    Grogger, Werner; Schaffer, Bernhard; Krishnan, Kannan M; Hofer, Ferdinand

    2003-09-01

    Energy-filtering TEM (EFTEM) has turned out to be a very efficient and rapid tool for the chemical characterization of a specimen on a nanometer and even subnanometer length scale. Especially, the detection and measurement of very thin layers has become a great application of this technique in many materials science fields, e.g. semiconductors and hard disk technology. There, the reliability of compositional profiles is an important issue. However, the experimentally obtainable spatial resolution strongly influences the appearance of a thin layer in an EFTEM image, when dimensions reach subnanometer levels, which mainly leads to a broadening of the layer in the image. This fact has to be taken into account, when measuring the thickness of such a thin layer. Additionally, the convolution decreases contrast which makes the layer less visible in the image and finally determines the detection limit. In this work we present a systematic study on specifically designed Mn/PdMn multilayer test specimens to explore the practical aspects of spatial resolution and detection limits in EFTEM. Although specific to the ionization edges used, we will present general conclusions about the practical limitations in terms of EFTEM spatial resolution. Additionally, work will be shown about low energy-loss imaging of thin oxide layers, where delocalization is the main factor responsible for broadening. PMID:12871810

  16. Comparison Between Eight- and Sixteen-Channel TEM Transceive Arrays for Body Imaging at 7 Tesla

    PubMed Central

    Snyder, CJ; DelaBarre, L; Moeller, S; Tian, J; Akgun, C; Van De Moortele, P-F; Bolan, PJ; Ugurbil, K; Vaughan, JT; Metzger, GJ

    2011-01-01

    Eight- and sixteen-channel transceive stripline/TEM body arrays were compared at 7 tesla (297 MHz) both in simulation and experimentally. Despite previous demonstrations of similar arrays for use in body applications, a quantitative comparison of the two configurations has not been undertaken to date. Results were obtained on a male pelvis for assessing transmit, SNR and parallel imaging performance and to evaluate local power deposition versus transmit B1 (B1+). All measurements and simulations were conducted after performing local B1+ phase shimming in the region of the prostate. Despite the additional challenges of decoupling immediately adjacent coils, the sixteen-channel array demonstrated improved or nearly equivalent performance to the eight-channel array based on the evaluation criteria. Experimentally, transmit performance and SNR were 22% higher for the sixteen-channel array while significantly increased reduction factors were achievable in the left-right direction for parallel imaging. Finite-difference time-domain simulations demonstrated similar results with respect to transmit and parallel imaging performance, however a higher transmit efficiency advantage of 33% was predicted. Simulations at both 3T and 7T verified the expected parallel imaging improvements with increasing field strength and showed that, for a specific B1+ shimming strategy employed, the sixteen-channel array exhibited lower local and global SAR for a given B1+. PMID:22102483

  17. Helical superstructure of continuum graphene cone uncovered by TEM analysis of herringbone-striped pattern in graphitic whiskers

    NASA Astrophysics Data System (ADS)

    Saito, Yukie; Nishio-Hamane, Daisuke

    2016-10-01

    Cone-shaped graphitic whiskers (CGWs) are a form of pyrolytic carbon, consisting of conically stacked hexagonal carbon layers with an apex angle of 135-140°. Under transmission electron microscopy (TEM), CGWs often exhibit herringbone-striped patterns. Bright-field (BF) and dark-field (DF) TEM images indicated that the stripes are due to periodical appearance of a strong inter-planar reflection, which is consistent with helical rotation of layers with stepwise "layer overlap". High-resolution TEM revealed that the period was 14-15 layers. The relationship between apex angle and stripe periodicity of CGWs could be consistently explained in terms of a helical superstructure of tightly coiled continuous graphene cone.

  18. In situ TEM studies of micron-sized all-solid-state fluoride ion batteries: Preparation, prospects, and challenges.

    PubMed

    Hammad Fawey, Mohammed; Chakravadhanula, Venkata Sai Kiran; Reddy, Munnangi Anji; Rongeat, Carine; Scherer, Torsten; Hahn, Horst; Fichtner, Maximilian; Kübel, Christian

    2016-07-01

    Trustworthy preparation and contacting of micron-sized batteries is an essential task to enable reliable in situ TEM studies during electrochemical biasing. Some of the challenges and solutions for the preparation of all-solid-state batteries for in situ TEM electrochemical studies are discussed using an optimized focused ion beam (FIB) approach. In particular redeposition, resistivity, porosity of the electrodes/electrolyte and leakage current are addressed. Overcoming these challenges, an all-solid-state fluoride ion battery has been prepared as a model system for in situ TEM electrochemical biasing studies and first results on a Bi/La0.9 Ba0.1 F2.9 half-cell are presented. Microsc. Res. Tech. 79:615-624, 2016. © 2016 Wiley Periodicals, Inc. PMID:27145192

  19. In Situ TEM Observations on the Sulfur-Assisted Catalytic Growth of Single-Wall Carbon Nanotubes.

    PubMed

    Zhang, Lili; Hou, Peng-Xiang; Li, Shisheng; Shi, Chao; Cong, Hong-Tao; Liu, Chang; Cheng, Hui-Ming

    2014-04-17

    The effect of sulfur on the catalytic nucleation and growth of single-wall carbon nanotubes (SWCNTs) from an iron catalyst was investigated in situ by transmission electron microscopy (TEM). The catalyst precursor of ferrocene and growth promoter of sulfur were selectively loaded inside of the hollow core of multiwall CNTs with open ends, which served as a nanoreactor powered by applying a voltage inside of the chamber of a TEM. It was found that a SWCNT nucleated and grew perpendicularly from a region of the catalyst nanoparticle surface, instead of the normal tangential growth that occurs with no sulfur addition. Our in situ TEM observation combined with CVD growth studies suggests that sulfur functions to promote the nucleation and growth of SWCNTs by forming inhomogeneous local active sites and modifying the interface bonding between catalysts and precipitated graphitic layers, so that carbon caps can be lifted off from the catalyst particle. PMID:26269989

  20. From dilute isovalent substitution to alloying in CdSeTe nanoplatelets† †Electronic supplementary information (ESI) available: TEM, XRD, TA and PLE experimental results. Detailed analysis of the PL fit of alloyed NPLs and spectral peak asymmetry of the doped NPLs. See DOI: 10.1039/c6cp01177b Click here for additional data file.

    PubMed Central

    Tenne, Ron; Pedetti, Silvia; Ithurria, Sandrine; Houben, Lothar; Nadal, Brice; Oron, Dan; Dubertret, Benoit

    2016-01-01

    Cadmium chalcogenide nanoplatelet (NPL) synthesis has recently witnessed a significant advance in the production of more elaborate structures such as core/shell and core/crown NPLs. However, controlled doping in these structures has proved difficult because of the restrictive synthetic conditions required for 2D anisotropic growth. Here, we explore the incorporation of tellurium (Te) within CdSe NPLs with Te concentrations ranging from doping to alloying. For Te concentrations higher than ∼30%, the CdSexTe(1–x) NPLs show emission properties characteristic of an alloyed material with a bowing of the band gap for increased concentrations of Te. This behavior is in line with observations in bulk samples and can be put in the context of the transition from a pure material to an alloy. In the dilute doping regime, CdSe:Te NPLs, in comparison to CdSe NPLs, show a distinct photoluminescence (PL) red shift and prolonged emission lifetimes (LTs) associated with Te hole traps which are much deeper than in bulk samples. Furthermore, single particle spectroscopy reveals dramatic modifications in PL properties. In particular, doped NPLs exhibit photon antibunching and emission dynamics significantly modified compared to undoped or alloyed NPLs. PMID:27211113

  1. XRD and mineralogical analysis of gypsum dunes at White Sands National Monument, New Mexico and applications to gypsum detection on Mars

    NASA Astrophysics Data System (ADS)

    Lafuente, B.; Bishop, J. L.; Fenton, L. K.; King, S. J.; Blake, D.; Sarrazin, P.; Downs, R.; Horgan, B. H.

    2013-12-01

    A field portable X-ray Diffraction (XRD) instrument was used at White Sands National Monument to perform in-situ measurements followed by laboratory analyses of the gypsum-rich dunes and to determine its modal mineralogy. The field instrument is a Terra XRD (Olympus NDT) based on the technology of the CheMin (Chemistry and Mineralogy) instrument onboard the Mars Science Laboratory (MSL) rover Curiosity which is providing the mineralogical and chemical composition of scooped soil samples and drilled rock powders collected at Gale Crater [1]. Using Terra at White Sands will contribute to 'ground truth' for gypsum-bearing environments on Mars. Together with data provided by VNIR spectra [2], this study clarifies our understanding of the origin and history of gypsum-rich sand dunes discovered near the northern polar region of Mars [3]. The results obtained from the field analyses performed by XRD and VNIR spectroscopy in four dunes at White Sands revealed the presence of quartz and dolomite. Their relative abundance has been estimated using the Reference Intensity Ratio (RIR) method. For this study, particulate samples of pure natural gypsum, quartz and dolomite were used to prepare calibration mixtures of gypsum-quartz and gypsum-dolomite with the 90-150μm size fractions. All single phases and mixtures were analyzed by XRD and RIR factors were calculated. Using this method, the relative abundance of quartz and dolomite has been estimated from the data collected in the field. Quartz appears to be present in low amounts (2-5 wt.%) while dolomite is present at percentages up to 80 wt.%. Samples from four dunes were collected and prepared for subsequent XRD analysis in the lab to estimate their composition and illustrate the changes in mineralogy with respect to location and grain size. Gypsum-dolomite mixtures: The dolomite XRD pattern is dominated by an intense diffraction peak at 2θ≈36 deg. which overlaps a peak of gypsum, This makes low concentrations of dolomite

  2. Network Analysis of Sequence-Function Relationships and Exploration of Sequence Space of TEM β-Lactamases.

    PubMed

    Zeil, Catharina; Widmann, Michael; Fademrecht, Silvia; Vogel, Constantin; Pleiss, Jürgen

    2016-05-01

    The Lactamase Engineering Database (www.LacED.uni-stuttgart.de) was developed to facilitate the classification and analysis of TEM β-lactamases. The current version contains 474 TEM variants. Two hundred fifty-nine variants form a large scale-free network of highly connected point mutants. The network was divided into three subnetworks which were enriched by single phenotypes: one network with predominantly 2be and two networks with 2br phenotypes. Fifteen positions were found to be highly variable, contributing to the majority of the observed variants. Since it is expected that a considerable fraction of the theoretical sequence space is functional, the currently sequenced 474 variants represent only the tip of the iceberg of functional TEM β-lactamase variants which form a huge natural reservoir of highly interconnected variants. Almost 50% of the variants are part of a quartet. Thus, two single mutations that result in functional enzymes can be combined into a functional protein. Most of these quartets consist of the same phenotype, or the mutations are additive with respect to the phenotype. By predicting quartets from triplets, 3,916 unknown variants were constructed. Eighty-seven variants complement multiple quartets and therefore have a high probability of being functional. The construction of a TEM β-lactamase network and subsequent analyses by clustering and quartet prediction are valuable tools to gain new insights into the viable sequence space of TEM β-lactamases and to predict their phenotype. The highly connected sequence space of TEM β-lactamases is ideally suited to network analysis and demonstrates the strengths of network analysis over tree reconstruction methods.

  3. Implication of Ile-69 and Thr-182 residues in kinetic characteristics of IRT-3 (TEM-32) beta-lactamase.

    PubMed Central

    Farzaneh, S; Chaibi, E B; Peduzzi, J; Barthelemy, M; Labia, R; Blazquez, J; Baquero, F

    1996-01-01

    The substitution of a methionine for an isoleucine at position 69 (Met69Ile), which causes inhibitor resistance to TEM-type beta-lactamases (IRT-3 and IRT-I69), altered the positions of the Asn-170 and Glu-166 side chains as well as the position of the catalytic water molecule. A novel hydrogen bond between the hydroxyl of Thr-182 and the carbonyl of Glu-64 was expected to be responsible for the increase in the catalytic activity of the IST-T182 and IRT-3 enzymes compared with those of TEM-1 and IRT-169, respectively. PMID:8891161

  4. TEM characterization of dislocations in TiB2 particles after hypervelocity impact.

    PubMed

    Guo, Q; Li, J F; Hou, L L; Sun, D L

    2014-12-01

    Characteristic of dislocations in TiB2 particles associated with hypervelocity impact craters in 65 vol.% TiB2/Al composite were investigated by transmission electron microscopy (TEM). Two kinds of dislocation networks in as-impacted TiB2 particles were identified. One is hexagonal dislocation networks including 1/3〈1̄21̄0〉, 〈0001〉, 1/3〈1̄21̄3〉 type dislocations on {0001}, {101̄0}, and {123̄0} planes. Another one is the hexagonal dislocation networks including 1/3〈112̄0〉, 〈0001〉, and 1/3〈112̄3〉 type dislocations on {0001}, {101̄0}, and {11̄00} planes. Formation of dislocation network should be contributed to the parallel sets of "a" type dislocations (1/3〈112̄0〉 or 1/3〈1̄21̄0〉 type dislocations) reacting with parallel sets of "b" type dislocations (〈0001〉 type dislocations) to form "c" type dislocations (1/3〈112̄3〉 or 1/3〈1̄21̄3〉 type dislocations). Moreover, dislocations reaction processes do not result in an energy reduction, and are called quasi-equilibrium configurations. Formation of dislocations may result from high temperature or pressure generated by hypervelocity impact. During the cooling from high temperature and unloading from high pressure, dislocations in TiB2 particles rearranged and transformed to dislocation networks to lower the defect energy. PMID:25108104

  5. SEM and TEM Characterization of As-Fabricated U-7Mo Disperson Fuel Plates

    SciTech Connect

    D. D. Keiser, Jr.; B. Yao; E. Perez; Y. H. Sohn

    2009-11-01

    The starting microstructure of a dispersion fuel plate can have a dramatic impact on the overall performance of the plate during irradiation. To improve the understanding of the as-fabricated microstructures of dispersion fuel plates, SEM and TEM analysis have been performed on RERTR-9A archive fuel plates, which went through an additional hot isostatic procsssing (HIP) step during fabrication. The fuel plates had depleted U-7Mo fuel particles dispersed in either Al-2Si or 4043 Al alloy matrix. For the characterized samples, it was observed that a large fraction of the ?-phase U-7Mo alloy particles had decomposed during fabrication, and in areas near the fuel/matrix interface where the transformation products were present significant fuel/matrix interaction had occurred. Relatively thin Si-rich interaction layers were also observed around the U-7Mo particles. In the thick interaction layers, (U)(Al,Si)3 and U6Mo4Al43 were identified, and in the thin interaction layers U(Al,Si)3, U3Si3Al2, U3Si5, and USi1.88-type phases were observed. The U3Si3Al2 phase contained some Mo. Based on the results of this work, exposure of dispersion fuel plates to relatively high temperatures during fabrication impacts the overall microstructure, particularly the nature of the interaction layers around the fuel particles. The time and temperature of fabrication should be carefully controlled in order to produce the most uniform Si-rich layers around the U-7Mo particles.

  6. From olivine to ringwoodite: a TEM study of a complex process

    NASA Astrophysics Data System (ADS)

    Pittarello, Lidia; Ji, Gang; Yamaguchi, Akira; Schryvers, Dominique; Debaille, Vinciane; Claeys, Philippe

    2015-05-01

    The study of shock metamorphism of olivine might help to constrain impact events in the history of meteorites. Although shock features in olivine are well known, so far, there are processes that are not yet completely understood. In shock veins, olivine clasts with a complex structure, with a ringwoodite rim and a dense network of lamellae of unidentified nature in the core, have been reported in the literature. A highly shocked (S5-6), L6 meteorite, Asuka 09584, which was recently collected in Antarctica by a Belgian-Japanese joint expedition, contains this type of shocked olivine clasts and has been, therefore, selected for detailed investigations of these features by transmission electron microscopy (TEM). Petrographic, geochemical, and crystallographic studies showed that the rim of these shocked clasts consists of an aggregate of nanocrystals of ringwoodite, with lower Mg/Fe ratio than the unshocked olivine. The clast's core consists of an aggregate of iso-oriented grains of olivine and wadsleyite, with higher Mg/Fe ratio than the unshocked olivine. This aggregate is crosscut by veinlets of nanocrystals of olivine, with extremely low Mg/Fe ratio. The formation of the ringwoodite rim is likely due to solid-state, diffusion-controlled, transformation from olivine under high-temperature conditions. The aggregate of iso-oriented olivine and wadsleyite crystals is interpreted to have formed also by a solid-state process, likely by coherent intracrystalline nucleation. Following the compression, shock release is believed to have caused opening of cracks and fractures in olivine and formation of olivine melt, which has lately crystallized under postshock equilibrium pressure conditions as olivine.

  7. Comparative studies of thin film growth on aluminium by AFM, TEM and GDOES characterization

    NASA Astrophysics Data System (ADS)

    Qi, Jiantao; Thompson, George E.

    2016-07-01

    In this present study, comparative studies of trivalent chromium conversion coating formation, associated with aluminium dissolution process, have been investigated using atomic force microscopy (AFM), transmission electron microscopy (TEM) and glow-discharge optical emission spectroscopy (GDOES). High-resolution electron micrographs revealed the evident and uniform coating initiation on the whole surface after conversion treatment for only 30 s, although a network of metal ridges was created by HF etching pre-treatment. In terms of conversion treatment process on electropolished aluminium, constant kinetics of coating growth, ∼0.30 ± 0.2 nm/s, were found after the prolonged conversion treatment for 600 s. The availability of electrolyte anions for coating deposition determined the growth process. Simultaneously, a proceeding process of aluminium dissolution during conversion treatment, of ∼0.11 ± 0.02 nm/s, was found for the first time, indicating constant kinetics of anodic reactions. The distinct process of aluminium consumption was assigned with loss of corrosion protection of the deposited coating material as evidenced in the electrochemical impedance spectroscopy. Based on the present data, a new mechanism of coating growth on aluminium was proposed, and it consisted of an activation period (0-30 s), a linear growth period (0.30 nm/s, up for 600 s) and limited growth period (0.17 nm/s, 600-1200 s). In addition, the air-drying post-treatment and a high-vacuum environment in the microscope revealed a coating shrinkage, especially in the coatings after conversion treatments for longer time.

  8. Ethiopian Geothermal Resources Inferred from Electromagnetic (AMT/MT, TEM) Data and Seismic Noise Interferometry

    NASA Astrophysics Data System (ADS)

    Lindsey, N. J.; Whaler, K. A.; Johnson, N.; Baptie, B.; Lemma, Y.; Desissa, M.; Ebinger, C. J.; Belachew, M.; Keir, D.; Fisseha, S.; Dawes, G.; Hautot, S.

    2012-12-01

    In Ethiopia, modern energy (hydroelectricity and foreign petroleum) is expensive and unpredictable, yet energy access is key to sustainable development. Active volcanoes and hot springs located in the slow-spreading rift zone of the Afar Depression suggest an abundant geothermal energy resource; however, before this energy can be utilized subsurface geophysical analysis is needed to study the geothermal system, its potential and identify drilling targets. The aim of this project is to use geophysical data (audio-magnetotelluric (AMT), magnetotelluric (MT), transient-electromagnetic (TEM) and passive seismic data), recently recorded in the Northern Tendaho Graben of Afar, Ethiopia, to constrain geothermal system parameters (i.e. geology, temperature, fluid properties, etc.). Recovery of these parameters enables the understanding of reservoir heat flow, geothermal energy potential, economic viability and development of an optimal drilling strategy. The AMT/MT data were recorded at 28 sites along two parallel profiles oriented perpendicular to regional geologic strike. Two-dimensional joint inversion of the TE and TM modes from all sites identifies two very strong conducting layers (~1 Ohm-m), at <500 m and 5-10 km, separated by a more resistive layer (~50 Ohm-m). This model is strongly correlated with borehole information. The deeper high conductivity anomaly shallows toward the center of the profile, at the location of highest recorded fluid temperature from early drilling operations. MT impedance tensor decomposition, phase tensor analysis and induction vector calculations, as well as forward modelling of the inversion results are mutually consistent. Two-dimensional surface wave tomography results from seismic noise interferometry add another layer of geophysical information to this interdisciplinary study, complementing the AMT/MT survey. This project was funded by the US-UK Fulbright Commission and the University of Edinburgh, and benefited from strong

  9. Nanoanalytical TEM Studies and Micromagnetic Modelling of Nd-Fe-B Magnets

    NASA Astrophysics Data System (ADS)

    Zickler, Gregor A.; Toson, Peter; Asali, Ahmad; Fidler, Josef

    We have analysed the influence of the microstructural features, such as intergranular grain boundary (GB) phases and misalignment of the hard magnetic grains, on the optimization of magnetization reversal processes in order to improve the coercive field of Nd-Fe-B magnets. The microstructural model of the grains and intergranular phases, which is used for theoretical simulations, has been derived from a detailed nanoanalytical TEM/STEM study of a Dy/Tb free magnet and a high coercive (Nd,Tb)-Fe-B magnet. Special attention is laid on the EELS analysis of GB with a thickness ranging from 2 - 30 nm. This analysis identified the majority of the GB phases to have about 50 -70 at.% of iron and only a few GBs, which are connecting two nearby grain boundary junctions (GBj), possess a similar chemical composition as the adjacent GBj with a low iron content (< 10 at. %) and a high rare earth and oxygen content. Finite element micromagnetic simulations have been carried out in order to study the influence of internal demagnetizing fields determined by the microstructure on the magnetization switching behaviour. Special emphasis was put on the influence of the GB and their magnetic properties, due to their substantial influence on the nucleation of reverse magnetic domains and the pinning of domain walls. The strongest reduction of the coercive field is caused by GB with soft ferromagnetic properties. Shielding the Nd-Fe-B grains from the nucleation sites at the GBj with Dy or Tb shells, leads to an increase of the coercivity from 2.5 to 3.6 T and 2.5 to 4.3 T, respectively.

  10. Synthesis, thermal, XRD and spectroscopic studies characterization of Tutton salt K2M (SO4)2·6H2O (M = Mg, Ni)

    NASA Astrophysics Data System (ADS)

    Marzougui, H.; Attia-Essaies, S.; Ben Hassen-Chehimi, D.

    2016-09-01

    Tutton's salts K2M(SO4)2·6H2O (M = Mg, Ni) have been synthesized by the slow evaporation method at room temperature. A complete structural characterization has been carried out by means of powder X-ray diffraction (XRD). The results indicate that the structure of these salts is monoclinic system with the space group P21/a (Z = 2). IR and Raman spectra of KMS6 (M = Mg,Ni) have been recorded and analyzed. From the spectra, the vibrations due to SO42- ion, the complex [M(H2O)6]2+ and the water molecules have been identified. Thermogravimetry, differential thermal analysis and XRD at high-temperature investigations show that the dehydration of these salts occurs between 300 and 500 K. This indicates the removal of all water molecules around 426 K.

  11. Multiscale structural characterizations of mixed U(iv)-An(iii) oxalates (An(iii) = Pu or Am) combining XAS and XRD measurements.

    PubMed

    Arab-Chapelet, B; Martin, P M; Costenoble, S; Delahaye, T; Scheinost, A C; Grandjean, S; Abraham, F

    2016-04-28

    Mixed actinide(III,IV) oxalates of the general formula M2.2UAn(C2O4)5·nH2O (An = Pu or Am and M = H3O(+) and N2H5(+)) have been quantitatively precipitated by oxalic precipitation in nitric acid medium (yield >99%). Thorough multiscale structural characterization using XRD and XAS measurements confirmed the existence of mixed actinide oxalate solid solutions. The XANES analysis confirmed that the oxidation states of the metallic cations, tetravalent for uranium and trivalent for plutonium and americium, are maintained during the precipitation step. EXAFS measurements show that the local environments around U(+IV), Pu(+III) and Am(+III) are comparable, and the actinides are surrounded by ten oxygen atoms from five bidentate oxalate anions. The mean metal-oxygen distances obtained by XAS measurements are in agreement with those calculated from XRD lattice parameters. PMID:26979820

  12. Quantitative assessment of alkali-reactive aggregate mineral content through XRD using polished sections as a supplementary tool to RILEM AAR-1 (petrographic method)

    SciTech Connect

    Castro, Nelia; Sorensen, Bjorn E.; Broekmans, Maarten A.T.M.

    2012-11-15

    The mineral content of 5 aggregate samples from 4 different countries, including reactive and non-reactive aggregate types, was assessed quantitatively by X-ray diffraction (XRD) using polished sections. Additionally, electron probe microanalyzer (EPMA) mapping and cathodoluminescence (CL) were used to characterize the opal-CT identified in one of the aggregate samples. Critical review of results from polished sections against traditionally powdered specimen has demonstrated that for fine-grained rocks without preferred orientation the assessment of mineral content by XRD using polished sections may represent an advantage over traditional powder specimens. Comparison of data on mineral content and silica speciation with expansion data from PARTNER project confirmed that the presence of opal-CT plays an important role in the reactivity of one of the studied aggregates. Used as a complementary tool to RILEM AAR-1, the methodology suggested in this paper has the potential to improve the strength of the petrographic method.

  13. Combining µXANES and µXRD mapping to analyse the heterogeneity in calcium carbonate granules excreted by the earthworm Lumbricus terrestris.

    PubMed

    Brinza, Loredana; Schofield, Paul F; Hodson, Mark E; Weller, Sophie; Ignatyev, Konstantin; Geraki, Kalotina; Quinn, Paul D; Mosselmans, J Frederick W

    2014-01-01

    The use of fluorescence full spectral micro-X-ray absorption near-edge structure (µXANES) mapping is becoming more widespread in the hard energy regime. This experimental method using the Ca K-edge combined with micro-X-ray diffraction (µXRD) mapping of the same sample has been enabled on beamline I18 at Diamond Light Source. This combined approach has been used to probe both long- and short-range order in calcium carbonate granules produced by the earthworm Lumbricus terrestris. In granules produced by earthworms cultured in a control artificial soil, calcite and vaterite are observed in the granules. However, granules produced by earthworms cultivated in the same artificial soil amended with 500 p.p.m. Mg also contain an aragonite. The two techniques, µXRD and µXANES, probe different sample volumes but there is good agreement in the phase maps produced. PMID:24365942

  14. High temperature XRD of Cu{sub 2.1}Zn{sub 0.9}SnSe{sub 4}

    SciTech Connect

    Chetty, Raju Mallik, Ramesh Chandra

    2014-04-24

    Quaternary compound with chemical composition Cu{sub 2.1}Zn{sub 0.9}SnSe{sub 4} is prepared by solid state synthesis. High temperature XRD (X-Ray Diffraction) of this compound is used in studying the effect of temperature on lattice parameters and thermal expansion coefficients. Thermal expansion coefficient is one of the important quantities in evaluating the Grüneisen parameter which further useful in determining the lattice thermal conductivity of the material. The high temperature XRD of the material revealed that the lattice parameters as well as thermal expansion coefficients of the material increased with increase in temperature which confirms the presence of anharmonicty.

  15. XRF, μ-XRD and μ-spectroscopic techniques for revealing the composition and structure of paint layers on polychrome sculptures after multiple restorations.

    PubMed

    Franquelo, M L; Duran, A; Castaing, J; Arquillo, D; Perez-Rodriguez, J L

    2012-01-30

    This paper presents the novel application of recently developed analytical techniques to the study of paint layers on sculptures that have been restored/repainted several times across centuries. Analyses were performed using portable XRF, μ-XRD and μ-Raman instruments. Other techniques, such as optical microscopy, SEM-EDX and μ-FTIR, were also used. Pigments and other materials including vermilion, minium, red lac, ivory black, lead white, barium white, zinc white (zincite), titanium white (rutile and anatase), lithopone, gold and brass were detected. Pigments from both ancient and modern times were found due to the different restorations/repaintings carried out. μ-Raman was very useful to characterise some pigments that were difficult to determine by μ-XRD. In some cases, pigments identification was only possible by combining results from the different analytical techniques used in this work. This work is the first article devoted to the study of sculpture cross-section samples using laboratory-made μ-XRD systems.

  16. Fast-Turnoff Transient Electromagnetic (TEM) Field Study at the Mars Analog Site of Rio Tinto, Spain

    NASA Astrophysics Data System (ADS)

    Jernsletten, J. A.

    2005-03-01

    This report describes a Fast-Turnoff Transient Electromagnetic (TEM) study at the Peña de Hierro ("Berg of Iron") field area of the Mars Analog Research and Technology Experiment (MARTE), near the towns Rio Tinto and Nerva, Andalucia region, Spain.

  17. Homology modeling and virtual screening of inhibitors against TEM- and SHV-type-resistant mutants: A multilayer filtering approach.

    PubMed

    Baig, Mohammad H; Balaramnavar, Vishal M; Wadhwa, Gulshan; Khan, Asad U

    2015-01-01

    TEM and SHV are class-A-type β-lactamases commonly found in Escherichia coli and Klebsiella pneumoniae. Previous studies reported S130G and K234R mutations in SHVs to be 41- and 10-fold more resistant toward clavulanic acid than SHV-1, respectively, whereas TEM S130G and R244S also showed the same level of resistance. These selected mutants confer higher level of resistance against clavulanic acid. They also show little susceptibility against other commercially available β-lactamase inhibitors. In this study, we have used docking-based virtual screening approach in order to screen potential inhibitors against some of the major resistant mutants of SHV and TEM types β-lactamase. Two different inhibitor-resistant mutants from SHV and TEM were selected. Moreover, we have retained the active site water molecules within each enzyme. Active site water molecules were placed within modeled structure of the mutant whose structure was unavailable with protein databank. The novelty of this work lies in the use of multilayer virtual screening approach for the prediction of best and accurate results. We are reporting five inhibitors on the basis of their efficacy against all the selected resistant mutants. These inhibitors were selected on the basis of their binding efficacies and pharmacophore features.

  18. PROPOSED ASTM METHOD FOR THE DETERMINATION OF ASBESTOS IN AIR BY TEM AND INFORMATION ON INTERFERING FIBERS

    EPA Science Inventory

    The draft of the ASTM Test Method for air entitled: "Airborne Asbestos Concentration in Ambient and Indoor Atmospheres as Determined by Transmission Electron Microscopy Direct Transfer (TEM)" (ASTM Z7077Z) is an adaptation of the International Standard, ISO 10312. It is currently...

  19. Characterizing the Phyllosilicates and Amorphous Phases Found by MSL Using Laboratory XRD and EGA Measurements of Natural and Synthetic Materials (Invited)

    NASA Astrophysics Data System (ADS)

    Rampe, E. B.; Morris, R. V.; Chipera, S.; Bish, D. L.; Bristow, T.; Archer, P. D.; Blake, D.; Achilles, C.; Ming, D. W.; Vaniman, D.; Crisp, J. A.; Des Marais, D. J.; Downs, R.; Farmer, J. D.; Morookian, J.; Morrison, S.; Sarrazin, P.; Spanovich, N.; Treiman, A. H.; Yen, A. S.; Team, M.

    2013-12-01

    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

  20. A Concept for the Development of Spatially Resolved Measurements for Soil Moisture with TEM Waveguides

    NASA Astrophysics Data System (ADS)

    Lapteva, Yulia; Schmidt, Felix; Bumberger, Jan

    2014-05-01

    's equations. It describes the one-dimensional wave propagation in a multi-layered medium, assuming the wave to be transverse electromagnetic (TEM). In the particular case of transmission lines with perpendicularly arranged layer transitions this assumption is very close to reality. Such waveguides and their frequency domain measurements in layered media are promising concerning a development ways working with soil moisture detection.

  1. TEM characterization of Au-based alloys to join YSZ to steel for SOFC applications

    SciTech Connect

    Lin, Kun-Lin; Singh, Mrityunjay; Asthana, Rajiv

    2012-01-15

    The microstructures of two gold-based alloys with compositions (in wt.%) of 96.4Au-3Ni-0.6Ti and 97.5Au-0.75Ni-1.75V following oxidation at 850 Degree-Sign C for 200 min were characterized by analytical transmission electron microscopy with energy dispersive spectroscopy and by scanning electron microscopy. In the oxidized 96.4Au-3Ni-0.6Ti interlayer, a dense scale composed of nickel oxide (NiO) and nickel titanate (NiTiO{sub 3}) formed at the alloy surface. No evidence of titanium oxide was found because there was not enough Ti present to form titanium oxide. In the oxidized 97.5Au-0.75Ni-1.75V interlayer, loose vanadium oxide (V{sub 2}O{sub 5}) and nickel vanadate (Ni{sub 2}V{sub 2}O{sub 7}) formed and were distributed within the oxidized 97.5Au-0.75Ni-1.75V interlayer. Similarly, because of the low Ni content in the alloys, no NiO formed. The oxide products in the 96.4Au-3Ni-0.6Ti and 97.5Au-0.75Ni-1.75V interlayers after oxidation are consistent with the Pilling-Bedworth (PB) ratio considerations. - Highlights: Black-Right-Pointing-Pointer Two commercial Au-based reactive metallic interlayers were oxidized at 850 Degree-Sign C for 200 min. Black-Right-Pointing-Pointer The oxidized products at the surface were characterized by TEM/EDS and SEM. Black-Right-Pointing-Pointer NiO and NiTiO{sub 3} formed at the oxidized 96.4Au-3Ni-0.6Ti interlayer. Black-Right-Pointing-Pointer V{sub 2}O{sub 5} and Ni{sub 2}V{sub 2}O{sub 7} were found in the oxidized 97.5Au-0.75Ni-1.75V interlayer. Black-Right-Pointing-Pointer These oxide products are consistent with the Pilling-Bedworth (PB) ratio considerations.

  2. Dynamics of early stage nano-oxidation by in situ UHV-TEM

    NASA Astrophysics Data System (ADS)

    Yang, Judith

    2011-03-01

    Environmental stability is one of the most important properties for materials exposed to air. As dimensions of engineered systems approach nanoscale, fundamental understanding of reactions with oxygen at this length scale is critical for environmental stability as well as for processing oxide nanostructures, where surface reactions are commonly utilized. The nanoscale stages of oxidation from the nucleation of the metal oxide to the formation of the thermodynamically stable oxide represent a scientifically challenging and technologically important terra incognito. The kinetics of early stage oxidation of Cu, Cu-Au and Cu-Ni alloys were visualized using in situ ultra-high vacuum transmission electron microscopy (UHV-TEM), where the initial oxidation stages can be observed in real-time under well-controlled surface conditions. We examined the dynamic responses of thin films to variations in thermodynamic variables such as temperature, oxygen pressure, strain, and crystallographic orientation. The kinetics of the nucleation and growth of three-dimensional oxide islands demonstrate that oxygen surface diffusion is the primary mechanism for oxide growth during initial oxidation in dry oxygen, and thus bears a striking resemblance to heteroepitaxy. Compared with the behavior of Cu films, the oxidation of Cu-Au alloys revealed more complexity. For example, the oxidation of (100)-oriented Cu-Au alloys with low Au content at ~ 600 C results in the formation of Cu2O oxide islands with a dendritic morphology and a non-uniform lateral distribution of Au around the islands. For Cu-Ni oxidation, the addition of Ni causes the formation Cu2O and/or NiO where the oxide type(s) and the relative orientation with the film depend on the Ni concentration, oxygen partial pressure and temperature. Evolution of the shape and size of the oxide islands can be quantitatively analyzed and provide fundamental insights into the complex kinetics and energetics of oxidation. Models based on

  3. Hydraulic and thermal soil Parameter combined with TEM data at quaternary coastal regions

    NASA Astrophysics Data System (ADS)

    Grabowski, Ima; Kirsch, Reinhard; Scheer, Wolfgang

    2014-05-01

    In order to generate a more efficient method of planning and dimensioning small- and medium sized geothermal power plants at quaternary subsurface a basic approach has been attempted. Within the EU-project CLIWAT, the coastal region of Denmark, Germany, Netherlands and Belgium has been investigated and air borne electro magnetic data was collected. In this work the regional focus was put on the isle of Föhr. To describe the subsurface with relevant parameters one need the information from drillings and geophysical well logging data. The approach to minimize costs and use existing data from state agencies led the investigation to the combination of specific electrical resistivity data and hydraulic and thermal conductivity. We worked out a basic soil/hydraulic conductivity statistic for the isle of Föhr by gathering all well logging data from the island and sorted the existing soil materials to associated kf -values. We combined specific electrical resistivity with hydraulic soil properties to generate thermal conductivity values by extracting porosity. Until now we generated a set of rough data for kf - values and thermal conductivity. The air borne TEM data sets are reliable up to 150 m below surface, depending on the conductivity of the layers. So we can suppose the same for the differentiated parameters. Since this is a very rough statistic of kf -values, further more investigation has to be made. Although the close connection to each area of investigation either over existing logging data or laboratory soil property values will remain necessary. Literature: Ahmed S, de Marsily G, Talbot A (1988): Combined Use of Hydraulic and Electrical Properties of an Aquifer in a Geostatistical Estimation of Transmissivity. - Groundwater, vol. 26 (1) Burschil T, Scheer W, Wiederhold H, Kirsch R (2012): Groundwater situation on a glacially affected barrier island. Submitted to Hydrology and Earth System Sciences - an Interactive Open Access Journal of the European

  4. High-Resolution Electron Energy-Loss Spectroscopy (HREELS) Using a Monochromated TEM/STEM

    NASA Technical Reports Server (NTRS)

    Sai, Z. R.; Bradley, J. P.; Erni, R.; Browning, N.

    2005-01-01

    A 200 keV FEI TF20 XT monochromated (scanning) transmission electron microscope funded by NASA's SRLIDAP program is undergoing installation at Lawrence Livermore National Laboratory. Instrument specifications in STEM mode are Cs =1.0 mm, Cc =1.2 mm, image resolution =0.18 nm, and in TEM mode Cs =1.3 mm, Cc =1.3 mm, information limit =0.14 nm. Key features of the instrument are a voltage-stabilized high tension (HT) supply, a monochromator, a high-resolution electron energy-loss spectrometer/energy filter, a high-resolution annular darkfield detector, and a solid-state x-ray energy-dispersive spectrometer. The high-tension tank contains additional sections for 60Hz and high frequency filtering, resulting in an operating voltage of 200 kV plus or minus 0.005V, a greater than 10-fold improvement over earlier systems. The monochromator is a single Wien filter design. The energy filter is a Gatan model 866 Tridiem-ERS high resolution GIF spec d for less than or equal to 0.15 eV energy resolution with 29 pA of current in a 2 nm diameter probe. 0.13 eV has already been achieved during early installation. The x-ray detector (EDAX/Genesis 4000) has a take-off angle of 20 degrees, an active area of 30 square millimeters, and a solid angle of 0.3 steradians. The higher solid angle is possible because the objective pole-piece allows the detector to be positioned as close as 9.47 mm from the specimen. The voltage-stabilized HT supply, monochromator and GIF enable high-resolution electron energy-loss spectroscopy (HREELS) with energy resolution comparable to synchrotron XANES, but with approximately 100X better spatial resolution. The region between 0 and 100 eV is called the low-loss or valence electron energy-loss spectroscopy (VEELS) region where features due to collective plasma oscillations and single electron transitions of valence electrons are observed. Most of the low-loss VEELS features we are detecting are being observed for the first time in IDPs. A major focus of

  5. A quantitative study of the microstructure and crystallographic fiber texture in nickel electrodeposits used in radio-frequency MEMS switches, including a new transmission electron microscopy (TEM) technique for polycrystalline films

    NASA Astrophysics Data System (ADS)

    Cantwell, Patrick R.

    The microstructure of electrodeposited nickel films in radio-frequency (RF) microelectromechanical systems (MEMS) switches has been quantitatively studied to inform and validate multi-scale, multi-physics computer simulations that aim to predict the lifetime and failure mechanisms of the RF MEMS switches. The RF MEMS switches are currently under study at the Purdue University center for the Prediction of Reliability, Integrity, and Survivability of Microsystems (PRISM). An array of microstructural characterization techniques including focused ion beam (FIB) microscopy, scanning electron microscopy (SEM), X-ray diffraction (XRD), and transmission electron microscopy have be used to study the nickel film and to quantify grain size and crystallographic texture and provide information about elemental impurities and surface roughness and impurity elements. Particular emphasis has been placed on quantifying the crystallographic fiber texture of the polycrystalline nickel film as a function of film height within a single specimen using a new transmission electron microscopy (TEM) microtexture method. The TEM method employs a special type of plan view TEM sample and uses hollow cone dark field (HCDF) TEM imaging to spatially map the orientation of individual crystallites at discrete film heights. A trend of increasing 001 fiber texture with film height was discovered, which has implications for the elastic behavior of the MEMS device. The method can be applied to study fiber texture evolution as a function of height in polycrystalline films to gather data that may elucidate fundamental film growth mechanisms. The method is explained in detail. It is well-known that the elastic properties of polycrystalline thin films used in MEMS devices can deviate from bulk isotropic values and become directionally-dependent if a crystallographic texture is present. Hence, the ability to predict the actual anisotropic elastic properties of textured films is important for MEMS design and

  6. Propagation of TEM- and PSE-Type β-Lactamases among Amoxicillin-Resistant Salmonella spp. Isolated in France

    PubMed Central

    Llanes, Catherine; Kirchgesner, Veronique; Plesiat, Patrick

    1999-01-01

    A survey conducted between 1987 and 1994 at the University Hospital of Besançon, France, demonstrated a dramatic increase (from 0 to 42.5%) in the prevalence of amoxicillin resistance among Salmonella spp. Of the 96 resistant isolates collected during this period (including 77 Typhimurium), 54 were found to produce TEM-1 β-lactamase, 40 produced PSE-1 (equivalent to CARB-2), one produced PSE-1 plus TEM-2, and one produced OXA-1 in isoelectric focusing and DNA hybridization experiments. Plasmids coding for these β-lactamases were further characterized by (i) profile analysis, (ii) restriction fragmentation pattern analysis, (iii) hybridization with an spvCD-orfE virulence probe, and (iv) replicon typing. In addition, isolates of S. typhimurium were genotypically compared by pulsed-field gel electrophoresis of XbaI-macrorestricted chromosomal DNA. Altogether, these methods showed that 40 of the 41 PSE-1 producers were actually the progeny of a single epidemic S. typhimurium strain lysotype DT104. Isolates of that strain were found to harbor RepFIC virulence plasmids with somewhat different restriction profiles, but which all carried the blaPSE-1 gene. Of these virulence/resistance plasmids, 15 were transmissible to Escherichia coli. TEM-1-producing S. typhimurium displayed much greater genotypic and plasmidic diversities, suggesting the acquisition of the blaTEM-1 gene from multiple bacterial sources by individual strains. In agreement with this, 32 of the 35 S. typhimurium plasmids encoding TEM-1 were found to be conjugative. These data show that development of amoxicillin resistance among Salmonella, especially in serovar Typhimurium, results from both gene transfers and strain dissemination. PMID:10508020

  7. Quantification of Electrochemical Nanoscale Processes in Lithium Batteries By OperandoEC-(S)TEM

    SciTech Connect

    Mehdi, Beata L.; Qian, Jiangfeng; Nasybulin, Eduard; Welch, David A.; Park, Chiwoo; Faller, Roland; Mehta, Hardeep S.; Henderson, Wesley A.; Xu, Wu; Evans, James E.; Liu, Jun; Zhang, Jiguang; Mueller, Karl T.; Browning, Nigel D.

    2015-07-27

    Lithium (Li)-ion batteries are currently used for a wide variety of portable electronic devices, electric vehicles and renewable energy applications. In addition, extensive worldwide research efforts are now being devoted to more advanced “beyond Li-ion” battery chemistries - such as lithium-sulfur (Li-S) and lithium-air (Li-O2) - in which the carbon anode is replaced with Li metal. However, the practical application of Li metal anode systems has been highly problematic. The main challenges involve controlling the formation of a solid-electrolyte interphase (SEI) layer and the suppression of Li dendrite growth during the charge/discharge process (achieving “dendrite-free” cycling). The SEI layer formation continuously consumes the electrolyte components creating highly resistive layer, which leads to the rapid decrease of cycling performance and degradation of the Li anode. The growth of Li metal dendrites at the anode contributes to rapid capacity fading (the presence of “dead Li” created during the discharge leads to an increased overpotential) and, in the case of continuous growth, leads to internal short circuits and extreme safety issues. Here we demonstrate the application of an operando electrochemical scanning transmission electron microscopy (ec-(S)TEM) cell to study the SEI layer formation and the initial stages of Li dendrite growth - the goal is to develop a mechanism for mitigating the degradation processes and increasing safety. Bright field (BF) STEM images in Figure 1 A-C show Li metal deposition and dissolution processes at the interface between the Pt working electrode and the lithium hexafluorophosphate (LiPF6) in propylene carbonate (PC) electrolyte during three charge/discharge cycles. A contrast reversal caused by Li metal being lighter/less dense than surrounding electrolyte (Li appears brighter than the background in BF STEM images) allows Li to be uniquely identified from the other components in the system - the only solid

  8. Use of an Ultrasonic/Sonic Driller/Corer to Obtain Sample Powder for CHEMIN, a Combined XRD/XRF Instrument

    NASA Technical Reports Server (NTRS)

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

    2003-01-01

    A miniature CHEMIN XRD/XRF (X-Ray Diffraction/X-Ray Fluourescence) instrument is currently being developed for definitive mineralogic analysis of soils and rocks on Mars. One of the technical issues that must be addressed in order to enable XRD analysis on an extraterrestrial body is how best to obtain a representative sample powder for analysis. For XRD powder diffraction 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 2-dimensional detector as used in the CHEMIN instrument will produce good results with poorly prepared powders, the quality of the data will improve if the sample is fine-grained and randomly oriented. An Ultrasonic/Sonic Driller/Corer (USDC) currently being developed at JPL is an effective mechanism of sampling rock to produce cores and powdered cuttings. It requires low axial load (< 5N) and thus offers significant advantages for operation from lightweight platforms and in low gravity environments. The USDC is lightweight (<0.5kg), and can be driven at low power (<5W) using duty cycling. It consists of an actuator with a piezoelectric stack, ultrasonic horn, free-mass, and drill bit. The stack is driven with a 20 kHz AC voltage at resonance. The strain generated by the piezoelectric is amplified by the horn by a factor of up to 10 times the displacement amplitude. The tip impacts the free-mass and drives it into the drill bit in a hammering action. The free-mass rebounds to interact with the horn tip leading to a cyclic rebound at frequencies in the range of 60-1000 Hz. It does not require lubricants, drilling fluid or bit sharpening and it has the potential to operate at high and low temperatures using a suitable choice of piezoelectric material. To assess whether the powder from an ultrasonic drill would be adequate for analyses by an XRD/XRF spectrometer such as CHEMIN, powders obtained from the JPL

  9. Study of the relation between Mg content and dissolution kinetics of natural lime stone using μXRF, μXRD and μXAS

    NASA Astrophysics Data System (ADS)

    Grunwaldt, H. S.; Zimina, A.; Göttlicher, J.; Steininger, R.; Grunwaldt, J.-D.

    2016-05-01

    The dissolution parameters of calcium carbonates play a key role in agriculture as they regulate the plant nutrients uptake and buffer the pH-value of the soil. The combination of μXRF, μXAS and μXRD mapping in the hard X-ray regime for the examination of both short- and long range order in natural limestones revealed that their dissolution properties depend both on the crystallinity of the mineral phases and their composition. The results particularly show that in many cases the presence of magnesium inhibits dissolution of the phases.

  10. Novel extended-spectrum TEM-type beta-lactamase from an Escherichia coli isolate resistant to ceftazidime and susceptible to cephalothin.

    PubMed Central

    Chanal-Claris, C; Sirot, D; Bret, L; Chatron, P; Labia, R; Sirot, J

    1997-01-01

    A novel extended-spectrum TEM-type beta-lactamase was detected in an Escherichia coli isolate which was resistant to ceftazidime and susceptible to cephalothin. The corresponding bla gene was sequenced. The deduced amino acid sequence showed the following three amino acid replacements with respect to the TEM-2 sequence: Glu-->Lys-104, Arg-->Ser-164, and Glu-->Lys-240. Since it confers a ceftazidimase-type resistance phenotype, we propose for this novel enzyme the designation CAZ-9, corresponding to TEM-46 in the sequential numbering scheme of TEM beta-lactamases. PMID:9056022

  11. Fibre-coupled red diode-pumped Alexandrite TEM00 laser with single and double-pass end-pumping

    NASA Astrophysics Data System (ADS)

    Arbabzadah, E. A.; Damzen, M. J.

    2016-06-01

    We report the investigation of an Alexandrite laser end-pumped by a fibre-coupled red diode laser module. Power, efficiency, spatial, spectral, and wavelength tuning performance are studied as a function of pump and laser cavity parameters. It is the first demonstration, to our knowledge, of greater than 1 W power and also highest laser slope efficiency (44.2%) in a diode-pumped Alexandrite laser with diffraction-limited TEM00 mode operation. Spatial quality was excellent with beam propagation parameter M 2 ~ 1.05. Wavelength tuning from 737–796 nm was demonstrated using an intracavity birefringent tuning filter. Using a novel double pass end-pumping scheme to get efficient absorption of both polarisation states of the scrambled fibre-delivered diode pump, a total output coupled power of 1.66 W is produced in TEM00 mode with 40% slope efficiency.

  12. Microstructural characterization of Ti-6Al-4V metal chips by focused ion beam (FIB) and transmission electron microscopy (TEM)

    SciTech Connect

    Schneider, Judy; Dong, Lei; Howe, Jane Y; Meyer III, Harry M

    2011-01-01

    The microstructure of the secondary deformation zone (SDZ) near the cutting surface in metal chips of Ti-6Al-4V formed during machining was investigated using focused ion beam (FIB) specimen preparation and transmission electron microscopy (TEM) imaging. Use of the FIB allowed precise extraction of the specimen across this region to reveal its inhomogeneous microstructure resulting from the non-uniform distribution of strain, strain rate, and temperature generated during the cutting process. Initial imaging from conventional TEM foil preparation revealed microstructures ranging from heavily textured to regions of fine grains. Using FIB preparation, the transverse microstructure could be interpreted as fine grains near the cutting surface which transitioned to coarse grains toward the free surface. At the cutting surface a 10 nm thick recrystallized layer was observed capping a 20 nm thick amorphous layer.

  13. In-situ TEM crystallization of anorthite-glass films on {alpha}-Al{sub 2}O{sub 3}

    SciTech Connect

    Mallamaci, M.P.; Carter, C.B.; Bentley, J.

    1993-12-31

    Anorthite-glass films have been grown by pulsed-laser deposition on single-crystal {alpha}-Al{sub 2}O{sub 3} substrates which were pre-thinned to electron transparency. The glass films were crystallized in the transmission electron microscope (TEM), which allowed direct observation and video-recording of the crystallization process. Crystallization of these films in the TEM resulted in the formation of hexagonal and orthorhombic anorthite. The orthorhombic phase was the predominant product of glass films grown at elevated substrate temperatures and displayed strong epitaxy with the underlying substrate. In contrast, the hexagonal phase was the major constituent of films grown at ambient substrate temperature and displayed no clear epitaxy with the substrate. The difference in degree of epitaxy and phase structure may be evidence of ordering at the original glass/oxide interface.

  14. Insights into the growth of bismuth nanoparticles on 2D structured BiOCl photocatalysts: an in situ TEM investigation.

    PubMed

    Chang, Xiaofeng; Wang, Shuangbao; Qi, Qi; Gondal, Mohammed A; Rashid, Siddique G; Gao, Si; Yang, Deyuan; Shen, Kai; Xu, Qingyu; Wang, Peng

    2015-09-28

    The synthetic techniques for novel photocatalytic crystals had evolved by a trial-and-error process that spanned more than two decades, and an insight into the photocatalytic crystal growth process is a challenging area and prerequisite for achieving an excellent photoactivity. Bismuth nanoparticle based hybrids, such as Bi/BiOCl composites, have recently been investigated as highly efficient photocatalytic systems because of the localized surface plasmon resonance (LSPR) of nanostructured bismuth. In this work, the observation towards the formation and growth of bismuth nanoparticles onto 2D structured BiOCl photocatalysts has been performed using a transmission electron microscope (TEM) directly in real time. The growth of bismuth nanoparticles on BiOCl nanosheets can be emulated and speeded up driven by the electron beam (e(-) beam) in TEM. The crystallinity, growth and the elemental evolution during the formation of bismuth nanoparticles have also been probed in this work.

  15. Resonant optical transmission through sub-wavelength annular apertures caused by a plasmonic transverse electromagnetic (TEM) mode

    NASA Astrophysics Data System (ADS)

    Ndao, A.; Salvi, J.; Salut, R.; Bernal, M.-P.; Alaridhee, T.; Belkhir, A.; Baida, F. I.

    2014-12-01

    We demonstrate enhanced transmission through annular aperture arrays (AAA) by the excitation of the transverse electromagnetic (TEM) guided mode. A complete numerical study is performed to correctly design the structure before it is experimentally characterized. Actually, the challenge was to get efficient TEM-based transmission in the visible range. It turned out to be a hard task because of the strong absorption associated with this guided mode. Nevertheless, we have succeeded to experimentally prove its excitation thanks to the enhanced transmission measured in the far-field. This is the first time we demonstrate experimental evidence of this phenomenon with such AAA structure illuminated at oblique incidence in the visible range. This increases the potential applications of such structures as well, single molecule spectroscopy, photovoltaic, spectral filtering, optical trapping, etc...

  16. Efficient single-mode (TEM{sub 00}) Nd : YVO{sub 4} laser with longitudinal 808-nm diode pumping

    SciTech Connect

    Donin, V I; Yakovin, D V; Yakovin, M D

    2013-10-31

    A single-mode Nd : YVO{sub 4} laser with unidirectional longitudinal pumping by laser diodes with λ = 808 nm and a power of 40 W is studied. In the TEM{sub 00} mode, the output laser power is 24 W with the optical efficiency η{sub opt} = 57.1 % (slope efficiency 63.3 %), which, as far as we know, is the best result for Nd{sup 3+} : YVO{sub 4} lasers with longitudinal pumping at λ = 808 nm from one face of the active crystal. Estimates of thermal effects show that, using a Nd : YVO{sub 4} crystal (length 20 mm, diameter 3 mm, dopant concentration 0.27 at%) with two undoped ends and bidirectional diode pumping with a total power of 170 W, one can obtain an output power of ∼100 W in the TEM{sub 00} mode from one active element. (lasers)

  17. Fibre-coupled red diode-pumped Alexandrite TEM00 laser with single and double-pass end-pumping

    NASA Astrophysics Data System (ADS)

    Arbabzadah, E. A.; Damzen, M. J.

    2016-06-01

    We report the investigation of an Alexandrite laser end-pumped by a fibre-coupled red diode laser module. Power, efficiency, spatial, spectral, and wavelength tuning performance are studied as a function of pump and laser cavity parameters. It is the first demonstration, to our knowledge, of greater than 1 W power and also highest laser slope efficiency (44.2%) in a diode-pumped Alexandrite laser with diffraction-limited TEM00 mode operation. Spatial quality was excellent with beam propagation parameter M 2 ~ 1.05. Wavelength tuning from 737-796 nm was demonstrated using an intracavity birefringent tuning filter. Using a novel double pass end-pumping scheme to get efficient absorption of both polarisation states of the scrambled fibre-delivered diode pump, a total output coupled power of 1.66 W is produced in TEM00 mode with 40% slope efficiency.

  18. TEM, HRTEM, electron holography and electron tomography studies of gamma' and gamma'' nanoparticles in Inconel 718 superalloy.

    PubMed

    Dubiel, B; Kruk, A; Stepniowska, E; Cempura, G; Geiger, D; Formanek, P; Hernandez, J; Midgley, P; Czyrska-Filemonowicz, A

    2009-11-01

    The aim of the study was the identification of gamma' and gamma'' strengthening precipitates in a commercial nickel-base superalloy Inconel 718 (Ni-19Fe-18Cr-5Nb-3Mo-1Ti-0.5Al-0.04C, wt %) using TEM dark-field, HRTEM, electron holography and electron tomography imaging. To identify gamma' and gamma'' nanoparticles unambiguously, a systematic analysis of experimental and theoretical diffraction patterns were performed. Using HRTEM method it was possible to analyse small areas of precipitates appearance. Electron holography and electron tomography techniques show new possibilities of visualization of gamma' and gamma'' nanoparticles. The analysis by means of different complementary TEM methods showed that gamma'' particles exhibit a shape of thin plates, while gamma' phase precipitates are almost spherical. PMID:19903242

  19. In Vivo Inflammatory Effects of Ceria Nanoparticles on CD-1 Mouse: Evaluation by Hematological, Histological, and TEM Analysis

    PubMed Central

    Poma, Anna; Ragnelli, Anna Maria; de Lapuente, Joaquin; Ramos, David; Borras, Miquel; Di Gioacchino, Mario; Santucci, Sandro; De Marzi, Laura

    2014-01-01

    The attention on CeO2-NPs environmental and in vivo effects is due to their presence in diesel exhaust and in diesel filters that release a more water-soluble form of ceria NPs, as well as to their use for medical applications. In this work, acute and subacute in vivo toxicity assays demonstrate no lethal effect of these NPs. Anyhow, performing in vivo evaluations on CD-1 mouse systems, we demonstrate that it is even not correct to assert that ceria NPs are harmless for living systems as they can induce status of inflammation, revealed by hematological-chemical-clinical assays as well as histological and TEM microscope observations. TEM analysis showed the presence of NPs in alveolar macrophages. Histological evaluation demonstrated the NPs presence in lungs tissues and this can be explained by assuming their ability to go into the blood stream and lately into the organs (generating inflammation). PMID:25032226

  20. Ion-beam implantation and cross-sectional TEM characterization of Gd 2Ti 2O 7 pyrochlore

    NASA Astrophysics Data System (ADS)

    Lian, Jie; Wang, L. M.; Ewing, R. C.; Boatner, L. A.

    2006-01-01

    Radiation effects in a wide range of pyrochlore compositions have been extensively investigated due to the potential application of pyrochlores as host matrices for the immobilization of actinides - particularly Pu. In this study, we have performed 1.0 MeV Kr2+ ion implantations in bulk samples of single crystal Gd2Ti2O7 at room temperature at different ion fluences of 1.875, 3.125 and 5 × 1014 ions/cm2. The microstructural evolution upon ion-beam implantation was examined by cross-sectional transmission electron microscopy (TEM). The critical amorphization dose at room temperature for 1 MeV Kr2+ implanted Gd2Ti2O7 was determined to be ∼0.143 dpa, which is significantly lower than the dose obtained by ion-irradiation under in situ TEM observation.

  1. Recent Advances in Electron Tomography: TEM and HAADF-STEM Tomography for Materials Science and IC Applications

    SciTech Connect

    Kubel, C; Voigt, A; Schoenmakers, R; Otten, M; Su, D; Lee, T; Carlsson, A; Engelmann, H; Bradley, J

    2005-11-09

    Electron tomograph tomography is a well y well-established technique for three-dimensional structure determination of (almost) amorphous specimens in life science applications. With the recent advances in nanotechnology and the semiconductor industry, there is also an increasing need for high-resolution 3D structural information in physical sciences. In this paper, we evaluate the capabilities and limitations of TEM and HAADF-STEM tomography for the 3D structural characterization of partially crystalline to highly crystalline materials. Our analysis of catalysts, a hydrogen storage material, and different semiconductor devices shows that features with a diameter as small as 1-2 nm can be resolved in 3D by electron tomography. For partially crystalline materials with small single crystalline domains, TEM tomography provides reliable 3D structural information. HAADF-STEM tomography is more versatile and can also be used for high-resolution 3D imaging of highly crystalline materials such as semiconductor devices.

  2. Characterization of laser-fired contacts in PERC solar cells: SIMS and TEM analysis applying advanced preparation techniques

    NASA Astrophysics Data System (ADS)

    Zastrow, U.; Houben, L.; Meertens, D.; Grohe, A.; Brammer, T.; Schneiderlöchner, E.

    2006-07-01

    In this study we apply ion-beam supported preparation techniques for both mesa formation by trench sputtering and FIB 'lift-out' lamella cutting for dynamic SIMS and TEM analysis of laser-fired Al point contacts on Si, respectively. Detailed compositional and structural informations about the metallurgical contact formation process are obtained combining both characterization techniques. While TEM micrographs and microdiffraction patterns reveal a mixture of Al- and Si-crystals within the ˜1 μm thick Al rich re-solidified surface layer according to the Al-Si phase diagram, spatially resolved SIMS depth profiling indicates ppm-range Al-diffusion a few hundred nm into the buried, substantially undisturbed Si-lattice.

  3. TEM Characterization of a Titanium Nitride (TiN) Inclusion in a Fe-Ni-Co Maraging Steel

    NASA Astrophysics Data System (ADS)

    Descotes, Vincent; Migot, Sylvie; Robaut, Florence; Bellot, Jean-Pierre; Perrin-Guérin, Valérie; Witzke, Sylvain; Jardy, Alain

    2015-07-01

    A TEM observation of a TiN inclusion associated to a spinel (MgAl2O4) and calcium sulfide germs is reported. It shows an orientation relationship between these three phases, indicating an epitaxial growth of the TiN over the spinel and CaS. This observation strengthens the hypothesis of a heterogeneous nucleation of TiN particles during the solidification of a maraging steel.

  4. Quantitative TEM-based phase retrieval of MgO nano-cubes using the transport of intensity equation.

    PubMed

    Petersen, Tim C; Keast, Vicki J; Paganin, David M

    2008-08-01

    Through focus series of images are collected from MgO nano-cube crystals in the transmission electron microscope (TEM). The experimental data is used to solve the transport of intensity equation (TIE) to retrieve phase maps, which portray the morphology of the cubes and are quantified by the mean inner potential V(0). Particular attention is given to the practical difficulties associated with TIE phase retrieval of non-conducting polyhedron particles.

  5. Efficient TEM(00)-mode operation of a laser-diode side-pumped Nd:YAG laser

    NASA Technical Reports Server (NTRS)

    Welford, D.; Rines, D. M.; Dinerman, B. J.

    1991-01-01

    The operation of a laser-diode side-pumped Nd:YAG laser with a novel pumping geometry that ensures efficient conversion of pump energy into the TEM(00) mode is reported. Of the 1064-nm output, 11.8 microJ of energy was obtained in a 200-microsec pulse with 64 microJ of pump energy at 808 nm. The overall conversion and slope efficiencies were 18 and 23 percent, respectively.

  6. Using ground-based geophysics to constrain the interpretation of airborne TEM data recorded across the Okavango Delta, Botswana

    NASA Astrophysics Data System (ADS)

    Podgorski, J. E.; Kalscheuer, T.; Doetsch, J.; Rabenstein, L.; Tshoso, G.; Meier, P.; Horstmeyer, H.; Kgotlhang, L.; Ploug, C.; Auken, E.; Kinzelbach, W. K.; Green, A. G.

    2011-12-01

    The Okavango Delta in northern Botswana is a near endorheic inland delta that has developed over the past ~2 MA in an active graben at the southwestern end of the East Africa Rift System. An annual flood from the north causes a slowly flowing surface water regime in the delta, but previous wetter climatic periods were responsible for intermittent lacustrine environments. The Okavango Delta is the largest permanent water body in the Kalahari Desert and, as such, represents an important resource for wildlife and humans alike. An airborne time-domain electromagnetic (TEM) survey, commissioned by the Botswana government, was undertaken in 2007 for the purpose of better understanding the hydrogeology of the delta. Initial processing and inversion of these data show within the main fan of the delta a resistive 20-50 m thick surface layer underlain by a 30-200 m thick conductive layer. In the upper fan, the conductive layer is underlain by a resistive unit beginning at about 150 m depth. This unit exhibits a dendritic pattern implying a fluvial origin. To help interpret this and other structures, geophysical field work was initiated in early 2011 at various locations in the delta. Seismic reflection and refraction, electrical resistive tomography (ERT), and ground TEM methods were employed. The seismic methods are useful for delineating the boundaries of the weathering and basement layers, whereas ERT provides an independent estimate of the resistivity structure, particularly at shallow depths. Ground TEM allows for a direct comparison with the airborne TEM soundings, helping to estimate the accuracy of the latter. Though still evolving, the current large-scale hydrogeological interpretation of the airborne data set includes a fresh water-saturated surface layer underlain by a saline aquifer and clay aquitard. In the upper fan of the delta, a fresh water aquifer appears to lie between the aquitard and the basement rock.

  7. Structural characterizaiton and gas reactions of small metal particles by high-resolution, in-situ TEM and TED

    NASA Technical Reports Server (NTRS)

    1984-01-01

    The existing in-situ transmission electron microscopy (TEM) facility was improved by adding a separately pumped mini-specimen chamber. The chamber contains wire-evaporation sources for three metals and a specimen heater for moderate substrate temperatures. A sample introduction device was constructed, installed, and tested, facilitating rapid introduction of a specimen into the mini-chamber while maintaining the background pressure in that chamber in the 10(-9) millibar range. Small particles and clusters of Pd, grown by deposition from the vapor phase in an in-situ TEM facility on amorphous and crystalline support films of alumina and on ultra-thin carbon films, were analyzed by conventional high-resolution TEM and image analysis in terms of detectability, number density, and size distribution. The smallest particles that could be detected and counted contained no more than 6 atoms; size determinations could be made for particles 1 nm in diameter. The influence of various oxygen plasma treatments, annealing treatments, and of increasing the substrate temperature during deposition was investigated. The TEM technique was employed to demonstrate that under otherwise identica l conditions the lattice parameter of Pd particles in the 1 to 2 nm size range and supported in random orientation on ex-situ prepared mica films is expanded by some 3% when compared to 5 nm size particles. It is believed that this expansion is neither a small-particle diffraction effect nor due to pseudomorphism, but that it is due to a annealing-induced transformation of the small as-deposited particles with predominantly composite crystal structures into larger particles with true f.c.c. structure and thus inherently smaller lattice parameter.

  8. Inactivation of TEM-1 by avibactam (NXL-104): insights from quantum mechanics/molecular mechanics metadynamics simulations.

    PubMed

    Sgrignani, Jacopo; Grazioso, Giovanni; De Amici, Marco; Colombo, Giorgio

    2014-08-12

    The fast and constant development of drug-resistant bacteria represents a serious medical emergence. To overcome this problem, the development of drugs with new structures and modes of action is urgently needed. In this context, avibactam represents a promising, innovative inhibitor of beta-lactamases with a novel molecular structure compared to previously developed inhibitors, showing a promising inhibitory activity toward a significant number of beta-lactamase enzymes. In this work, we studied, at the atomistic level, the mechanisms of formation of the covalent complex between avibactam and TEM-1, an experimentally well-characterized class A beta-lactamase, using classical and quantum mechanics/molecular mechanics (QM/MM) simulations combined with metadynamics. Our simulations provide a detailed structural and energetic picture of the molecular steps leading to the formation of the avibactam/TEM-1 covalent adduct. In particular, they support a mechanism in which the rate-determining step is the water-assisted Glu166 deprotonation by Ser70. In this mechanistic framework, the predicted activation energy is in good agreement with experimental kinetic measurements. Additionally, our simulations highlight the important role of Lys73 in assisting the Ser70 and Ser130 deprotonations. While based on the specific case of the avibactam/TEM-1, the simple protocol we present here can be immediately extended and applied to the study of covalent complex formation in different enzyme-inhibitor pairs.

  9. Transrotational Micro-, Nanocrystals Revealed by TEM: New Solid State Order or Novel Extended Imperfection in Crystallizing Amorphous Films

    NASA Astrophysics Data System (ADS)

    Kolosov, Vladimir Yu.

    2012-02-01

    Unexpected transrotational structure [1] has been revealed by transmission electron microscopy (TEM) for crystal growth in thin (10-100nm) amorphous films of different chemical nature (oxides, chalcogenides, metals and alloys) prepared by various methods. Primarily we use our TEM bend contour technique but also HREM, EDX, CBED and AFM are used in due cases. The unusual phenomenon can be traced in situ in TEM column: strong dislocation independent regular internal bending of crystal lattice planes in a growing crystal. Such transrotation (unit cell translation is complicated by small rotation realized round an axis lying in the film plane) can result in strong regular lattice orientation gradients (up to 300^o/μm) of different geometries: cylindrical, ellipsoidal, toroidal, etc. Transrotational crystal corresponds to ideal single crystal enclosed in a curved space. It can be considered also as hypothetical endless 2.5 D analogy of MW nanotube/nano-onion halves. Transrotation is strongly increasing as the film gets thinner. Transrotations supplement dislocations (in crystals) and disclinations (in liquid crystals). Transrotational order can be regarded as intermediate one between amorphous and crystalline. [1] V. Yu. Kolosov and A. R.Tholen, Acta Mater., 48 (2000) 1829.

  10. Duplex Oxide Formation during Transient Oxidation of Cu-5%Ni(001) Investigated by In situ UHV-TEM and XPS

    SciTech Connect

    Yang, J.C.; Starr, D.; Kang, Y.; Luo, L.; Tong, X.; Zhou, G.

    2012-05-20

    The transient oxidation stage of a model metal alloy thin film was characterized with in situ ultra-high vacuum (UHV) transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS) and analytic high-resolution TEM. We observed the formations of nanosized NiO and Cu{sub 2}O islands when Cu-5a5%Ni(100) was exposed to oxygen partial pressure, pO{sub 2} = 1 x 10{sup -4} Torr and various temperatures in situ. At 350 C epitaxial Cu{sub 2}O islands formed initially and then NiO islands appeared on the surface of the Cu{sub 2}O island, whereas at 750 C NiO appeared first. XPS and TEM was used to reveal a sequential formation of NiO and then Cu{sub 2}O islands at 550 C. The temperature-dependant oxide selection may be due to an increase of the diffusivity of Ni in Cu with increasing temperature.

  11. Investigation of a catalyst ink dispersion using both ultra-small-angle X-ray scattering and cryogenic TEM.

    PubMed

    Xu, Fan; Zhang, HangYu; Ilavsky, Jan; Stanciu, Lia; Ho, Derek; Justice, Matthew J; Petrache, Horia I; Xie, Jian

    2010-12-21

    The dispersion of Nafion ionomer particles and Pt/C catalyst aggregates in liquid media was studied using both ultra-small-angle X-ray scattering (USAXS) and cryogenic TEM. A systematic approach was taken to study first the dispersion of each component (i.e., ionomer particles and Pt/C aggregates), then the combination of the components, and last the catalyst ink. Multiple-level curve fitting was used to extract the particle size, size distribution, and geometry of the Pt/C aggregates and the Nafion particles in liquid media from the scattering data. The results suggest that the particle size, size distribution, and geometry are not uniform throughout the systems but rather vary significantly. It was found that the interaction of each component (i.e., the Nafion ionomer particles and the Pt/C aggregates) occurs in the dispersion. Cryogenic TEM was used to observe the size and geometry of the particles in liquid directly and to validate the scattering results. The TEM results showed excellent agreement.

  12. TEM microstructural characterization of melt-spun aged Al-6Si-3Cu-xMg alloys

    SciTech Connect

    Lopez, Ismeli Alfonso . E-mail: post18@jupiter.umich.mx; Zepeda, Cuauhtemoc Maldonado; Gonzalez Reyes, Jose Gonzalo; Flores, Ariosto Medina; Rodriguez, Juan Serrato; Gomez, Luis Bejar

    2007-06-15

    Three Al-6Si-3Cu-xMg alloys (x = 0.59, 3.80 and 6.78 wt.%) were produced using melt-spinning. As-melt-spun ribbons were aged at 150, 180 and 210 deg. C for times between 0.05 and 100 h. Microstructural changes were examined using transmission electron microscopy (TEM) and microhardness was measured. TEM analysis of the as-melt-spun alloys revealed 5 nm nanoparticles and larger particles (50 nm) composed of Al{sub 2}Cu ({theta}) for the 0.59% Mg alloy and Al{sub 5}Cu{sub 2}Mg{sub 8}Si{sub 6} (Q) for 3.80% and 6.78% Mg alloys. Silicon solid solubility was extended to 9.0 at.% and Mg in solid solution reached 6.7 at.%. After aging treatments the 6.78% Mg alloy exhibited the most significant increase in microhardness, reaching 260 kg/mm{sup 2}. TEM analysis of aged specimens also showed {theta} and Q phase (5-20 nm nanoparticles and 35-40 nm particles). The combination of the volume fraction and size of the particles plays an important role in microhardness variation.

  13. Validation studies of gyrokinetic ITG and TEM turbulence simulations in a JT-60U tokamak using multiple flux matching

    NASA Astrophysics Data System (ADS)

    Nakata, Motoki; Honda, Mitsuru; Yoshida, Maiko; Urano, Hajime; Nunami, Masanori; Maeyama, Shinya; Watanabe, Tomo-Hiko; Sugama, Hideo

    2016-08-01

    Quantitative validation studies of flux-tube gyrokinetic Vlasov simulations on ion and electron heat transport are carried out for the JT-60U tokamak experiment. The ion temperature gradient (ITG) and/or trapped electron modes (TEM) driven turbulent transport and zonal flow generations are investigated for an L-mode plasma in the local turbulence limit with a sufficiently small normalized ion thermal gyroradius and weak mean radial electric fields. Nonlinear turbulence simulations by the GKV code successfully reproduce radial profiles of the ion and electron energy fluxes in the core region. The numerical results show that the TEM-driven zonal flow generation in the outer region is more significant than that in the core region with ITG- and ITG–TEM-dominated turbulence, leading to moderate transport shortfall of the ion energy flux. Error levels in the prediction of the ion and electron temperature gradient profiles in the core region are estimated as less than +/- 30% , based on a multiple flux matching technique, where the simulated ion and electron energy fluxes are simultaneously matched to the experimental values.

  14. High-field actively detuneable transverse electromagnetic (TEM) coil with low-bias voltage for high-power RF transmission.

    PubMed

    Avdievich, Nikolai I; Bradshaw, Ken; Kuznetsov, Andrey M; Hetherington, Hoby P

    2007-06-01

    The design and construction of a 4T (170 MHz) transverse electromagnetic (TEM) actively detuneable quadrature head coil is described. Conventional schemes for active detuning require high negative bias voltages (>300 V) to prevent leakage of RF pulses with amplitudes of 1-2 kW. To extend the power handling capacity and avoid the use of high DC bias voltages, we developed an alternate method of detuning the volume coil. In this method the PIN diodes in the detuning circuits are shorted when the RF volume coil is tuned, and negatively biased with -12 V when the coil is detuned. To preserve the high Q(U)/Q(L) ratio of the TEM coil, we modified the method of Nabetani and Watkins (Proceedings of the 13th Annual Meeting of ISMRM, Kyoto, Japan, 2004, abstract 1574) by utilizing a high-impedance (approximately 200 Omega), lumped-element, quarter-wavelength transformer. A Q(U) of 500 was achieved for the detuneable TEM, such that incorporation of the detuning network had minimal effect (<1 dB) on the performance of the coil in vivo. PMID:17534919

  15. Direct correlation of structural and electrical properties of electron-doped individual VO2 nanowires on devised TEM grids

    NASA Astrophysics Data System (ADS)

    Jo, Y.-R.; Kim, M.-W.; Kim, B.-J.

    2016-10-01

    Nano-scale VO2 wires with controlled parameters such as electron-doping have attracted intense interest due to their capability of suppressing the temperature of the metal-insulator transition (MIT). However, because their diameters are smaller than the spatial resolutions of the conventional measuring equipment, the ability to perform a thorough examination of the wires has been hindered. Here, we report the fabrication of a transmission electron microscopy (TEM) grid with an optimum design of Si3N4 windows on which the photolithography for individual electron-doped VO2 nanowire devices can be safely accomplished, allowing the cross-examination of the structural and electrical properties. TEM dark-field imaging was used to quantitatively investigate the fractions of rutile and M1 phases, and their lattice alignments were observed using high-resolution TEM (HRTEM) with small area diffraction. Moreover, electron energy loss spectroscopy (EELS) revealed that the rutile domain would be created by the strain induced by oxygen vacancies. Importantly, we successfully tuned the transition temperature by changing the rutile fraction while maintaining a high level of resistivity change. The resistivity at room temperature linearly decreased with the rutile fraction, following a simple model. Furthermore, the T dependence of the threshold voltage can be attributed to the Joule heating, exhibiting an identical thermal dependence, irrespective of the rutile fraction.

  16. In situ targeting TEM8 via immune response and polypeptide recognition by wavelength-modulated surface plasmon resonance biosensor.

    PubMed

    Wang, Yimin; Luo, Zewei; Liu, Kunping; Wang, Jie; Duan, Yixiang

    2016-01-01

    There is an increasing interest in real-time and in situ monitoring of living cell activities in life science and medicine. This paper reports a whole cell sensing protocol over the interface of Au film coupled in a wavelength-modulated surface plasmon resonance (WMSPR) biosensor. With dual parabolic mirrors integrated in the sensor, the compact and miniaturized instrument shows satisfactory refractive index sensitivity (2220 nm/RIU) and a high resolution of resonance wavelength shift of 0.3 nm to liquid samples. The affinity interactions between the biomarker of human tumor endothelial marker 8 (TEM8) and antibody (Ab) or specific polypeptide (PEP) were firstly introduced to WMSPR biosensor analysis. Both the interaction events of Ab-cell and PEP-cell over the Au film interface can be recognized by the sensor and the balance time of interactions is about 20 min. The concentration range of Ab for quantitative monitoring of the TEM8 expression on human colon carcinoma SW620 cells was investigated. The present low-cost and time-saving method provides a time resolution of binding specificity between Ab/PEP and TEM8 for real-time analysis of antigen on living tumor cell surface. PMID:26822761

  17. Validation studies of gyrokinetic ITG and TEM turbulence simulations in a JT-60U tokamak using multiple flux matching

    NASA Astrophysics Data System (ADS)

    Nakata, Motoki; Honda, Mitsuru; Yoshida, Maiko; Urano, Hajime; Nunami, Masanori; Maeyama, Shinya; Watanabe, Tomo-Hiko; Sugama, Hideo

    2016-08-01

    Quantitative validation studies of flux-tube gyrokinetic Vlasov simulations on ion and electron heat transport are carried out for the JT-60U tokamak experiment. The ion temperature gradient (ITG) and/or trapped electron modes (TEM) driven turbulent transport and zonal flow generations are investigated for an L-mode plasma in the local turbulence limit with a sufficiently small normalized ion thermal gyroradius and weak mean radial electric fields. Nonlinear turbulence simulations by the GKV code successfully reproduce radial profiles of the ion and electron energy fluxes in the core region. The numerical results show that the TEM-driven zonal flow generation in the outer region is more significant than that in the core region with ITG- and ITG-TEM-dominated turbulence, leading to moderate transport shortfall of the ion energy flux. Error levels in the prediction of the ion and electron temperature gradient profiles in the core region are estimated as less than +/- 30% , based on a multiple flux matching technique, where the simulated ion and electron energy fluxes are simultaneously matched to the experimental values.

  18. In situ targeting TEM8 via immune response and polypeptide recognition by wavelength-modulated surface plasmon resonance biosensor

    PubMed Central

    Wang, Yimin; Luo, Zewei; Liu, Kunping; Wang, Jie; Duan, Yixiang

    2016-01-01

    There is an increasing interest in real-time and in situ monitoring of living cell activities in life science and medicine. This paper reports a whole cell sensing protocol over the interface of Au film coupled in a wavelength-modulated surface plasmon resonance (WMSPR) biosensor. With dual parabolic mirrors integrated in the sensor, the compact and miniaturized instrument shows satisfactory refractive index sensitivity (2220 nm/RIU) and a high resolution of resonance wavelength shift of 0.3 nm to liquid samples. The affinity interactions between the biomarker of human tumor endothelial marker 8 (TEM8) and antibody (Ab) or specific polypeptide (PEP) were firstly introduced to WMSPR biosensor analysis. Both the interaction events of Ab-cell and PEP-cell over the Au film interface can be recognized by the sensor and the balance time of interactions is about 20 min. The concentration range of Ab for quantitative monitoring of the TEM8 expression on human colon carcinoma SW620 cells was investigated. The present low-cost and time-saving method provides a time resolution of binding specificity between Ab/PEP and TEM8 for real-time analysis of antigen on living tumor cell surface. PMID:26822761

  19. Irradiation effects in 6H-SiC induced by neutron and heavy ions: Raman spectroscopy and high-resolution XRD analysis

    NASA Astrophysics Data System (ADS)

    Chen, Xiaofei; Zhou, Wei; Feng, Qijie; Zheng, Jian; Liu, Xiankun; Tang, Bin; Li, Jiangbo; Xue, Jianming; Peng, Shuming

    2016-09-01

    Irradiation effects of neutron and 3 MeV C+, Si+ in 6H-SiC were investigated by Raman spectroscopy and high-resolution XRD. The total disorder values of neutron irradiated SiC agree well with that of samples irradiated by ions at the same doses respectively. On the other hand, high-resolution XRD results shows that the lattice strain rate caused by neutron irradiation is 6.8%/dpa, while it is only 2.6%/dpa and 4.2%/dpa for Si+ and C+ irradiations respectively. Our results illustrate that the total disorder in neutron irradiated SiC can be accurately simulated by MeV Si+ or C+ irradiations at the same dose, but for the lattice strain and strain-related properties like surface hardness, the depth profile of irradiation damages induced by energetic ions must be considered. This research will contribute to a better understanding of the difference in irradiation effects between neutron and heavy ions.

  20. In situ characterization of uranium and americium oxide solid solution formation for CRMP process: first combination of in situ XRD and XANES measurements.

    PubMed

    Caisso, Marie; Picart, Sébastien; Belin, Renaud C; Lebreton, Florent; Martin, Philippe M; Dardenne, Kathy; Rothe, Jörg; Neuville, Daniel R; Delahaye, Thibaud; Ayral, André

    2015-04-14

    Transmutation of americium in heterogeneous mode through the use of U1-xAmxO2±δ ceramic pellets, also known as Americium Bearing Blankets (AmBB), has become a major research axis. Nevertheless, in order to consider future large-scale deployment, the processes involved in AmBB fabrication have to minimize fine particle dissemination, due to the presence of americium, which considerably increases the risk of contamination. New synthesis routes avoiding the use of pulverulent precursors are thus currently under development, such as the Calcined Resin Microsphere Pelletization (CRMP) process. It is based on the use of weak-acid resin (WAR) microspheres as precursors, loaded with actinide cations. After two specific calcinations under controlled atmospheres, resin microspheres are converted into oxide microspheres composed of a monophasic U1-xAmxO2±δ phase. Understanding the different mechanisms during thermal conversion, that lead to the release of organic matter and the formation of a solid solution, appear essential. By combining in situ techniques such as XRD and XAS, it has become possible to identify the key temperatures for oxide formation, and the corresponding oxidation states taken by uranium and americium during mineralization. This paper thus presents the first results on the mineralization of (U,Am) loaded resin microspheres into a solid solution, through in situ XAS analysis correlated with HT-XRD. PMID:25742991

  1. Characterization of wet precipitation by X-ray diffraction (XRD) and scanning electron microscopy (SEM) in the metropolitan area of Porto Alegre, Brazil.

    PubMed

    Migliavacca, Daniela Montanari; Teixeira, Elba Calesso; Gervasoni, Fernanda; Conceição, Rommulo Vieira; Rodriguez, Maria Teresa Raya

    2009-11-15

    The purpose of this study is to assess the composition of wet precipitation in three sites of the metropolitan area of Porto Alegre. Besides the variables usually considered, such as pH, conductivity, major ions (Cl(-), NO(3)(-), F(-), SO(4)(2-), Na(+), K(+), Mg(2+), NH(4)(+) and Ca(2+)) and metallic elements (Cd, Co, Cr, Cu, Fe, Mn and Ni), the suspended matter was examined by X-ray diffraction (XRD) and scanning electron microscopy (SEM), with energy dispersive system (EDS), for better identification of possible anthropogenic material in this wet precipitation. Results showed an alkaline pH in the samples analyzed and higher concentrations for Na(+), Cl(-) and SO(4)(2-). The acidification and neutralization potential between anions (SO(4)(2-)+NO(3)(-)) and cations (Ca(2+)+Mg(2+)+K(+)+NH(4)(+)) showed a good correlation (0.922). The metallic elements with highest values were Zn, Fe and Mn. Results of XRD identified the presence of some minerals such as quartz, feldspar, mica, clay, carbonates and sulfates. In samples analyzed with SEM, we detected pyroxene, biotite, amphibole and oxides. Cluster analysis (CA) was applied to the data matrix to identify potential pollution sources of metals (natural or anthropogenic) and the association with minerals found in the analysis of SEM.

  2. An experimental study of the (Ti-6Al-4V)-xH phase diagram using in situ synchrotron XRD and TGA/DSC techniques.

    SciTech Connect

    Sun, Pei; Fang, Z. Zak; Koopman, Mark; Paramore, James D.; Chandran, K. S. Ravi; Ren, Yang; Lu, Jun

    2015-02-01

    Hydrogen has been investigated for decades as a temporary alloying element to refine the microstructure of Ti-6Al-4V, and is now being used in a novel powder metallurgy method known as "hydrogen sintering and phase transformation". Pseudo-binary phase diagrams of (Ti-6Al-4V)-xH have been studied and developed, but are not well established due to methodological limitations. In this paper, in situ studies of phase transformations during hydrogenation and dehydrogenation of (Ti-6Al-4V)-xH alloys were conducted using high-energy synchrotron X-ray diffraction (XRD), thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC). The eutectoid phase transformation of β ↔ α + δ was observed in the (Ti-6Al-4V)-xH alloy via in situ synchrotron XRD at 211 °C with a hydrogen concentration of 37.5 at.% (measured using TGA-DSC). The relationships of hydrogen composition to partial pressure and temperature were investigated in the temperature range 450-900°C. Based on these results, a partial pseudo-binary phase diagram of (Ti-6Al-4V)-xH is proposed for hydrogen compositions up to 60 at.% in the temperature range 100-900°C. Using the data collected in real time under controlled parameters of temperature, composition and hydrogen partial pressure, this work characterizes relevant phase transformations and microstructural evolution for practical titanium-hydrogen technologies of Ti-6Al-4V.

  3. Mineralogical In-situ Investigation of Acid-Sulfate Samples from the Rio Tinto River, Spain, with a Portable XRD/XRF Instrument

    NASA Technical Reports Server (NTRS)

    Sarrazin, P.; Ming, D. W.; Morris, R. V.; Fernandez-Remolar, D.; Amils, R.; Arvidson, R. E.; Blake, D.; Bish, D. L.

    2007-01-01

    A field campaign was organized in September 2006 by Centro de Astobiologica (Spain) and Washington University (St Louis, USA) for the geological study of the Rio Tinto river bed sediments using a suite of in-situ instruments comprising an ASD reflectance spectrometer, an emission spectrometer, panoramic and close-up color imaging cameras, a life detection system and NASA's CheMin 4 XRD/XRF prototype. The primary objectives of the field campaign were to study the geology of the site and test the potential of the instrument suite in an astrobiological investigation context for future Mars surface robotic missions. The results of the overall campaign will be presented elsewhere. This paper focuses on the results of the XRD/XRF instrument deployment. The specific objectives of the CheMin 4 prototype in Rio Tinto were to 1) characterize the mineralogy of efflorescent salts in their native environments; 2) analyze the mineralogy of salts and oxides from the modern environment to terraces formed earlier as part of the Rio Tinto evaporative system; and 3) map the transition from hematite-dominated terraces to the mixed goethite/salt-bearing terraces where biosignatures are best preserved.

  4. Thermoluminescence (TL) properties and x-ray diffraction (XRD) analysis of high purity CaSO{sub 4}:Dy TL material

    SciTech Connect

    Kamarudin, Nadira; Abdullah, Wan Saffiey Wan; Dollah, Mohd Taufik; Hamid, Muhammad Azmi Abdul

    2014-09-03

    This paper presents the characterization and TL properties of dysprosium (Dy) doped calcium sulfate (CaSO{sub 4}) TL material produced by co-precipitation technique with 0.5mol% concentration of dopant. The morphology of the produced TL material was studied using scanning electron microscope (SEM) and the micrograph shows that rectangular parallelepiped shaped crystal with the average of 150 μm in length were produced. The crystallinity of the produced powder was studied using x-ray powder diffraction (XRD). The XRD spectra show that the TL material produced is high purity anhydrite CaSO{sub 4} with average crystallite size of 74 nm with orthorhombic crystal system. The TL behavior of produced CaSO{sub 4}:Dy was studied using a TLD reader after exposure to gamma ray by Co{sup 60} source with the doses of 1,5 and 10 Gy. The glow curve shows linear response with glow peak around 230°C which is desired development in the field of radiation dosimetry.

  5. Structure analysis and spectroscopic characterization of 2-Fluoro-3-Methylpyridine-5-Boronic Acid with experimental (FT-IR, Raman, NMR and XRD) techniques and quantum chemical calculations

    NASA Astrophysics Data System (ADS)

    Alver, Özgür; Dikmen, Gökhan

    2016-03-01

    Possible stable conformers, geometrical molecular structures, vibrational properties as well as band assignments, nuclear magnetic shielding tensors of 2-Fluoro-3-Methylpyridine-5-Boronic Acid (2F3MP5BA) were studied experimentally and theoretically using FT-IR, Raman, (CP/MAS) NMR and XRD spectroscopic methods. FT-IR and Raman spectra were evaluated in the region of 3500-400 cm-1, and 3200-400 cm-1, respectively. The optimized geometric structures, vibrational wavenumbers and nuclear magnetic shielding tensors were examined using Becke-3-Lee-Yang-Parr (B3LYP) hybrid density functional theory method with 6-311++G(d, p) basis set. 1H, 13C NMR chemical shifts were calculated using the gauge invariant atomic orbital (GIAO) method. 1H, 13C, APT and HETCOR NMR experiments of title molecule were carried out in DMSO solution. 13C CP/MAS NMR measurement was done with 4 mm zirconium rotor and glycine was used as an external standard. Single crystal of 2F3MP5BA was also prepared for XRD measurements. Assignments of vibrational wavenumbers were also strengthened by calculating the total energy distribution (TED) values using scaled quantum mechanical (SQM) method.

  6. Combined In-Situ XRD and In-Situ XANES Studies on the Reduction Behavior of a Rhenium Promoted Cobalt Catalyst

    SciTech Connect

    Kumar, Nitin; Payzant, E Andrew; Jothimurugesan, K; Spivey, James J

    2011-01-01

    A 10% Co 4% Re/(2% Zr/SiO2) catalyst was prepared by co-impregnation using a silica support modified by 2% Zr. The catalyst was characterized by temperature programmed reduction (TPR), in situ XRD and in situ XANES analysis where it was simultaneously exposed to H2 using a temperature programmed ramp. The results showed the two step reduction of large crystalline Co3O4 with CoO as an intermediate. TPR results showed that the reduction of highly dispersed Co3O4 was facilitated by reduced rhenium by a H2-spillover mechanism. In situ XRD results showed the presence of both, Co-hcp and Co-fcc phases in the reduced catalyst at 400 C. However, the Co-hcp phase was more abundant, which is thought to be the more active phase as compared to the Co-fcc phase for CO hydrogenation. CO hydrogenation at 270 C and 5 bar pressure produces no detectable change in the phases during the time of experiment. In situ XANES results showed a decrease in the metallic cobalt in the presence of H2/CO, which can be attributed due to oxidation of the catalyst by reaction under these conditions.

  7. Magnetic composites from minerals: study of the iron phases in clay and diatomite using Mössbauer spectroscopy, magnetic measurements and XRD

    NASA Astrophysics Data System (ADS)

    Cabrera, M.; Maciel, J. C.; Quispe-Marcatoma, J.; Pandey, B.; Neri, D. F. M.; Soria, F.; Baggio-Saitovitch, E.; de Carvalho, L. B.

    2014-01-01

    Magnetic particles as matrix for enzyme immobilization have been used and due to the enzymatic derivative can be easily removed from the reaction mixture by a magnetic field. This work presents a study about the synthesis and characterization of iron phases into magnetic montmorillonite clay (mMMT) and magnetic diatomaceous earth (mDE) by 57Fe Mössbauer spectroscopy (MS), magnetic measurements and X-ray diffraction (XRD). Also these magnetic materials were assessed as matrices for the immobilization of invertase via covalent binding. Mössbauer spectra of the magnetic composites performed at 4.2 K showed a mixture of magnetite and maghemite about equal proportion in the mMMT, and a pure magnetite phase in the sample mDE. These results were verified using XRD. The residual specific activity of the immobilized invertase on mMMT and mDE were 83 % and 92.5 %, respectively. Thus, both magnetic composites showed to be promising matrices for covalent immobilization of invertase.

  8. In-situ investigation of stress conditions during expansion of bare metal stents and PLLA-coated stents using the XRD sin(2)ψ-technique.

    PubMed

    Kowalski, Wolfgang; Dammer, Markus; Bakczewitz, Frank; Schmitz, Klaus-Peter; Grabow, Niels; Kessler, Olaf

    2015-09-01

    Drug eluting stents (DES) consist of platform, coating and drug. The platform often is a balloon-expandable bare metal stent made of the CoCr alloy L-605 or stainless steel 316 L. The function of the coating, typically a permanent polymer, is to hold and release the drug, which should improve therapeutic outcome. Before implantation, DES are compressed (crimped) to allow implantation in the human body. During implantation, DES are expanded by balloon inflation. Crimping, as well as expansion, causes high stresses and high strains locally in the DES struts, as well as in the polymer coating. These stresses and strains are important design criteria of DES. Usually, they are calculated numerically by finite element analysis (FEA), but experimental results for validation are hardly available. In this work, the X-ray diffraction (XRD) sin(2)ψ-technique is applied to in-situ determination of stress conditions of bare metal L-605 stents, and Poly-(L-lactide) (PLLA) coated stents. This provides a realistic characterization of the near-surface stress state and a validation option of the numerical FEA. XRD-results from terminal stent struts of the bare metal stent show an increasing compressive load stress in tangential direction with increasing stent expansion. These findings correlate with numerical FEA results. The PLLA-coating also bears increasing compressive load stress during expansion.

  9. Local probing of structure and property in dimensionally confined amorphous and crystalline structures by S/TEM

    NASA Astrophysics Data System (ADS)

    Yan, Aiming

    The characterization of materials' microstructure has been brought up to a new level since the invention and broad application of transmission electron microscope (TEM) thanks to the high-energy electron beam source which guarantees an unsurpassable spatial resolution and theoretical study of interaction between electron and matter. The advent of nano-world has imposed an urgent request to characterize nano-assemblies in nano- or even sub-nano-scale and scanning transmission electron microscopy (STEM) which typically utilizes an electron probe with a size of 1nm or even smaller has found its unique advantage to unravel the local structure, chemical and physical properties of these emerging nanostructures. Dimensionally constrained nanostructures such as thin films and nanopatterned systems have attracted people's attention for decades due to their novel chemical and physical properties and popularity in energy storage, biological integration and etc. This dissertation focuses on the unique characterization capability of S/TEM to study the local order in amorphous transparent conducting oxide thin films, disordering in 2-D layered materials, localized surface plasmons in nanoporous gold patterns on 2-D layered structures and crystallization process in dimensionally and spatially constrained oxide nanopatterns observed by in-situ TEM. Electron diffraction and x-ray diffraction are commonly used techniques to study the crystallinity in a certain material - crystalline or amorphous. In amorphous materials which lack long-range order, normal electron diffraction and x-ray diffraction techniques won't be able to extract any useful information regarding the ordering or disordering in the materials. We have developed a unique set of electron diffraction methods in both TEM and STEM, combined with density functional theory molecular dynamics of liquid quench to study the short-range (< 1 nm) and medium-range order (between 1 nm and 3 nm) in amorphous transparent oxide films

  10. Focused Ion Beam (FIB) combined with SEM (FIB/SEM) and TEM: Advanced tools for nano-analysis in Geosciences

    NASA Astrophysics Data System (ADS)

    Wirth, R.; Morales, L. G.

    2011-12-01

    Focused ion beam (FIB) techniques have been successfully applied to the preparation of site-specific electron transparent membranes for transmission electron microscopy (TEM) investigations in Geosciences since several years. For example, systematic TEM studies of nano-inclusions in diamond foils prepared with FIB have improved our knowledge on diamond formation. However, FIB is not exclusively used for sample preparation for TEM application because it has been proved that one and the same TEM foil can also be used for Synchrotron IR, Synchrotron X-Ray fluorescence (XRF), scanning transmission X-Ray microscopy (STXM) and NanoSIMS analysis. In addition, FIB milling turned out to be very useful for sample preparation of Brillouin scattering experiments and has a strong potential for preparation of highly-polished, micrometer-scale samples. However, a real break through in FIB application was achieved combining a Ga-ion source of the FIB with an electron source of a scanning electron microscope (SEM) in one single instrument. The combination of FIB/SEM renders access to the third dimension of the sample possible. A cavity normal to the sample surface is sputtered with Ga-ions and this newly created inner surface is imaged with the electron beam. Alternating slicing and viewing along these cavities allow the acquisition of a sequence of images that allows the observation in 3 dimensions. Recently, this technique has been successfully applied to image the structure of grain or phase boundaries in metamorphic rocks as well as micro- and nanoporosity in shales, but its applicability goes far beyond these few examples. Combining slicing and viewing with X-Ray and electron backscatter diffraction (EBSD) analysis can provide 3D elemental mapping and 3D crystallographic orientation mapping of crystalline materials. Combined FIB/SEM devices also facilitate the preparation of substantially thinner and cleaner TEM foils (approximately 30 nm) because electron beam imaging

  11. β-lactamases produced by amoxicillin-clavulanate-resistant enterobacteria isolated in Buenos Aires, Argentina: a new blaTEM gene.

    PubMed

    Di Conza, José A; Badaracco, Alejandra; Ayala, Juan; Rodríguez, Cynthia; Famiglietti, Angela; Gutkind, Gabriel O

    2014-01-01

    Resistance to β-lactam/β-lactamase inhibitors in enterobacteria is a growing problem that has not been intensively studied in Argentina. In the present work, 54/843 enterobacteria collected in a teaching hospital of Buenos Aires city were ampicillin-sulbactam-resistant isolates remaining susceptible to second- and third-generation cephalosporins. The enzymatic mechanisms present in the isolates, which were also amoxicillin-clavulanic acid (AMC)-resistant (18/54) were herein analyzed. Sequencing revealed two different variants of blaTEM-1, being blaTEM-1b the most frequently detected allelle (10 Escherichia coli, 3 Klebsiella pneumoniae, 2 Proteus mirabilis and 1 Raoultella terrigena) followed by blaTEM-1a (1 K. pneumoniae). Amoxicillin-clavulanate resistance seems to be mainly associated with TEM-1 overproduction (mostly in E. coli) or co-expressed with OXA-2-like and/or SHV β-lactamases (K. pneumoniae and P. mirabilis). A new blaTEM variant (TEM-163) was described in an E. coli strain having an AMC MIC value of 16/8μg/ml. TEM-163 contains Arg275Gln and His289Leu amino acid substitutions. On the basis of the high specific activity and low IC50 for clavulanic acid observed, the resistance pattern seems to be due to overproduction of the new variant of broad spectrum β-lactamase rather than to an inhibitor-resistant TEM (IRT)-like behavior.

  12. TEM-71, a Novel Plasmid-Encoded, Extended-Spectrum β-Lactamase Produced by a Clinical Isolate of Klebsiella pneumoniae

    PubMed Central

    Rasheed, J. Kamile; Anderson, Gregory J.; Queenan, Anne Marie; Biddle, James W.; Oliver, Antonio; Jacoby, George A.; Bush, Karen; Tenover, Fred C.

    2002-01-01

    TEM-71, a novel extended-spectrum β-lactamase from a Klebsiella pneumoniae clinical isolate, had an isoelectric point of 6.0 and a substrate profile showing preferential hydrolysis of cefotaxime over ceftazidime. It differed from TEM-1 by two substitutions, Gly238Ser and Glu240Lys, and was under the control of the strong P4 promoter. PMID:12019125

  13. Raman-Mössbauer-XRD studies of selected samples from "Los Azulejos" outcrop: A possible analogue for assessing the alteration processes on Mars

    NASA Astrophysics Data System (ADS)

    Lalla, E. A.; Sanz-Arranz, A.; Lopez-Reyes, G.; Sansano, A.; Medina, J.; Schmanke, D.; Klingelhoefer, G.; Rodríguez-Losada, J. A.; Martínez-Frías, J.; Rull, F.

    2016-06-01

    The outcrop of "Los Azulejos" is visible at the interior of the Cañadas Caldera in Tenerife Island (Spain). It exhibits a great variety of alteration processes that could be considered as terrestrial analogue for several geological processes on Mars. This outcrop is particularly interesting due to the content of clays, zeolite, iron oxides, and sulfates corresponding to a hydrothermal alteration catalogued as "Azulejos" type alteration. A detailed analysis by portable and laboratory Raman systems as well as other different techniques such as X-ray diffraction (XRD) and Mössbauer spectroscopy has been carried out (using twin-instruments from Martian lander missions: Mössbauer spectrometer MIMOS-II from the NASA-MER mission of 2001 and the XRD diffractometer from the NASA-MSL Curiosity mission of 2012). The mineral identification presents the following mineral species: magnetite, goethite, hematite, anatase, rutile, quartz, gregoryite, sulfate (thenardite and hexahydrite), diopside, feldspar, analcime, kaolinite and muscovite. Moreover, the in-situ Raman and Micro-Raman measurements have been performed in order to compare the capabilities of the portable system specially focused for the next ESA Exo-Mars mission. The mineral detection confirms the sub-aerial alteration on the surface and the hydrothermal processes by the volcanic fluid circulations in the fresh part. Therefore, the secondary more abundant mineralization acts as the color agent of the rocks. Thus, the zeolite-illite group is the responsible for the bluish coloration, as well as the feldspars and carbonates for the whitish and the iron oxide for the redish parts. The XRD system was capable to detect a minor proportion of pyroxene, which is not visible by Raman and Mössbauer spectroscopy due to the "Azulejos" alteration of the parent material on the outcrop. On the other hand, Mössbauer spectroscopy was capable of detecting different types of iron-oxides (Fe3+/2+-oxide phases). These analyses

  14. Integration of TEM/Hrtem onservations and C-isotope geochemistry to characterize organic matter in early Archaean rocks

    NASA Astrophysics Data System (ADS)

    Glikson, M.; Golding, S.; Duck, L.; Webb, R.

    2009-04-01

    TEM was applied to observe and characterize carbonaceous materials (CM) extracted from black cherts in the 'white smoker type' deposit of the ca.3.5Ga (model Pb/Pb ages =3.49-3.51Ga) Dresser ormation, and the overlying black argillites of the 3.46Ga Salgash Subgroup, in the Pilbara of Western Australia. These were characterized by Transmission Electron Microscopy (TEM) coupled with electron dispersive spectral analysis (EDS), High Resolution TEM (HRTEM) to determine molecular ordering, and C-isotope geochemistry. Observations using TEM and HRTEM enabled morphological and fine structure distinctions between the various populations of CM both in the Dresser and Salgash samples. These formed the basis for their interpretations. Organic petrology using reflected light microscopy was applied to whole rock samples to observe mineral-organic relationship and structure relative to host rock texture. These supported insitu, syn-depositional mode for the Dresser Formation CM. Reflectance % (Ro) of CM determined on polished whole rock samples and polished resin-embedded CM concentrates enabled the reconstruction of its thermal history. These yielded several Ro populations in the Dresser Formation samples: probable microbial cells preserved in fluid inclusions within quartz crystals, severely thermally degraded CM possibly originally belonging to microbial cells, CM coating mineral grains and reworked CM particles. On the other hand, the Salgash suite of samples from the Apex Basalt Formation yielded consistent very high Ro values corresponding to graphite stage organic metamorphism. the weak optical anisotropy of the graphite points to a defferent mode of formation than regional metamorphism. Two main graphite forms have been identified, namely a platy and tubular. The tubular form when observed in HRTEM showed nano-tubes and fullerenes. Dresser Formation samples are isotopically light in the range of -32.1 to -38.2per mil supporting a biological source. Although in TEM four

  15. Substructural Properties and Anisotropic Peak Broadening in Zn1-x Mn x Te Films Determined by a Combined Methodology Based on SEM, HRTEM, XRD, and HRXRD

    NASA Astrophysics Data System (ADS)

    Martinez-Tomas, C.; Klymov, O.; Agouram, S.; Kurbatov, D.; Opanasyuk, A.; Muñoz-Sanjosé, V.

    2016-09-01

    Lattice deformation and extended defects such as grain boundaries and dislocations affect the crystalline quality of films and can dramatically change material's properties. In particular, magnetic and optoelectronic properties depend strongly on these structural and substructural characteristics. In this paper, a combined methodology based on SEM, HRTEM, XRD, and HRXRD measurements is used to determine and assess the structural and substructural characteristics of films. This combined methodology has been applied to Zn1-x Mn x Te films grown on glass substrates by close-spaced vacuum sublimation. Nevertheless the methodology can be applied to a wide variety of materials and could become a useful characterization method which would be particularly valuable in semiconductor growth field. The knowledge of the structural and substructural characteristics can allow not only the optimization of growth parameters, but also the selection of specific samples having the desired characteristics (crystallite size, minimum dislocation content, etc.) for high-quality technological devices.

  16. A new approach in quantitative in-situ XRD of cement pastes: Correlation of heat flow curves with early hydration reactions

    SciTech Connect

    Hesse, Christoph; Goetz-Neunhoeffer, Friedlinde; Neubauer, Juergen

    2011-01-15

    XRD measurements of the hydration of synthetical cement (SyCem) were used to calculate the resulting heat flow from changes in the phase content. Calculations were performed by application of thermodynamic data. The comparison with data recorded from heat flow calorimetry was in good agreement with the calculated heat flow. The initial maximum of heat flow mainly is caused by the aluminate reaction. During the entire main period the silicate reaction dominates hydration with a high and long first maximum of heat flow. The second but less intense heat flow maximum - only visible as a shoulder in most of the technical cements - can be attributed to an acceleration of the aluminate reaction with the enhanced dissolution of C{sub 3}A and the final formation of ettringite. Moreover, the investigation showed that the dissolution process of C{sub 3}A is directly controlled by the availability of the calcium sulfate phases.

  17. Incorporation of Co(II) in dealuminated BEA zeolite at lattice tetrahedral sites evidenced by XRD, FTIR, diffuse reflectance UV-Vis, EPR, and TPR.

    PubMed

    Dzwigaj, S; Che, M

    2006-06-29

    A CoSiBEA zeolite is prepared by a two-step postsynthesis method that consists of first creating vacant T-sites with associated silanol groups by dealumination of TEABEA zeolite with nitric acid and then impregnating the resulting SiBEA zeolite with an aqueous solution of Co(NO3)2. The incorporation of Co into lattice sites of SiBEA is evidenced by XRD. The consumption of OH groups is monitored by FTIR. The presence of Co in its II oxidation state and in tetrahedral coordination is evidenced by diffuse reflectance UV-vis and EPR spectroscopy. The very high reduction temperature (1120 K) of cobalt in CoSiBEA zeolite determined by TPR confirms that Co interacts strongly with the zeolite support, consistent with lattice tetrahedral (T(d)) coordination.

  18. An AEM-TEM study of nanometer-scale mineral associations in an aquifer sand: Implications for colloid mobilization

    NASA Astrophysics Data System (ADS)

    Swartz, Christopher H.; Ulery, April L.; Gschwend, Philip M.

    1997-02-01

    Analytical and transmission electron microscopy (AEM-TEM) techniques were used to identify mineral juxtapositions at the nanometer-scale in the interstitial matrix of a shallow, Southeastern Coastal plain aquifer sand (Georgetown, South Carolina, USA). In doing so, we sought to infer particle-particle interaction mechanisms holding the matrix intact. The aquifer is a fine-to-medium quartz sand with approximately 12% by weight <63 μm size fraction composing the interstitial matrix. The clay-size fraction contains kaolinite, goethite, gibbsite, and vermiculite. The arrangement of the clay minerals is that of a framework of face-associated domains. Selective extraction revealed that goethite constituted 95% by weight of the free iron oxyhydroxides in the <63 μm size fraction, but AEM-TEM and high resolution TEM (HRTEM) indicated that the goethite occurred only in discrete aggregates among the clays. Conversely, the remaining 5% of the free iron oxyhydroxides comprised an amorphous iron phase which was found to be distributed throughout the matrix and directly associated with the clay particles. This evidence suggests that the amorphous iron oxyhydroxide phase could act as an effective binding intermediary among the clay-clay associations, possibly electrostatically or through bond linkages with the clay surfaces. In addition, HRTEM indicated the presence of another amorphous phase which appeared to hold the clay particle aggregates in a cementitious web. AEM suggested that this amorphous phase was silicon enriched, probably biogenic opal. This evidence suggests that instigating dissolution of the opaline silica phase may be necessary to induce substantial colloid mobilization in this aquifer sediment.

  19. A Generic 1D Forward Modeling and Inversion Algorithm for TEM Sounding with an Arbitrary Horizontal Loop

    NASA Astrophysics Data System (ADS)

    Li, Zhanhui; Huang, Qinghua; Xie, Xingbing; Tang, Xingong; Chang, Liao

    2016-08-01

    We present a generic 1D forward modeling and inversion algorithm for transient electromagnetic (TEM) data with an arbitrary horizontal transmitting loop and receivers at any depth in a layered earth. Both the Hankel and sine transforms required in the forward algorithm are calculated using the filter method. The adjoint-equation method is used to derive the formulation of data sensitivity at any depth in non-permeable media. The inversion algorithm based on this forward modeling algorithm and sensitivity formulation is developed using the Gauss-Newton iteration method combined with the Tikhonov regularization. We propose a new data-weighting method to minimize the initial model dependence that enhances the convergence stability. On a laptop with a CPU of i7-5700HQ@3.5 GHz, the inversion iteration of a 200 layered input model with a single receiver takes only 0.34 s, while it increases to only 0.53 s for the data from four receivers at a same depth. For the case of four receivers at different depths, the inversion iteration runtime increases to 1.3 s. Modeling the data with an irregular loop and an equal-area square loop indicates that the effect of the loop geometry is significant at early times and vanishes gradually along the diffusion of TEM field. For a stratified earth, inversion of data from more than one receiver is useful in noise reducing to get a more credible layered earth. However, for a resistive layer shielded below a conductive layer, increasing the number of receivers on the ground does not have significant improvement in recovering the resistive layer. Even with a down-hole TEM sounding, the shielded resistive layer cannot be recovered if all receivers are above the shielded resistive layer. However, our modeling demonstrates remarkable improvement in detecting the resistive layer with receivers in or under this layer.

  20. Characterization of the groundwater aquifers at El Sadat City by joint inversion of VES and TEM data

    NASA Astrophysics Data System (ADS)

    Massoud, Usama; Kenawy, Abeer A.; Ragab, El-Said A.; Abbas, Abbas M.; El-Kosery, Heba M.

    2014-12-01

    Vertical Electrical Sounding (VES) and Transient ElectroMagnetic (TEM) survey have been applied for characterizing the groundwater aquifers at El Sadat industrial area. El-Sadat city is one of the most important industrial cities in Egypt. It has been constructed more than three decades ago at about 80 km northwest of Cairo along the Cairo-Alexandria desert road. Groundwater is the main source of water supplies required for domestic, municipal and industrial activities in this area due to the lack of surface water sources. So, it is important to maintain this vital resource in order to sustain the development plans of this city. In this study, VES and TEM data were identically measured at 24 stations along 3 profiles trending NE-SW with the elongation of the study area. The measuring points were arranged in a grid-like pattern with both inter-station spacing and line-line distance of about 2 km. After performing the necessary processing steps, the VES and TEM data sets were inverted individually to multi-layer models, followed by a joint inversion of both data sets. Joint inversion process has succeeded to overcome the model-equivalence problem encountered in the inversion of individual data set. Then, the joint models were used for the construction of a number of cross sections and contour maps showing the lateral and vertical distribution of the geoelectrical parameters in the subsurface medium. Interpretation of the obtained results and correlation with the available geological and hydrogeological information revealed TWO aquifer systems in the area. The shallow Pleistocene aquifer consists of sand and gravel saturated with fresh water and exhibits large thickness exceeding 200 m. The deep Pliocene aquifer is composed of clay and sand and shows low resistivity values. The water-bearing layer of the Pleistocene aquifer and the upper surface of Pliocene aquifer are continuous and no structural features have cut this continuity through the investigated area.