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Sample records for xrd hrtem magnetic

  1. 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.

    2016-12-01

    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.

  2. HRTEM, SAED and XRD investigations of RE{sub 4}O{sub 4}[AsO{sub 4}]Cl (RE = La, Pr, Nd, Sm, Eu, Gd)

    SciTech Connect

    Ben Yahia, Hamdi; Rodewald, Ute Ch.; Boulahya, Khalid; Pöttgen, Rainer

    2014-05-01

    Graphical abstract: The new compounds RE{sub 4}O{sub 4}[AsO{sub 4}]Cl (RE = La, Pr, Nd, Sm, Eu, Gd) were synthesised by solid state reaction via a salt flux route and investigated by HRTEM, SAED, and single crystal X-ray diffraction. - Highlights: • We discovered the series of RE{sub 4}O{sub 4}[AsO{sub 4}]Cl (RE = La, Pr, Nd, Sm, Eu, Gd) compounds. • The RE{sub 4}O{sub 4}[AsO{sub 4}]Cl single crystals were grown using NaCl/KCl flux. • The RE{sub 4}O{sub 4}[AsO{sub 4}]Cl structures were solved using single crystal X-ray diffraction data. • The layered RE{sub 4}O{sub 4}[AsO{sub 4}]Cl compounds were further characterized using HRTEM and SAED. • We observed an alternation of ordered-[RE{sub 4}O{sub 4}]{sup 4+} and disordered-[ClAsO{sub 4}]{sup 4–} layers. - Abstract: The new compounds RE{sub 4}O{sub 4}[AsO{sub 4}]Cl (RE = La, Pr, Nd, Sm, Eu, Gd) were synthesised by solid state reaction via a salt flux route and investigated by HRTEM, SAED, and single crystal X-ray diffraction. The samples crystallise with a tetragonal cell, space group P4{sub 2}/mnm and Z = 2. Their crystal structure consists of an alternation of [RE{sub 4}O{sub 4}]{sup 4+} and [ClAsO{sub 4}]{sup 4–} layers. The [RE{sub 4}O{sub 4}]{sup 4+} layer contains ORE{sub 4/4} tetrahedra which share common edges. The anions AsO{sub 4}{sup 3–} and Cl{sup –} are located between these layers in disordered manner. SAED and HRTEM experiments confirmed this structural model and enabled us to propose an ordered model for the [ClAsO{sub 4}]{sup 4–} layers.

  3. Evolution of clay mineral assemblages in the Tinguiririca geothermal field, Andean Cordillera of central Chile: an XRD and HRTEM-AEM study

    NASA Astrophysics Data System (ADS)

    Vázquez, M.; Nieto, F.; Morata, D.; Droguett, B.; Carrillo-Rosua, F. J.; Morales, S.

    2014-08-01

    HRTEM textural evidence shows that clay minerals in the Tinguiririca geothermal field (Andean Cordillera, central Chile) are the result of direct alteration of former volcanic glass and minerals by hydrothermal fluids at similar temperatures to the present day. They show the classical pattern of diagenetic transformation from smectite at the top to illite at the bottom, with the progressive formation of corrensite and chlorite. The high fluid/rock ratio, disposability of necessary cations and absence of previous detrital phyllosilicates allow the consideration of this area as a natural laboratory to establish the extreme ideal conditions for very low-T reactions. Transformations from smectite to R1 illite-smectite (I-S) and from these to R3 mixed-layers occur respectively at 80-120 °C and 125-180 °C. In spite of ideal genetic conditions, the new-formed minerals show all the defective character and lack of textural and chemical equilibrium previously described in the literature for diagenetic and hydrothermal low-temperature assemblages. Chemistry of smectite-illite phases evolves basically through a diminution of the pyrophyllitic component toward a theoretical muscovite (Si4 + + □ -> Al3 ++ K+). However, a second chemical vector (Si4 ++ Mg2 + → Al3 ++ Al3 +), that is, decreasing of the tschermack component, also contributes to the evolution toward the less Si-more Al rich muscovite in relation to the original smectite. Residual Mg (and Fe) from the latter reaction is consumed in the genesis of chloritic phases. Nevertheless, as a consequence of the lack of chemical equilibrium (probably because of the short time-scale of the geothermal alteration processes), the composition of clay minerals is highly heterogeneous at the level of a single sample. Consequently, the respective fields of smectite, R1 I-S and R3 I-S overlap each other, making the distinction among these three phases impossible based exclusively on chemical data.

  4. High Resolution Transmission Electron Microscopy (HRTEM) of nanophase ferric oxides

    NASA Technical Reports Server (NTRS)

    Golden, D. C.; Morris, R. V.; Ming, D. W.; Lauer, H. V., Jr.

    1994-01-01

    Iron oxide minerals are the prime candidates for Fe(III) signatures in remotely sensed Martian surface spectra. Magnetic, Mossbauer, and reflectance spectroscopy have been carried out in the laboratory in order to understand the mineralogical nature of Martian analog ferric oxide minerals of submicron or nanometer size range. Out of the iron oxide minerals studied, nanometer sized ferric oxides are promising candidates for possible Martian spectral analogs. 'Nanophase ferric oxide (np-Ox)' is a generic term for ferric oxide/oxihydroxide particles having nanoscale (less than 10 nm) particle dimensions. Ferrihydrite, superparamagnetic particles of hematite, maghemite and goethite, and nanometer sized particles of inherently paramagnetic lepidocrocite are all examples of nanophase ferric oxides. np-Ox particles in general do not give X-ray diffraction (XRD) patterns with well defined peaks and would often be classified as X-ray amorphous. Therefore, different np-Oxs preparations should be characterized using a more sensitive technique e.g., high resolution transmission electron microscopy (HRTEM). The purpose of this study is to report the particle size, morphology and crystalline order, of five np-Ox samples by HRTEM imaging and electron diffraction (ED).

  5. 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.

  6. FTIR, magnetic, mass spectral, XRD and thermal studies of metal chelates of tenoxicam

    NASA Astrophysics Data System (ADS)

    Zayed, M. A.; El-Dien, F. A. Nour; Mohamed, Gehad G.; El-Gamel, Nadia E. A.

    2007-09-01

    Metal chelates of anti-inflammatory drug, tenoxicam (Ten), are synthesized and characterized using elemental analyses, IR, solid reflectance, magnetic, mass spectra, thermal analyses (TGA and DTA) and X-ray powder diffraction techniques. The chelates are found to have the general formulae [M(H 2L) 2(H 2O) x] (A) 2· yH 2O (where H 2L = neutral Ten, A = Cl in case of Ni(II) and Co(II) or AcO in case of Cu(II) and Zn(II) ions, x = 0-2 and y = 0-2.5) and [M(H 2L) 3](A) z· yH 2O (A = SO 4 in case of Fe(II) ion ( z = 1) or Cl in case of Fe(III) ( z = 3) and y = 0-4). IR spectra reveal that Ten behaves as a neutral bidentate ligand coordinated to the metal ions through the pyridyl- N and carbonyl- O of the amide moiety. The solid reflectance spectra and magnetic moment measurements reveal that these chelates have tetrahedral, square planar and octahedral geometrical structures. Mass spectra are also used to confirm the proposed formulae and the possible fragments resulted from fragmentation of Ten and its Zn(II) and Cu(II) chelates are suggested. The thermal behaviour of the chelates (TG/DTG, DTA) are discussed in detailed manner and revealed that water molecules of crystallization together with anions are removed in the first and second steps while the Ten molecules are removed in the subsequent steps. Different thermodynamic parameters are evaluated and the relative thermal stabilities of the complexes are discussed. X-ray powder diffraction patterns are used to indicate the polymorphic form of Ten and if the complexes have molecular similarity with respect to type of coordination.

  7. HRTEM of extended defects in Tl-2212 thin films

    SciTech Connect

    Newcomer, P.P.; Venturini, E.L.; Doyle, B.L.; Schoene, H.

    1997-02-01

    Many applications of high temperature superconductors, HTS, require the presence of lattice defects in the material structure to suppress the motion of magnetic vortices and enhance the critical current density, J{sub c}. The microstructure of Tl{sub 2}Ba{sub 2}CaCu{sub 2}O{sub 8{minus}{delta}} (Tl-2212) thin films which have extended defects induced by high energy Au and Cu ion irradiation is studied using high resolution transmission electron microscopy, HRTEM, with slow scan digital imaging. In order to optimize the HTS properties and better analyze the consequent microstructural modification, the fluence is varied. At moderate fluences, resulting in {approximately}4% reduction of the superconducting transition, large enhancements of J{sub c} and vortex pinning potential are observed. The density and microstructure of isolated defects and surrounding structure will be discussed and compared to damage profiles calculated using the TRIM code. Correlation will be made between the HRTEM results and the changes in HTS properties.

  8. Electronic structure, magnetic and structural properties of Ni doped ZnO nanoparticles

    SciTech Connect

    Kumar, Shalendra; Vats, Prashant; Gautam, S.; Gupta, V.P.; Verma, K.D.; Chae, K.H.; Hashim, Mohd; Choi, H.K.

    2014-11-15

    Highlights: • XRD, and HR-TEM results show the single phase nature of Ni doped ZnO nanoparticles. • dc magnetization results indicate the RT-FM in Ni doped ZnO nanoparticles. • Ni L{sub 3,2} edge NEXAFS spectra infer that Ni ions are in +2 valence state. • O K edge NEXAFS spectra show that O vacancy increases with Ni doping in ZnO. - Abstract: We report structural, magnetic and electronic structural properties of Ni doped ZnO nanoparticles prepared by auto-combustion method. The prepared nanoparticles were characterized by using X-ray diffraction (XRD), high resolution transmission electron microscopy (HR-TEM), near edge X-ray absorption fine structure (NEXAFS) spectroscopy, and dc magnetization measurements. The XRD and HR-TEM results indicate that Ni doped ZnO nanoparticles have single phase nature with wurtzite lattice and exclude the presence of secondary phase. NEXAFS measurements performed at Ni L{sub 3,2}-edges indicates that Ni ions are in +2 valence state and exclude the presence of Ni metal clusters. O K-edge NEXAFS spectra indicate an increase in oxygen vacancies with Ni-doping, while Zn L{sub 3,2}-edge show the absence of Zn-vacancies. The magnetization measurements performed at room temperature shows that pure and Ni doped ZnO exhibits ferromagnetic behavior.

  9. The Peak Pairs algorithm for strain mapping from HRTEM images.

    PubMed

    Galindo, Pedro L; Kret, Sławomir; Sanchez, Ana M; Laval, Jean-Yves; Yáñez, Andrés; Pizarro, Joaquín; Guerrero, Elisa; Ben, Teresa; Molina, Sergio I

    2007-11-01

    Strain mapping is defined as a numerical image-processing technique that measures the local shifts of image details around a crystal defect with respect to the ideal, defect-free, positions in the bulk. Algorithms to map elastic strains from high-resolution transmission electron microscopy (HRTEM) images may be classified into two categories: those based on the detection of peaks of intensity in real space and the Geometric Phase approach, calculated in Fourier space. In this paper, we discuss both categories and propose an alternative real space algorithm (Peak Pairs) based on the detection of pairs of intensity maxima in an affine transformed space dependent on the reference area. In spite of the fact that it is a real space approach, the Peak Pairs algorithm exhibits good behaviour at heavily distorted defect cores, e.g. interfaces and dislocations. Quantitative results are reported from experiments to determine local strain in different types of semiconductor heterostructures.

  10. Ceramic/metal nanocomposites by lyophilization: Processing and HRTEM study

    SciTech Connect

    Gutierrez-Gonzalez, C.F.; Agouram, S.; Torrecillas, R.; Moya, J.S.; Lopez-Esteban, S.

    2012-02-15

    Highlights: Black-Right-Pointing-Pointer A cryogenic route has been used to obtain ceramic/metal nanostructured powders. Black-Right-Pointing-Pointer The powders present good homogeneity and dispersion of metal. Black-Right-Pointing-Pointer The metal nanoparticle size distributions are centred in 17-35 nm. Black-Right-Pointing-Pointer Both phases, ceramic and metal, present a high degree of crystallinity. Black-Right-Pointing-Pointer Good metal/ceramic interfaces due to epitaxial growth, studied by HRTEM. -- Abstract: This work describes a wet-processing route based on spray-freezing and subsequent lyophilization designed to obtain nanostructured ceramic/metal powders. Starting from the ceramic powder and the corresponding metal salt, a water-based suspension is sprayed on liquid nitrogen. The frozen powders are subsequently freeze-dried, calcined and reduced. The material was analyzed using X-ray diffraction analysis at all stages. High resolution transmission electron microscopy studies showed a uniform distribution of metal nanoparticles on the ceramic grain surfaces, good interfaces and high crystallinity, with an average metal particle size in the nanometric range.

  11. Magnetic properties of carbon-encapsulated Fe-Co alloy nanoparticles.

    PubMed

    Wu, Aibing; Yang, Xuwei; Yang, Hua

    2013-04-14

    Carbon-encapsulated Fe-Co alloy nanoparticles (Fe-Co(C)) have been fabricated with different Co/Fe ratios by an efficient solid-state route using melamine as carbon source. The structure and morphology of Fe-Co(C) nanoparticles were characterized by X-ray diffraction (XRD) and transmission electron microscopy (TEM) and high-resolution transmission electron microscopy (HRTEM). The XRD characterization results reveal that all products are alloys with no carbide impurity. The TEM and HRTEM observations show that the alloy nanoparticles are encapsulated in carbon shells. Additionally, the reactions involved in the syntheses are postulated. The variation of magnetic properties of Fe-Co(C) with Co/Fe has been discussed according to the room temperature VSM measurement results.

  12. Synthesis, characterization and magnetic property of maghemite (γ-Fe{sub 2}O{sub 3}) nanoparticles and their protective coating with pepsin for bio-functionalization

    SciTech Connect

    Bandhu, A.; Sutradhar, S.; Mukherjee, S.; Greneche, J.M.; Chakrabarti, P.K.

    2015-10-15

    Highlights: • Maghemite nanoparticles were prepared by a modified co-precipitation method. • Nanoparticles were then successfully coated with pepsin for bio-functionlization. • XRD and Mössbauer spectra confirmed the maghemite phase of the nanoparticles. • Magnetic data were analysed to evaluate particle size, anisotropy etc. - Abstract: Maghemite nanoparticles (γ-Fe{sub 2}O{sub 3}) are prepared by co-precipitation method. To obtain bio-functionalized magnetic nanoparticles for magnetically controlled drug delivery, the prepared nanoparticles are successfully coated with pepsin, a bio-compatible polymer and digestive enzyme. Crystallographic phase of the nanoparticles is confirmed by X-ray diffractograms (XRD), high resolution transmission electron microscopy (HRTEM) and {sup 57}Fe Mössbauer spectrometry. The average size of nanoparticles/nanocrystallites is estimated from the (3 1 1) peak of the XRD pattern using Debye–Scherrer formula. Results of HRTEM of coated and bare samples are in good agreement with those extracted from the XRD analysis. The dynamic magnetic properties are observed and different quantities viz., coercive field, magnetization, remanence, hysteresis losses etc., are estimated, which confirmed the presence of superparamagnetic relaxation of nanoparticles. Mössbauer spectra of the samples recorded at both 300 and 77 K, confirmed that the majority of particles are maghemite together with a very small fraction of magnetite nanoparticles.

  13. Synthesis and electro-magnetic properties of flower-like Fe2O3-Ag nanocomposite using direct subsidence loading method

    NASA Astrophysics Data System (ADS)

    Zhou, Xing; Wu, Zhengying; Xu, Nan; Liu, Shouqing; Zhao, Guizhe; Liu, Yaqing

    2015-10-01

    Novel flower-like Fe2O3/Ag nanocomposites were synthesized by a simple direct subsidence loading method. The composition and morphology of the obtained samples were characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high resolution transmission electron microscopy (HRTEM) and selected area electron diffraction (SEAD) techniques. The Ag nanoparticles which loaded on the surface of petals exhibit spherical morphology. Further, the magnetic and electrical conductive properties reveal the well controllable performance. Room temperature magnetic measurement of the flower-like nanocomposites demonstrated its ferromagnetic properties and the saturation magnetization (Ms) decreased from 0.6 to 0.11 emu/g.

  14. HRTEM study of zircon from Eliseev anorthosite complex, Antarctica

    SciTech Connect

    Wirth, R.; Kaempf, H.; Hoehndorf, A.

    1996-12-31

    Zircon-bearing rocks of this study are metamorphic oxide-apatite gabbronorites (OAGN) from the Eliseev Anorthosite Complex, Wohlthat-Massif, East Antarctica. These unusual rocks are strongly enriched in accessory minerals apatite: <10 vol.%; zircon: < 1 vol.. Three steps in the evolution of these rocks are distinguished: a magnetic formation, followed by a granulite facies metamorphism and finally a tectonomagmatic overprint. The zircon crystals of this study are brown colored, up to 12 mm in length and up to 3 mm wide. Petrological investigations show that zircon has formed during the granulite facies event. Optical microscopy and cathodoluminiscence microscopy reveal a rhythmic zoning and many microcracks. The concentrations of uranium and thorium are low (U: 34-89 ppm and Th: 3-9 ppm). The radiation damage by radioactive decay of U and Th is expected to be minor due to the low uranium and thorium content. The investigations were carried out in a Philips CM200 transmission electron microscope. Analytical electron microscopy was performed by energy dispersive analysis (EDAX).

  15. Structural, magnetic and electronic structure properties of Co doped ZnO nanoparticles

    SciTech Connect

    Kumar, Shalendra; Song, T.K.; Gautam, Sanjeev; Chae, K.H.; Kim, S.S.; Jang, K.W.

    2015-06-15

    Highlights: • XRD and HR-TEM results show the single phase nature of Co doped ZnO nanoparticles. • XMCD and dc magnetization results indicate the RT-FM in Co doped ZnO nanoparticles. • Co L{sub 3,2} NEXAFS spectra infer that Co ions are in 2+ valence state. • O K edge NEXAFS spectra show that O vacancy increases with Co doping in ZnO. - Abstract: We reported structural, magnetic and electronic structure studies of Co doped ZnO nanoparticles. Doping of Co ions in ZnO host matrix has been studied and confirmed using various methods; such as X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), energy dispersed X-ray (EDX), high resolution transmission electron microscopy (HR-TEM), Fourier transform infrared spectroscopy (FT-IR), near edge X-ray absorption fine structure (NEXAFS) spectroscopy, magnetic hysteresis loop measurements and X-ray magnetic circular dichroism (XMCD). From the XRD and HR-TEM results, it is observed that Co doped ZnO nanoparticles have single phase nature with wurtzite structure and exclude the possibility of secondary phase formation. FE-SEM and TEM micrographs show that pure and Co doped nanoparticles are nearly spherical in shape. O K edge NEXAFS spectra indicate that O vacancies increase with Co doping. The Co L{sub 3,2} edge NEXAFS spectra revealed that Co ions are in 2+ valence state. DC magnetization hysteresis loops and XMCD results clearly showed the intrinsic origin of temperature ferromagnetism in Co doped ZnO nanoparticles.

  16. Interfacial magnetic coupling between Fe nanoparticles in Fe–Ag granular alloys.

    PubMed

    Alonso, J; Fdez-Gubieda, M L; Sarmiento, G; Chaboy, J; Boada, R; García Prieto, A; Haskel, D; Laguna-Marco, M A; Lang, J C; Meneghini, C; Fernández Barquín, L; Neisius, T; Orue, I

    2012-01-20

    The role of the interface in mediating interparticle magnetic interactions has been analysed in Fe50Ag50 and Fe55Ag45 granular thin films deposited by the pulsed laser deposition technique (PLD). These samples are composed of crystalline bcc Fe (2–4 nm) nanoparticles and fcc Ag (10–12 nm) nanoparticles, separated by an amorphous Fe50Ag50 interface, occupying around 20% of the sample volume, as determined by x-ray diffraction (XRD), x-ray absorption spectroscopy (XAS), and high resolution transmission electron microscopy (HRTEM). Interfacial magnetic coupling between Fe nanoparticles is studied by dc magnetization and x-ray magnetic circular dichroism (XMCD) measurements at the Fe K and Ag L2,3 edges. This paper reveals that these thin films present two magnetic transitions, at low and high temperatures, which are strongly related to the magnetic state of the amorphous interface, which acts as a barrier for interparticle magnetic coupling.

  17. XAS and HR-TEM Analyses of the Nakhlite Hydrothermal Minerals

    NASA Astrophysics Data System (ADS)

    Hicks, L. J.; Bridges, J. C.; Gurman, S. J.

    2012-09-01

    We use Fe-K XANES and EXAFS, with HR-TEM observations, to show that the phyllosilicate minerals found in the Lafayette nakhlite are saponite and serpentine. An increase in ferric/ferrous ratio is identified as part of the hydrothermal activity.

  18. Multislice simulations for in-situ HRTEM studies of nanostructured magnesium hydride at ambient hydrogen pressure.

    PubMed

    Surrey, Alexander; Schultz, Ludwig; Rellinghaus, Bernd

    2017-01-31

    The use of transmission electron microscopy (TEM) for the structural characterization of many nanostructured hydrides, which are relevant for solid state hydrogen storage, is hindered due to a rapid decomposition of the specimen upon irradiation with the electron beam. Environmental TEM allows to stabilize the hydrides by applying a hydrogen back pressure of up to 4.5 bar in a windowed environmental cell. The feasibility of high-resolution TEM (HRTEM) investigations of light weight metals and metal hydrides in such a "nanoreactor" is studied theoretically by means of multislice HRTEM contrast simulations using Mg and its hydride phase, MgH2, as model system. Such a setup provides the general opportunity to study dehydrogenation and hydrogenation reactions at the nanoscale under technological application conditions. We analyze the dependence of both the spatial resolution and the HRTEM image contrast on parameters such as the defocus, the metal/hydride thickness, and the hydrogen pressure in order to explore the possibilities and limitations of in-situ experiments with windowed environmental cells. Such simulations may be highly valuable to pre-evaluate future experimental studies.

  19. HRTEM Study of the Role of Nanoparticles in ODS Ferritic Steel

    SciTech Connect

    Hsiung, L; Tumey, S; Fluss, M; Serruys, Y; Willaime, F

    2011-08-30

    Structures of nanoparticles and their role in dual-ion irradiated Fe-16Cr-4.5Al-0.3Ti-2W-0.37Y{sub 2}O{sub 3} (K3) ODS ferritic steel produced by mechanical alloying (MA) were studied using high-resolution transmission electron microscopy (HRTEM) techniques. The observation of Y{sub 4}Al{sub 2}O{sub 9} complex-oxide nanoparticles in the ODS steel imply that decomposition of Y{sub 2}O{sub 3} in association with internal oxidation of Al occurred during mechanical alloying. HRTEM observations of crystalline and partially crystalline nanoparticles larger than {approx}2 nm and amorphous cluster-domains smaller than {approx}2 nm provide an insight into the formation mechanism of nanoparticles/clusters in MA/ODS steels, which we believe involves solid-state amorphization and re-crystallization. The role of nanoparticles/clusters in suppressing radiation-induced swelling is revealed through TEM examinations of cavity distributions in (Fe + He) dual-ion irradiated K3-ODS steel. HRTEM observations of helium-filled cavities (helium bubbles) preferably trapped at nanoparticle/clusters in dual-ion irradiated K3-ODS are presented.

  20. Surface effects in the magnetic properties of crystalline 3 nm ferrite nanoparticles chemically synthesized

    NASA Astrophysics Data System (ADS)

    Lima, E.; De Biasi, E.; Mansilla, M. Vasquez; Saleta, M. E.; Effenberg, F.; Rossi, L. M.; Cohen, R.; Rechenberg, H. R.; Zysler, R. D.

    2010-11-01

    We have systematically studied the magnetic properties of ferrite nanoparticles with 3, 7, and 11 nm of diameter with very narrow grain size distributions. Samples were prepared by the thermal decomposition of Fe(acac)3 in the presence of surfactants giving nanoparticles covered by oleic acid. High resolution transmission electron microscopy (HRTEM) images and XRD diffraction patterns confirms that all samples are composed by crystalline nanoparticles with the spinel structure expected for the iron ferrite. ac and dc magnetization measurements, as well in-field Mössbauer spectroscopy, indicate that the magnetic properties of nanoparticles with 11 and 7 nm are close to those expected for a monodomain, presenting large MS (close to the magnetite bulk). Despite the crystalline structure observed in HRTEM images, the nanoparticles with 3 nm are composed by a magnetically ordered region (core) and a surface region that presents a different magnetic order and it contains about 66% of Fe atoms. The high saturation and irreversibility fields in the M(H ) loops of the particles with 3 nm together with the misalignment at 120 kOe in the in-field Mössbauer spectrum of surface component indicate a high surface anisotropy for the surface atoms, which is not observed for the core. For T <10 K, we observe an increase in the susceptibility and of the magnetization for former sample, indicating that surface moments tend to align with applied field increasing the magnetic core size.

  1. 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

  2. Comparative investigation of NiO nano- and microstructures for structural, optical and magnetic properties

    NASA Astrophysics Data System (ADS)

    Manikandan, A.; Judith Vijaya, J.; John Kennedy, L.

    2013-03-01

    Nickel oxide (NiO) nano- and microstructures were synthesized by the microwave combustion method (MCM) and the conventional combustion method (CCM) using urea as the fuel. The as-synthesized NiO powders were characterized by X-ray powder diffraction (XRD), high resolution scanning electron microscopy (HR-SEM), high resolution transmission electron microscopy (HR-TEM), energy dispersive X-ray analysis (EDX), diffuse reflectance spectroscopy (DRS), photoluminescence (PL) spectroscopy, Brunauer-Emmett-Teller (BET) analysis and vibrating sample magnetometer (VSM) analysis. The XRD results confirmed the formation of cubic phase NiO. The formation of NiO nano- and microstructures were confirmed by HR-SEM and HR-TEM and their possible formation mechanisms were also proposed. The optical absorption and photoluminescence emissions were determined by DRS and PL spectra respectively. The band gap was measured using the Kubelka-Munk model and it shows 3.36 eV for NiO (MCM) and 2.70 eV for NiO (CCM). The magnetic properties of the synthesized NiO nano- and microstructures were investigated with a vibrating sample magnetometer (VSM) and their hysteresis loops were obtained at room temperature. The relatively high saturation magnetization (21.22 emu/g) of NiO-MCM shows that it is ferromagnetic and low saturation magnetization (7.43 emu/g) of NiO-CCM confirms the superparamagnetic behavior.

  3. HRTEM of microcrystalline opal in chert and porcelanite from the Monterey Formation, California

    SciTech Connect

    Cady, S.L.; Wenk, H.R.; Downing, K.H.

    1996-11-01

    Microcrystalline opal was investigated using low-dose transmission electron microscopy (TEM) methods to identify microstructural characteristics and possible phase-transformation mechanisms that accommodate silica diagenesis. High-resolution TEM (HRTEM) revealed that microcrystalline opal in opal-CT chert (>90 wt% silica) and opal-CT porcelanite (50-90 wt% silica) from the Miocene Monterey Formation of California displays various amounts of structural disorder and coherent and incoherent lamellar intergrowths. Species of microfibrous opal identified by HRTEM in early-formed opal-CT chert include length-slow opal-C and unidimensionally disordered length-slow opal-CT ({open_quotes}lussatite{close_quotes}). These fibers often display a microstructure characterized by an aperiodic distribution of highly strained domains that separate ordered domains located at discrete positions along the direction of the fiber axes. Microfibrous opal occurs as several types of fiber-aggregation forms. TEM revealed that the siliceous matrix in later-formed opal-CT porcelanite consists of equidimensional, nanometer-size opal-CT crystallites and lussatite fibers. Pseudo-orthorhombic tridymite (PO-2) was identified by HRTEM in one sample of opal-CT porcelanite. Burial diagenesis of chert and porcelanite results in the precipitation of opal-C and the epitaxial growth of opal-C domains on opal-CT substrates. Diagenetic maturation of lussatite was identified by TEM in banded opal-CT-quartz chert to occur as a result of solid-state ordering. The primary diagenetic silica phase transformations between noncrystalline opal, microcrystalline opal, and quartz occur predominantly by a series of dissolution-precipitation reactions. However, TEM showed that in banded opal-CT-quartz chert, the epitaxial growth of quartz on microfibrous opal enhances the rate of silica diagenesis.

  4. HRTEM and HAADF-STEM of precipitates at peak ageing of cast A319 aluminium alloy.

    PubMed

    Wiengmoon, Amporn; Pearce, John T H; Chairuangsri, Torranin; Isoda, Seiji; Saito, Hikaru; Kurata, Hiroki

    2013-02-01

    High-resolution transmission electron microscopy (HRTEM) and high-angle annular-dark-field scanning transmission electron microscopy (HAADF-STEM) were applied to investigate the precipitates formed during age hardening at 170±5°C for up to 48h of cast A319 aluminium alloy (Al-4.93wt%Si-3.47wt%Cu). The precipitates at the peak-aged condition have been identified as mainly θ" together with a smaller amount of θ'. It is proposed that the θ" is responsible for hardening at peak ageing at 170°C of the cast A319 aluminium alloy.

  5. Influence of total beam current on HRTEM image resolution in differentially pumped ETEM with nitrogen gas.

    PubMed

    Bright, A N; Yoshida, K; Tanaka, N

    2013-01-01

    Environmental transmission electron microscopy (ETEM) enables the study of catalytic and other reaction processes as they occur with Angstrom-level resolution. The microscope used is a dedicated ETEM (Titan ETEM, FEI Company) with a differential pumping vacuum system and apertures, allowing aberration corrected high-resolution transmission electron microscopy (HRTEM) imaging to be performed with gas pressures up to 20 mbar in the sample area and with significant advantages over membrane-type E-cell holders. The effect on image resolution of varying the nitrogen gas pressure, electron beam current density and total beam current were measured using information limit (Young's fringes) on a standard cross grating sample and from silicon crystal lattice imaging. As expected, increasing gas pressure causes a decrease in HRTEM image resolution. However, the total electron beam current also causes big changes in the image resolution (lower beam current giving better resolution), whereas varying the beam current density has almost no effect on resolution, a result that has not been reported previously. This behavior is seen even with zero-loss filtered imaging, which we believe shows that the drop in resolution is caused by elastic scattering at gas ions created by the incident electron beam. Suitable conditions for acquiring high resolution images in a gas environment are discussed. Lattice images at nitrogen pressures up to 16 mbar are shown, with 0.12 nm information transfer at 4 mbar.

  6. HRTEM and EELS study of screw dislocation cores in SrTiO3

    NASA Astrophysics Data System (ADS)

    Zhang, Zaoli; Sigle, Wilfried; Kurtz, Wolfgang

    2004-04-01

    A [100] twist low-angle grain boundary in SrTiO3 was systemically studied by means of conventional transmission electron microscopy, high-resolution transmission electron microscopy (HRTEM), lattice distortion analysis, and electron energy-loss spectroscopy (EELS). A dislocation network is formed in the grain boundary by two sets of a<100> screw dislocations. HRTEM images show that the image contrast in the core region is different from that in the surrounding bulk. Image analysis reveals that compared with an ideal screw dislocation the dislocation core is expanded, probably due to both surface relaxation and a reconstruction of the core. The EELS spectra show a small increase of the Ti/O ratio but no significant change of the Sr/Ti ratio in the core region. From the increase of the Ti/O ratio it is concluded that the dislocation cores are oxygen deficient, which may be responsible for the expansion of the core. Ti L2,3 EELS spectra show a reduction of Ti in the screw dislocation cores as well as a reduced crystal field splitting, both of which are in accordance with a loss of oxygen.

  7. Structural and Magnetic Response in Bimetallic Core/Shell Magnetic Nanoparticles

    PubMed Central

    Nairan, Adeela; Khan, Usman; Iqbal, Munawar; Khan, Maaz; Javed, Khalid; Riaz, Saira; Naseem, Shahzad; Han, Xiufeng

    2016-01-01

    Bimagnetic monodisperse CoFe2O4/Fe3O4 core/shell nanoparticles have been prepared by solution evaporation route. To demonstrate preferential coating of iron oxide onto the surface of ferrite nanoparticles X-ray diffraction (XRD), High resolution transmission electron microscope (HR-TEM) and Raman spectroscopy have been performed. XRD analysis using Rietveld refinement technique confirms single phase nanoparticles with average seed size of about 18 nm and thickness of shell is 3 nm, which corroborates with transmission electron microscopy (TEM) analysis. Low temperature magnetic hysteresis loops showed interesting behavior. We have observed large coercivity 15.8 kOe at T = 5 K, whereas maximum saturation magnetization (125 emu/g) is attained at T = 100 K for CoFe2O4/Fe3O4 core/shell nanoparticles. Saturation magnetization decreases due to structural distortions at the surface of shell below 100 K. Zero field cooled (ZFC) and Field cooled (FC) plots show that synthesized nanoparticles are ferromagnetic till room temperature and it has been noticed that core/shell sample possess high blocking temperature than Cobalt Ferrite. Results indicate that presence of iron oxide shell significantly increases magnetic parameters as compared to the simple cobalt ferrite. PMID:28335200

  8. Microstructure and magnetic behavior of Cu-Co-Si ternary alloy synthesized by mechanical alloying and isothermal annealing

    NASA Astrophysics Data System (ADS)

    Chabri, Sumit; Bera, S.; Mondal, B. N.; Basumallick, A.; Chattopadhyay, P. P.

    2017-03-01

    Microstructure and magnetic behavior of nanocrystalline 50Cu-40Co-10Si (at%) alloy prepared by mechanical alloying and subsequent isothermal annealing in the temperature range of 450-650 °C have been studied. Phase evolution during mechanical alloying and isothermal annealing is characterized by X-ray diffraction (XRD), differential thermal analyzer (DTA), high resolution transmission electron microscopy (HRTEM) and magnetic measurement. Addition of Si has been found to facilitate the metastable alloying of Co in Cu resulting into the formation of single phase solid solution having average grain size of 9 nm after ball milling for 50 h duration. Annealing of the ball milled alloy improves the magnetic properties significantly and best combination of magnetic properties has been obtained after annealing at 550 °C for 1 h duration.

  9. TEM and HRTEM of Soot-in-oil particles and agglomerates from internal combustion engines

    NASA Astrophysics Data System (ADS)

    Fay, M. W.; La Rocca, A.; Shayler, P. J.

    2014-06-01

    Over time, the performance of lubricating oil in a diesel engine is affected by the build-up of carbon soot produced by the combustion process. TEM and HRTEM are commonly used to investigate the characteristics of individual and agglomerated particles from diesel exhaust, to understand the structure and distribution of the carbon sheets in the primary particles and the nanostructure morphology. However, high resolution imaging of soot-in-oil is more challenging, as mineral oil is a contaminant for the electron microscope and leads to instability under the electron beam. In this work we compare solvent extraction and centrifugation techniques for removing the mineral oil contaminant, and the effect on particle size distribution.

  10. Mutual transformation between crystalline phases in silicon after treatment in a planetary mill: HRTEM studies.

    PubMed

    Kulnitskiy, Boris; Annenkov, Mikhail; Perezhogin, Igor; Popov, Mikhail; Ovsyannikov, Danila; Blank, Vladimir

    2016-10-01

    High-resolution transmission electron microscopy (HRTEM) studies of silicon after treatment in a planetary mill have been performed. It is shown that along with the initial phase of silicon, Si-I, the sample also contains some high-pressure phases: Si-III (Kasper phase) and Si-IV (lonsdaleite). We studied the orientation relationship between the particles of different phases, finding that there are, in general, two mechanisms of formation of Si-IV: (1) through the stacking faults formation; (2) through the transformation first to the Kasper phase (Si-III), and then from the Kasper phase to Si-IV. Estimations of temperature and pressure conditions in the planetary ball mill made previously are in accordance with the conditions of formation of the above-mentioned phases.

  11. Characterization of boron doped diamond-like carbon film by HRTEM

    NASA Astrophysics Data System (ADS)

    Li, X. J.; He, L. L.; Li, Y. S.; Yang, Q.; Hirose, A.

    2015-12-01

    Boron doped diamond-like carbon (B-DLC) film was synthesized on silicon (1 0 0) wafer by biased target ion beam deposition. High-resolution transmission electron microscopy (HRTEM) is employed to investigate the microstructure of the B-DLC thin film in cross-sectional observation. Many crystalline nanoparticles randomly dispersed and embedded in the amorphous matrix film are observed. Through chemical compositional analysis of the B-DLC film, some amount of O element is confirmed to be contained. And also, some nanoparticles with near zone axes are indexed, which are accordance with B2O phase. Therefore, the contained O element causing the B element oxidized is proposed, resulting in the formation of the nanoparticles. Our work indicates that in the B-DLC film a significant amount of the doped B element exists as boron suboxide nanoparticles.

  12. Magnetic properties of nanosized Mg0.5Mn0.5(RE)0.1Fe1.9O4 ferrites synthesized by glycol-thermal method

    NASA Astrophysics Data System (ADS)

    Abdallah, Hafiz M. I.; Moyo, T.; Msomi, J. Z.

    2013-04-01

    Nanosized Mg0.5Mn0.5(RE)0.1Fe1.9O4 ferrites, where RE are the rare earth elements, have been synthesized by the glycol-thermal method from pure metal chlorides. The as-prepared samples in the form of powders were characterized by X-ray diffraction (XRD) and high-resolution transmission electron microscopy (HRTEM). The XRD and HRTEM data show formation of the single-phase cubic spinel structure. The grain sizes are found in the range 9-15 nm. Magnetic properties of the as-prepared samples were obtained at room temperature by 57Fe-Mössbauer spectroscopy and by a vibrating sample magnetometer. The distributions of Fe3+ ions were also deduced from Mössbauer measurements. The variations of grain size, lattice parameter, coercive field, magnetizations are presented as a function of the number of (RE)3+ 4f electrons. Our results show the evidence for superparamagnetic behavior of the rare earth substituted compounds. The highest grain size and magnetizations are obtained for the Gd substituted sample. We also find strong correlation of the saturation magnetizations, grain sizes and microstrains with the de Gennes factor.

  13. Synthesis and characterization of Ni0.5Zn0.4Cu0.1Fe2O4 as a magnetic feeder for electromagnetic transmitter application

    NASA Astrophysics Data System (ADS)

    Shafie, Afza; Pransisco, Prengki; Guan, Beh Hoe; Annur, Robithoh

    2016-11-01

    Material ferrites with composition Ni0.5Zn0.4Cu0.1Fe2O4 has been successfully synthesized through sol gel method in difference calcination temperature 600 °C, 700 °C, 800 °C and 900 °C respectively. The temperatures calcination of the material was obtained from thermo-gravimetric analysis (TGA) results. Phase and crystallite size of material were investigated using X-Ray diffraction (XRD). Microstructure, shape and distribution particles of Ni0.5Zn0.4Cu0.1Fe2O4 were examined using high resolution transmission electron microscopy (HRTEM). Magnetic properties were investigated using vibrating sample magnetometer (VSM). Initial permeability and magnetic loss factor were examined by impedance analyzer. Computer simulation technique (CST) was used to simulate electromagnetic transmitter (antenna) with magnetic feeder. The thermo-gravimetric analysis result shows that the total weight loss of Ni0.5Zn0.4Cu0.1Fe2O4 was completed at temperature 572 °C. XRD result shows single phase and no secondary phase was detected and it has a variation of crystallite size in the range of 0.2 to 1.3 nm. The HRTEM result exhibits microstructure particle in interval value of 46-89 nm with agglomeration shape. The highest magnetic saturation was founded at highest calcination temperature 900 °C. The Initial permeability and relative loss factor of the material were 187 and 0.03 respectively. Electromagnetic transmitter with magnetic feeder Ni0.5Zn0.4Cu0.1Fe2O4 exhibits magnitude of magnetic field 1.03×10-6 tesla, which is higher as compared to the transmitter without magnetic feeder with magnitude magnetic field 8.4×10-14 Tesla.

  14. TEM and HRTEM studies of ball milled 6061 aluminium alloy powder with Zr addition.

    PubMed

    Lityńska-Dobrzyńska, L; Dutkiewicz, J; Maziarz, W; Rogal, Ł

    2010-03-01

    The effect of mechanical alloying on the microstructure of atomized 6061 aluminium alloy powder and 6061 powder with a zirconium addition was studied in the work. The atomized 6061 aluminium alloy powder and 6061 powder with addition of 2 wt.% Zr were milled in a planetary ball mill and investigated using X-ray diffraction measurements, conventional and high-resolution electron microscopy (TEM/HRTEM) and high-angle annular dark field scanning transmission electron microscopy combined with energy dispersive X-ray microanalysis. An increase of stresses was observed in milled powders after the refinement of crystallites beyond 100 nm. In the powder with zirconium addition, some part of the Zr atoms diffused in aluminium forming a solid solution containing up to 0.5 wt.% Zr. The remaining was found to form Zr-rich particles containing up to 88 wt.% Zr and were identified as face centred cubic (fcc) phase with lattice constant a= 0.48 nm. That fcc phase partially transformed into the L1(2) ordered phase. Eighty-hour milling brought an increase of microhardness (measured with Vickers method) from about 50 HV (168 MPa) for the initial 6061 powder to about 170 HV (552 MPa). The addition of zirconium had no influence on the microhardness.

  15. HRTEM Study of Oxide Nanoparticles in K3-ODS Ferritic Steel Developed for Radiation Tolerance

    SciTech Connect

    Hsiung, L; Fluss, M; Tumey, S; Kuntz, J; El-Dasher, B; Wall, M; Choi, W; Kimura, A; Willaime, F; Serruys, Y

    2009-11-02

    Crystal and interfacial structures of oxide nanoparticles and radiation damage in 16Cr-4.5Al-0.3Ti-2W-0.37 Y{sub 2}O{sub 3} ODS ferritic steel have been examined using high-resolution transmission electron microscopy (HRTEM) techniques. Oxide nanoparticles with a complex-oxide core and an amorphous shell were frequently observed. The crystal structure of complex-oxide core is identified to be mainly monoclinic Y{sub 4}Al{sub 2}O{sub 9} (YAM) oxide compound. Orientation relationships between the oxide and the matrix are found to be dependent on the particle size. Large particles (> 20 nm) tend to be incoherent and have a spherical shape, whereas small particles (< 10 nm) tend to be coherent or semi-coherent and have a faceted interface. The observations of partially amorphous nanoparticles and multiple crystalline domains formed within a nanoparticle lead us to propose a three-stage mechanism to rationalize the formation of oxide nanoparticles containing core/shell structures in as-fabricated ODS steels. Effects of nanoparticle size and density on cavity formation induced by (Fe{sup 8+} + He{sup +}) dual-beam irradiation are briefly addressed.

  16. 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.

  17. In-situ synthesis of magnetic (NiFe{sub 2}O{sub 4}/CuO/FeO) nanocomposites

    SciTech Connect

    Srivastava, Manish; Ojha, Animesh K.; Chaubey, S.; Singh, Jay

    2010-11-15

    In-situ synthesis of magnetic nanocomposites with (NiFe{sub 2}O{sub 4}/CuO/FeO) crystal phases has been done using a sol-gel method by taking a non-stoichiometric composition of the precursors. The average particle size of the nanocomposites was calculated using X-ray diffraction (XRD) and high resolution tunneling electron microscope (HR-TEM) and it turns out to be {approx}20 nm. The vibrating sample magnetometer (VSM) measurements demonstrate the ferromagnetic nature of the nanocomposites. The synthesized nanocomposite was used to prepare magnetic fluid using tetramethylammonium hydroxide as a surfactant and its stability in the solution was also discussed. -- Graphical abstract: Magnetic nanocomposites containing (NiFe{sub 2}O{sub 4}/CuO/FeO) phases having particle size {approx}17 nm were synthesized by a sol-gel method. The synthesized nanocomposites exhibit ferromagnetic nature with small value of coercivity.

  18. Synthesis, Characterization and Studies on Optical, Dielectric and Magnetic Properties of undoped and Cobalt doped Nanocrystalline Bismuth Ferrite

    NASA Astrophysics Data System (ADS)

    Sarkar, K.; Mukherjee, Soumya; Mukherjee, S.; Mitra, M. K.

    2014-10-01

    Multiferroic perovskite nanocrystalline Bismuth ferrite (BFO) and Co doped Bismuth ferrite are synthesized by chemical route annealed at 500, 550 and 600 °C. XRD studies revealed the phases formed during synthesis while crystallite size is calculated in the range of 15.4-55 nm by Scherrer's formula from the identified XRD major peaks. The FTIR spectra of undoped BFO sample synthesized at 500, 550 and 600 °C exhibits clear presence of peaks at 554 cm-1 confirms the existence of Bi-O, Fe-O stretching and bending behavior of two different M-O co-ordination using Shimadzu-8400S Spectroscopy. The microstructure, lattice image and interplanar spacing are obtained by HRTEM analysis. The particle sizes are also measured from HRTEM while the chemistry is verified by energy dispersive x-ray analysis (EDX) (Oxford Instruments, INCA). Dielectric properties are observed for both undoped and Co doped samples. The band gap energy is measured by UV-VIS characterization using Tauc equation. Magnetic measurements are carried out using Physical Properties Measurement systems.

  19. HRTEM study of track evolution in 120-MeV U irradiated Gd2Ti2O7

    SciTech Connect

    Jozwik Biala, Iwona; Jagielski, Jacek K.; Thome, Lionel; Arey, Bruce W.; Kovarik, Libor; Sattonay, G.; Debelle, A.; Monnet, I.

    2012-09-01

    High resolution Scanning Transmission Electron Microscopy (HRTEM) experiments were performed on Gd2Ti2O7 pyrochlores irradiated with 120-MeV U ions. A judicious choice of irradiation energy, sample preparation (using Focused Ion Beam) and analytical technique (HRTEM) allowed us to visualize the complete evolution of tracks from the surface of samples down to depths exceeding the projected range of irradiating ions. Such features as variation of track diameters, changes in track directions and discontinuous segments of tracks were clearly documented at various depths. By using two different STEM imaging modes: High- and Low-Angle Annular Dark Field imaging (HAADF and LAADF), it was possible to observe the layered structure of tracks composed of an amorphous core surrounded by a strained crystalline envelope.

  20. Structural and chemical characterization of Yb2O3-ZrO2 system by HAADF-STEM and HRTEM.

    PubMed

    Angeles-Chavez, C; Salas, P; Díaz-Torres, L A; de la Rosa, E; Esparza, R; Perez, R

    2009-02-01

    ZrO2:Yb3+ nanocrystalline phosphors with high concentrations of ytterbium ions were prepared using the sol-gel method. X-ray diffraction, high-angle annular-dark-field scanning transmission electron microscopy (HAADF-STEM), energy dispersive X-ray spectroscopy, and high-resolution transmission electron microscopy (HRTEM) were used to characterize the nanocrystalline phosphors annealed at 1000 degrees C. Unit-cell distortion and changes in the crystalline structure of the monoclinic zirconia to tetragonal zirconia, and subsequently cubic zirconia, were observed with increased Yb concentration. Yb ions were randomly distributed into the lattice of the crystalline structure. No segregation of Yb2O3 phase was observed. The substitution of Zr atoms by Yb atoms on different crystalline phases was confirmed by the experimental results and theoretical simulations of HRTEM and HAADF-STEM.

  1. 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.

  2. A facile hydrothermal synthesis, characterization and magnetic properties of mesoporous CoFe2O4 nanospheres

    NASA Astrophysics Data System (ADS)

    Reddy, M. Penchal; Mohamed, A. M. A.; Zhou, X. B.; Du, S.; Huang, Q.

    2015-08-01

    Mesoporous CoFe2O4 nanospheres with an average size of 180 nm were fabricated via a facile hydrothermal process using ethylene glycol as solvent and sodium acetate (NaAc) as electrostatic stabilizer. In this method, ethylene glycol plays a vital role in the formation of cobalt nanoospheres as a solvent and reducing agent. The structure and morphology of the prepared materials were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high-resolution TEM (HRTEM), Fourier transform infrared spectroscopy (FTIR) and X-ray photoelectron spectroscopy (XPS). The nanospheres exhibited ferromagnetic properties with high saturation magnetization value of about 60.19 emu/g at room temperature. The BET surface area of the nanospheres was determined using the nitrogen absorption method. The porous CoFe2O4 nanospheres displayed good magnetic properties, which may provide a very promising candidate for their applications in target drug delivery.

  3. Aloe vera plant-extracted solution hydrothermal synthesis and magnetic properties of magnetite (Fe3O4) nanoparticles

    NASA Astrophysics Data System (ADS)

    Phumying, Santi; Labuayai, Sarawuth; Thomas, Chunpen; Amornkitbamrung, Vittaya; Swatsitang, Ekaphan; Maensiri, Santi

    2013-06-01

    Magnetite (Fe3O4) nanoparticles have been successfully synthesized by a novel hydrothermal method using ferric acetylacetonate (Fe(C5H8O2)3) and aloe vera plant-extracted solution. The influences of different reaction temperatures and times on the structure and magnetic properties of the synthesized Fe3O4 nanoparticles were investigated. The synthesized nanoparticles are crystalline and have particle sizes of ˜6-30 nm, as revealed by transmission electron microscopy (TEM). The results of X-ray diffraction (XRD), High resolution TEM (HRTEM) and selected area electron diffraction (SAED) indicate that the synthesized Fe3O4 nanoparticles have the inverse cubic spinel structure without the presence of any other phase impurities. The hysteresis loops of the Fe3O4 nanoparticles at room temperature show superparamagnetic behavior and the saturation magnetization of the Fe3O4 samples increases with increasing reaction temperature and time.

  4. HRTEM low dose: the unfold of the morphed graphene, from amorphous carbon to morphed graphenes.

    PubMed

    Calderon, H A; Okonkwo, A; Estrada-Guel, I; Hadjiev, V G; Alvarez-Ramírez, F; Robles Hernández, F C

    We present experimental evidence under low-dose conditions transmission electron microscopy for the unfolding of the evolving changes in carbon soot during mechanical milling. The milled soot shows evolving changes as a function of the milling severity or time. Those changes are responsible for the transformation from amorphous carbon to graphenes, graphitic carbon, and highly ordered structures such as morphed graphenes, namely Rh6 and Rh6-II. The morphed graphenes are corrugated layers of carbon with cross-linked covalently nature and sp(2)- or sp(3)-type allotropes. Electron microscopy and numerical simulations are excellent complementary tools to identify those phases. Furthermore, the TEAM 05 microscope is an outstanding tool to resolve the microstructure and prevent any damage to the sample. Other characterization techniques such as XRD, Raman, and XPS fade to convey a true identification of those phases because the samples are usually blends or mixes of the mentioned phases.

  5. The chaotic points and XRD analysis of Hg-based superconductors

    NASA Astrophysics Data System (ADS)

    Aslan, Ö.; Güven Özdemir, Z.; Keskin, S. S.; Onbaşli, Ü.

    2009-03-01

    In this article, high Tc mercury based cuprate superconductors with different oxygen doping rates have been examined by means of magnetic susceptibility (magnetization) versus temperature data and X-ray diffraction pattern analysis. The under, optimally and over oxygen doping procedures have been defined from the magnetic susceptibility versus temperature data of the superconducting sample by extracting the Meissner critical transition temperature, Tc and the paramagnetic Meissner temperature, TPME, so called as the critical quantum chaos points. Moreover, the optimally oxygen doped samples have been investigated under both a.c. and d.c. magnetic fields. The related a.c. data for virgin(uncut) and cut samples with optimal doping have been obtained under a.c. magnetic field of 1 Gauss. For the cut sample with the rectangular shape, the chaotic points have been found to occur at 122 and 140 K, respectively. The Meissner critical temperature of 140 K is the new world record for the high temperature oxide superconductors under normal atmospheric pressure. Moreover, the crystallographic lattice parameters of superconducting samples have a crucial importance in calculating Josephson penetration depth determined by the XRD patterns. From the XRD data obtained for under and optimally doped samples, the crystal symmetries have been found in tetragonal structure.

  6. Two-phase nc-TiN/a-(C,CNx) nanocomposite films: A HRTEM and MC simulation study

    NASA Astrophysics Data System (ADS)

    Guo, J.; Lu, Y. H.; Hu, X. J.; Shen, Y. G.

    2013-06-01

    The grain growth in two-phase nanocomposite Ti-Cx-Ny thin films grown by reactive close-field unbalanced magnetron sputtering in an Ar-N2 gas mixture with microstructures comprising of nanocrystalline (nc-) Ti(N,C) phase surrounded by amorphous (a-) (C,CNx) phase was investigated by a combination of high-resolution transmission electron microscopy (HRTEM) and Monte Carlo (MC) simulations. The HRTEM results revealed that amorphous-free solid solution Ti(C,N) thin films exhibited polycrystallites with different sizes, orientations and irregular shapes. The grain size varied in the range between several nanometers and several decade nanometers. Further increase of C content (up to ˜19 at.% C) made the amorphous phase wet nanocrystallites, which strongly hindered the growth of nanocrystallites. As a result, more regular Ti(C,N) nanocrystallites with an average size of ˜5 nm were found to be separated by ˜0.5-nm amorphous phases. When C content was further increased (up to ˜48 at.% in this study), thicker amorphous matrices were produced and followed by the formation of smaller sized grains with lognormal distribution. Our MC analysis indicated that with increasing amorphous volume fraction (i.e. increasing C content), the transformation from nc/nc grain boundary (GB)-curvature-driven growth to a/nc GB-curvature-driven growth is directly responsible for the observed grain growth from great inhomogeneity to homogeneity process.

  7. IMAGE-WARP: a real-space restoration method for high-resolution STEM images using quantitative HRTEM analysis.

    PubMed

    Recnik, Aleksander; Möbus, Günter; Sturm, Saso

    2005-07-01

    We have developed a new method for processing distorted high-resolution scanning transmission electron microscopy (STEM) images. The method is based on finding the displaced vertices in the experimental STEM image and warping to geometrically correct reference grid of the object. As a reference grid for warping a structural model obtained using a high-resolution transmission electron microscopy (HRTEM) analysis of the area of interest is utilised. Combined with quantitative HRTEM analysis the IMAGE-WARP method provides a real-space restoration of high-resolution high-angle annular dark-field (HAADF) STEM images without affecting the original Z-contrast information. The method can be applied to extract valuable compositional atomic-column data from any HAADF-STEM image of any kind of bulk crystals with local occupancy or chemistry fluctuations, stacking faults, special grain boundaries or interfaces, for which we have an available structural model. After the warping, distortion-corrected images can be further enhanced using conventional image-filtering techniques, and finally quantified with HAADF-STEM image simulations. The applicability of the IMAGE-WARP method was illustrated using experimental HAADF-STEM images of a strontium titanate crystal disrupted with a Ruddlesden-Popper-type antiphase boundary.

  8. Advancements in the characterization of 'hyper-thin' oxynitride gate dielectrics through exit wave reconstruction HRTEM and XPS

    SciTech Connect

    Principe, E.L.; Watson, D.G.; Kisielowski, C.

    2002-09-01

    The physical thickness of silicon oxynitride gate dielectric materials currently in development have dimensions in the range of 15-20 Angstrom ({approx}6-8 oxygen atoms), while approaching the dielectric constant equivalent oxide thickness (EOT) of 12 Angstrom silicon dioxide. These structures present serious challenges in meeting stringent requirements within the semiconductor industry for precise determination of thickness, interfacial roughness and chemical distribution. Limitations in conventional HRTEM must be removed that would minimize errors in such measurements. Our approach was to use the National Center for Electron Microscopy (NCEM) One Angstrom Microscope (O Angstrom M), together with focal series acquisition (FSA) and exit wave reconstruction (EWR) techniques to obtain <0.8A interpretable resolution. HRTEM data on the same oxynitride materials from an aberration corrected (Cs=0) microscope were also collected as part of this work, as were scanning TEM (STEM) measurements. The H RTEM characterization provides an absolute calibration and validation for a precise ''near-line'' metrology to determine gate oxide thickness and nitrogen dose using x-ray photoelectron spectroscopy (XPS).

  9. Investigation of the Distribution of Fission Products Silver, Palladium and Cadmium in Neutron Irradiated SIC using a Cs Corrected HRTEM

    SciTech Connect

    I. J. van Rooyen; E. Olivier; J. H Neethlin

    2014-10-01

    Electron microscopy examinations of selected coated particles from the first advanced gas reactor experiment (AGR-1) at Idaho National Laboratory (INL) provided important information on fission product distribution and chemical composition. Furthermore, recent research using STEM analysis led to the discovery of Ag at SiC grain boundaries and triple junctions. As these Ag precipitates were nano-sized, high resolution transmission electron microscopy (HRTEM) examination was used to provide more information at the atomic level. This paper describes some of the first HRTEM results obtained by examining a particle from Compact 4-1-1, which was irradiated to an average burnup of 19.26% fissions per initial metal atom (FIMA), a time average, volume-averaged temperature of 1072°C; a time average, peak temperature of 1182°C and an average fast fluence of 4.13 x 1021 n/cm2. Based on gamma analysis, it is estimated that this particle may have released as much as 10% of its available Ag-110m inventory during irradiation. The HRTEM investigation focused on Ag, Pd, Cd and U due to the interest in Ag transport mechanisms and possible correlation with Pd, Ag and U previously found. Additionally, Compact 4-1-1 contains fuel particles fabricated with a different fuel carrier gas composition and lower deposition temperatures for the SiC layer relative to the Baseline fabrication conditions, which are expected to reduce the concentration of SiC defects resulting from uranium dispersion. Pd, Ag, and Cd were found to co-exist in some of the SiC grain boundaries and triple junctions whilst U was found to be present in the micron-sized precipitates as well as separately in selected areas at grain boundaries. This study confirmed the presence of Pd both at inter- and intragranular positions; in the latter case specifically at stacking faults. Small Pd nodules were observed at a distance of about 6.5 micron from the inner PyC/SiC interface.

  10. Diagenetic Microcrystalline Opal Varieties from the Monterey Formation, CA: HRTEM Study of Structures and Phase Transformation Mechanisms

    NASA Technical Reports Server (NTRS)

    Cady, Sherry L.; Wenk, H.-R.; DeVincenzi, Don (Technical Monitor)

    1994-01-01

    Microcrystalline opal varieties form as intermediary precipitates during the diagenetic transformation of biogenically precipitated non-crystalline opal (opal-A) to microquartz. With regard to the Monterey Formation of California, X-ray powder diffraction studies have shown that a decrease in the primary d-spacing of opal-CT toward that of cristobalite occurs with increasing diagenesis. The initial timing of opal-CT/quartz formation and the value of the primary opal-CT d-spacing, are influenced by the sediment. lithology. Transmission electron microscopy methods (CTEM/HRTEM) were used to investigate the structure of the diagenetic phases and establish transformation mechanisms between the varieties of microcrystalline opals in charts and porcelanites from the Monterey Formation. HRTEM images revealed that the most common fibrous varieties of microcrystalline opals contain varying amounts of structural disorder. Finite lamellar units of cristobalite-and tridymite-type. layer sequences were found to be randomly stacked in a direction perpendicular to the fiber axis. Disordered and ordered fibers were found to have coprecipitated within the same radial fiber bundles that formed within the matrix of the Most siliceous samples. HRTEM images, which reveal that the fibers within radial and lepispheric fiber bundles branch non-crystallographically, support an earlier proposal that microspheres in chert grow via a spherulitic growth mechanism. A less common variety of opal-CT was found to be characterized by non-parallel (low-angle) stacking sequences that often contain twinned lamellae. Tabular-shaped crystals of orthorhombic tridymite (PO-2) were also identified in the porcelanite samples. A shift in the primary d-spacing of opal-CT has been interpreted as an indication of solid-state ordering g toward a predominantly cristobalite structure, (opal-C). Domains of opal-C were identified as topotactically-oriented overgrowths on discrete Sections of opal-CT fibers and as

  11. Preparation, microstructure and magnetic properties of Sm(Co,Hf)7/Co nanocomposite particles by polyol method

    NASA Astrophysics Data System (ADS)

    Bu, Shao-Jing; Duan, Xiu-Li; Han, Xu-Hao; Sun, Ji-Bing; Chi, Xiang; Cui, Chun-Xiang

    2017-02-01

    Hard/soft Sm-Co/Co nanocomposite particles were prepared by reducing CoCl2·6H2O in the solution containing ball-milled Sm(Co, Hf)7 particles by a simple polyol method with ethylene glycol as the solvent. Phase composition, microstructure and magnetic properties of the particles were analyzed by XRD, TEM (HRTEM) and VSM, respectively. It has been found that Sm-Co/Co core/shell structure is formed in which the Co shell is 3-5 nm in thickness and mainly exists in hcp-Co phase. At the same time, fcc-Co tends to nucleate and grow independently between Sm-Co particles. The formation mechanism of Sm-Co/Co composite particles is discussed and corresponding model is established. Sm-Co/Co composite particles perform obvious remanence enhancement effects especially after being heated at 450 °C for 15 min

  12. Influence of Fe doping on the structural, optical and magnetic properties of ZnS diluted magnetic semiconductor

    NASA Astrophysics Data System (ADS)

    Saikia, D.; Raland, RD.; Borah, J. P.

    2016-09-01

    Fe doped ZnS nanoparticles with different concentrations of Fe, synthesized by microwave assisted co-precipitation method have been reported. The incorporation of Fe2+ and Fe3+ ions into ZnS lattice are confirmed by X-ray diffraction (XRD) and Electron Paramagnetic resonance (EPR) study. XRD and High Resolution Transmission electron Microscope (HRTEM) results confirm the phase purity of the samples and indicate a reduction of the particle size with increase in Fe concentration. EDAX analysis confirms the presence of Zn, S and Fe in the samples. A yellow-orange emission peak is observed in Photoluminescence (PL) spectra which exhibits the Characteristic 4T2 (4G)-6A1 (6S) transition of Fe3+ ion. The room temperature magnetic studies as analyzed from M-H curves were investigated from vibrating samples magnetometer (VSM) which shows a weak ferro and superparamagnetic like behavior in 1% and 3% Fe-doped ZnS nanocrystals, whereas; at 10% Fe-doping concentrations, antiferromagnetism behavior is achieved. The ZFC-FC measurement reveals that the blocking temperature of the nanoparticle is above the room temperature.

  13. PIXE, SR-XRD and EXAFS analysis of Cu-doped ZnO films

    NASA Astrophysics Data System (ADS)

    Zhang, B.; Yang, C.; Wang, J. Z.; Shi, L. Q.; Cheng, H. S.

    2014-08-01

    Cu-doped ZnO films were prepared by rf magnetron sputtering on sapphire substrate at different atmosphere. Microstructure of these films and Cu occupation sites were investigated using PIXE, SR-XRD and EXAFS. Only 2.9 at.% Cu, no other magnetic impurities (e.g., Fe, Co and Ni) were detected. The ZnO:Cu films possessed the wurtzite ZnO structures and no precipitates (e.g., CuO and Cu2O or Cu cluster) were found. Cu atoms were incorporated into ZnO crystal lattice by occupying Zn atomic sites.

  14. Room temperature magnetic ordering, enhanced magnetization and exchange bias of GdMnO3 nanoparticles in (GdMnO3)0.70(CoFe2O4)0.30

    NASA Astrophysics Data System (ADS)

    Mitra, A.; Mahapatra, A. S.; Mallick, A.; Chakrabarti, P. K.

    2017-02-01

    Nanoparticles of GdMnO3 (GMO) are prepared by sol-gel method. To enhance the magnetic property and also to obtain the magnetic ordering at room temperature (RT), nanoparticles of GMO are incorporated in the matrix of CoFe2O4 (CFO). Desired crystallographic phases of CFO, GMO and GMO-CFO are confirmed by analyzing X-ray diffractrograms (XRD) using Rietveld method. The average size of nanoparticles and their distribution, crystallographic phase, nanocrystallinity etc. are studied by high-resolution transmission electron microscope (HRTEM). Magnetic hysteresis loops (M-H) of GMO-CFO under zero field cooled (ZFC) and field cooled (FC) conditions are observed at different temperatures down to 5 K. Magnetization vs. temperature (M-T) under ZFC and FC conditions are also recorded. Interestingly, exchange bias (EB) is found at low temperature which suggests the encapsulation of the ferromagnetic (FM) nanoparticles of GMO by the ferrimagnetic nanoparticles of CFO below 100 K. Enhanced magnetization, EB effect and RT magnetic ordering of GMO-CFO would be interesting for both theoretical and experimental investigations.

  15. CONDENSED MATTER: ELECTRONIC STRUCTURE, ELECTRICAL, MAGNETIC, AND OPTICAL PROPERTIES: Structures and magnetic anisotropy of β-Mn2V2O7 crystals synthesized by the molten salt method

    NASA Astrophysics Data System (ADS)

    Zhou, Chuan-Cang; Liu, Fa-Min; Ding, Peng

    2009-11-01

    β-Mn2V2O7 crystals with strip shape are successfully prepared by the molten salt method in a closed crucible, and are characterized by x-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), selected area of electron diffraction (SAED) and high-resolution transmission electron microscopy (HRTEM). The results indicate that the sample is of the β-Mn2V2O7 crystal with monoclinic symmetry, level natural cleavage facets and directional growth. Magnetic properties are measured by vibration sample magnetometry (VSM) at room temperature, and the magnetic hysteresis loop indicates that the β-Mn2V2O7 has anti-ferromagnetic properties with low coercive force and remnant magnetization. The magnetic measurement results in different directions exhibit that the β-Mn2V2O7 has magnetic anisotropy, which is due to the fact that the magnetic interaction energy of the β-Mn2V2O7 is lowest only when the electron configuration is in a certain direction.

  16. 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.

  17. Extraordinary high dielectric constant, electrical and magnetic properties of ferrite nanoparticles at room temperature

    NASA Astrophysics Data System (ADS)

    Batoo, Khalid Mujasam; Mir, Feroz Ahmed; Abd El-sadek, M.-S.; Shahabuddin, Md.; Ahmed, Niyaz

    2013-11-01

    Nanoparticles of spinel ferrites of basic composition Ni1- x Co x Fe2O4 (0.0 ≤ x ≤ 0.05) were synthesized through modified co-precipitation method, and were characterized for structural, transport electrical and magnetic properties using XRD, HRTEM, FTIR, LCR meter and VSM techniques, respectively. XRD analysis showed that all the samples are single-phase cubic spinel in structure. The average crystallite sizes of the nanoparticles were found between 30 nm to 45 nm. Real and imaginary parts of the impedance ( Z' and Z″) suggested coexistence of two relaxation regimes: one was introduced by electrode polarization, while the other was attributed to the coeffect of grain and grain boundary effects. The dielectric constant of the samples was found very high, which showed non-Debye relaxation phenomena, while conductivity of the samples exhibited a two-segment behavior with frequency. The room temperature M-H curves suggested that the samples exhibit supermagnetism, and the saturation magnetization increases with increasing Co2+ ion substitution.

  18. HRTEM investigations between minerals, fluids and lithobiontic communities during natural weathering. Progress report, September 1, 1993--February 28, 1994

    SciTech Connect

    Banfield, J.F.; Barker, W.W.

    1994-02-01

    HRTEM and AEM analysis of riebeckite and acmite from the interiors of moderately weathered syenite reveals that interaction of these minerals with surficial fluids resulted in the almost complete removal of Na, Ca, and Si. Fe remained relatively immobile, forming arrays of semi-oriented nanocrystalline ferrihydrite and goethite at the primary mineral-secondary mineral interface. The goethite intimately contacts an irregularly corroded amphibole surface. Smectite occurs sporadically as isolated crystallites a few layers thick which are surrounded by goethite. No obvious structural alignment between clay and amphibole or pyroxene was seen. Data suggest that almost all Si is transported in solution to more open regions between islands of nanocrystalline goethite, where it crystallizes as an Fe - rich smectite. Alteration assemblages in wider channels are comprised of euhedral goethite crystals that, within a submicron-sized area, range in size from 5--40 manometers. Sub-grain boundary structures and the porosity distribution suggests evolution of particle size by coarsening. Optical microscopy demonstrates intimate contact between lichen thalli and mineral surfaces. Lichen thalli exploit cracks and open cleavages to extend several millimeters within mineral interiors. Preliminary TEM data suggest the alteration assemblage consists of a polymer-bound mass of chemically complex aluminosilicates.

  19. In-situ HRTEM study of the reactive carbide phase of Co/MoS2 catalyst.

    PubMed

    Ramos, Manuel; Ferrer, Domingo; Martinez-Soto, Eduan; Lopez-Lippmann, Hugo; Torres, Brenda; Berhault, Gilles; Chianelli, Russell R

    2013-04-01

    Hydrotreatment catalytic operations are commonly performed industrially by layered molybdenum sulfide promoted by cobalt or nickel in order to remove heteroelements (S, N, O) from fossil fuels and biofuels. Indeed, these heteroelements are responsible of the emission of pollutants when these fuels are used in vehicles. In this respect, previous studies made by our research group have shown that the active phase under steady state conditions is partially carbided while strong bending effects of MoS2 slabs were also observed. However, up to now, the morphology of the resulting Co/MoSxCy carbided catalyst has not been fully characterized. In the present study, for the first time, a chemical reaction between the carbon content of a TEM Cu/C grid and a freshly sulfide Co/MoS2 catalyst was in situ observed at 300 °C and 450 °C by HRTEM experimental techniques at ~10 nm of resolution. Results indicate that bending of MoS2 layers occurred due to carbon addition on MoS2 edge sites, as observed in stabilized catalysts after HDS reaction. Using a silicon grid, only cracks of MoS2 slabs were observed without bending effect confirming the role of structural-carbon in this change of morphology.

  20. Seed-mediated synthesis, properties and application of {gamma}-Fe{sub 2}O{sub 3}-CdSe magnetic quantum dots

    SciTech Connect

    Lin, Alex W.H.; Ang, Chung Yen; Patra, Pranab K.; Han Yu; Gu Hongwei; Le Breton, Jean-Marie; Juraszek, Jean; Chiron, Hubert; Papaefthymiou, Georgia C.; Tamil Selvan, Subramanian; Ying, Jackie Y.

    2011-08-15

    Seed-mediated growth of fluorescent CdSe quantum dots (QDs) around {gamma}-Fe{sub 2}O{sub 3} magnetic cores was performed at high temperature (300 deg. C) in the presence of organic surfactants. Bi-functional magnetic quantum dots (MQDs) with tunable emission properties were successfully prepared. The as-synthesized MQDs were characterized by high-resolution transmission electron microscopy (HRTEM) and dynamic light scattering (DLS), which confirmed the assembly of heterodimers. When a longer growth period was employed, a homogeneous dispersion of QDs around a magnetic nanoparticle was obtained. The magnetic properties of these nanocomposites were examined. The MQDs were superparamagnetic with a saturation magnetization of 0.40 emu/g and a coercivity of 138 Oe at 5 K. To demonstrate their potential application in bio-labeling, these MQDs were coated with a thin silica shell, and functionalized with a polyethylene glycol (PEG) derivative. The functionalized MQDs were effectively used for the labeling of live cell membranes of 4T1 mouse breast cancer cells and HepG2 human liver cancer cells. - Graphical abstract: (a) HRTEM image of oleic acid capped MPs. The size of MPs ranges from 8 to 10 nm. (b) XRD pattern of {gamma}-Fe{sub 2}O{sub 3} MPs. Highlights: > The fabrication of MQDs through a seed-mediated approach has been demonstrated. > The formation and assembly of these bi-functional nanocomposites have been elucidated. > The MQDs exhibit superparamagnetism and tunable emissions characteristic of the components. > MQDs with thin silica coating were successfully employed in the labeling of cancer cell membranes.

  1. Nanostructure investigation of magnetic nanomaterial Ni{sub 0.5}Zn{sub 0.3}Cu{sub 0.2}Fe{sub 2}O{sub 4} synthesized by sol-gel method

    SciTech Connect

    Pransisco, Prengki; Shafie, Afza Guan, Beh Hoe

    2015-07-22

    Magnetic nanomaterial Ni{sub 0.5}Zn{sub 0.3}Cu{sub 0.2}Fe{sub 2}O{sub 4} was successfully prepared by using sol-gel method. Heat treatment on material is always giving defect on properties of material. This paper investigates the effect of heat treatment on nanostructure of magnetic nanomaterial Ni{sub 0.5}Zn{sub 0.3}Cu{sub 0.2}Fe{sub 2}O{sub 4}. According to thermo gravimetric analysis (TGA) that after 600°C there is no more weight loss detected and it was decided as minimum calcination temperature. Intensity, crystallite size, structure, lattice parameter and d-spacing of the material were investigated by using X-ray diffraction (XRD). High resolution transmission electron microscope (HRTEM) was used to examine nanostructure, nanosize, shape and distribution particle of magnetic material Ni{sub 0.5}Zn{sub 0.3}Cu{sub 0.2}Fe{sub 2}O{sub 4} and variable pressure field emission scanning electron microscope (VP-FESEM) was used to investigate the surface morphology and topography of the material. The XRD result shows single-phase cubic spinel structure with average crystallite size in the range of 25.6-95.9 nm, the value of the intensity of the material was increased with increasing temperature, and followed by lattice parameter was increased with increasing calcination temperature, value of d-spacing was relatively decreased with accompanied increasing temperature. From HRTEM result the distribution of particles was tend to be agglomerates with particle size of 7.8-17.68 nm. VP-FESEM result shows that grain size of the material increases with increasing calcination temperature and the surface morphology shows that the material is in hexagonal shape and it was also proved by mapping result which showing the presence each of constituents inside the compound.

  2. Structural and magnetic properties of Gd3+ ion substituted magnesium ferrite nanopowders

    NASA Astrophysics Data System (ADS)

    Elkady, Ashraf S.; Hussein, Shaban I.; Rashad, Mohamed M.

    2015-07-01

    Nanocrystalline MgGdxFe2-xO4 powders (where x=0, 0.05, 0.1, 0.2, 0.25, 0.3) have been synthesized by the ethylene diamine tetraacetic acid (EDTA)-based sol-gel combustion method. X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, high resolution transmission electron microscopy (HRTEM) and vibrating sample magnetometer (VSM) were applied in order to study the effect of variation of Gd3+ ion substitution and its impact on crystal structure, crystallite size, lattice parameters, nanostructure and magnetic properties of the formed powders. XRD indicated that, after doping and calcination at 400 °C for 2 h, all samples have two spinel ferrite structures namely cubic and tetragonal phases, which are dependent on Gd3+ ion concentration. The cubic phase is found to increase with increasing the Gd3+ ion molar ratio up to 0.1, compared to pure MgFe2O4 and higher Gd3+ content samples. Indeed, with increasing Gd3+ ion, the crystallite size was almost unchanged whereas the lattice parameter was found to increase. FT-IR spectrum showed broadening of the ν2 band and the presence of another band in the range (465-470 cm-1) upon adding Gd3+ ion, which confirm the presence of Gd3+ ion in addition to Fe3+ ion at octahedral site. Besides, these bands were assigned to the formation of (Gd3+-O2-) complexes at B-sites. HRTEM images showed that the studied samples consist of nanocrystallites having average particle sizes around 9 nm for pure MgFe2O4 up to 27 and 42 nm for the Gd3+ ion substituted MgFe2O4 of molar ratio 0.05 and 0.30, respectively. An examination of the magnetic properties revealed an increase in saturation magnetization with increasing Gd concentration incorporation up to x=0.1, as a result of the change of cubic and tetragonal spinel ratio and lattice parameters. Meanwhile, the formed powders exhibited superparamagnetic characteristics. Therefore, such newly synthesized superparamagnetic nanoparticles, containing Gd3+ ion can be considered as a

  3. Correlating structural, magnetic, and luminescence properties with the cation distribution of Co0.5Zn0.5+xFe2-xO4 nanoferrite

    NASA Astrophysics Data System (ADS)

    Wahba, Adel Maher; Mohamed, Mohamed Bakr; Imam, N. G.

    2016-06-01

    Structural, magnetic, and luminescence properties have been investigated for Co0.5Zn0.5+xFe2-xO4 nanoferrite (0.0≤x≤0.4, with a step increment of 0.1) prepared by citrate autocombustion method. X-ray diffraction (XRD) patterns and Fourier-transform infrared (FTIR) spectra proved the formation of a pure cubic spinel phase for all AP samples. Although the ionic radius of Zn2+ is larger than that of either Fe3+ or Co2+, Rietveld analysis showed that the lattice parameter mostly decreases with increasing Zn substitution. The crystallite size of AP samples decreases gradually with increasing Zn substitution from 16 to 10 nm, which is confirmed with high-resolution (HRTEM) micrographs. Magnetic parameters such as saturation magnetization, coercivity, and remanent field obtained from vibrating sample magnetometry (VSM) revealed a strong dependence on the cation distribution being proposed according to the experimental data of XRD, FTIR, and VSM. The cation distribution indicated that introduced nonstoichiometry is compensated by oxidizing Co2+ into Co3+, which explains the trend of the lattice parameter with increasing x. The distribution of Fe3+ ions between octahedral and tetrahedral sites was further confirmed by photoluminescence (PL) emission spectra.

  4. 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%.

  5. 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

  6. XRD analysis and leachability of solidified phenol-cement mixtures

    SciTech Connect

    Vipulanandan, C.; Krishnan, S. . Department of Civil and Environmental Engineering)

    1993-07-01

    The microstructure and leachability of phenol from solidified phenol-Portland cement mixtures cured up to 6 months were investigated. Phenol was solidified with Type I Portland cement at concentrations of 0.5% and 2% by weight of the cement. XRD studies and pore fluid analyses indicate that phenol inhibits cement setting by reacting with the calcium hydroxide produced during the hydration of cement. Phenol leachability was studied using the Toxicity Characteristic Leaching Procedure (TCLP) test recommended by the U. S. EPA. The quantity of phenol leached is dependent on the initial phenol concentration and the curing time and a simple model has been proposed to predict the leachability. Phenol increases the initial and final setting times of cement. The compressive strength of the solidified cement-phenol mixtures decrease with increasing phenol content in the matrix and increase with curing time. The relationship between leaching of phenol and strength of cement-phenol mixtures has been verified.

  7. High temperature XRD of Cu2GeSe3

    NASA Astrophysics Data System (ADS)

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

    2015-06-01

    The Cu2GeSe3 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 Cu2GeSe3 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.

  8. [Infrared spectroscopy and XRD studies of coral fossils].

    PubMed

    Chen, Quan-li; Zhou, Guan-min; Yin, Zuo-wei

    2012-08-01

    Coral fossil is an old remain of multicellular animal on the earth, and formed by various geological processes. The structural characteristics and compositions of the coral fossils with different color and radial texture on the surface were studied by infrared absorption spectroscopy and X-ray powder diffraction analyses. The results show that the studied coral fossils mainly are composed of SiO2, and the radial microstructure characterized by the calcareous coral cross-section is preserved. It is formed by metasomatism by SiO2. The infrared absorption spectra of the coral fossil with different color and texture are essentially the same, showing typical infrared absorption spectra of the quartz jade. XRD analysis shows that the main components of the coral fossils with different color and texture are consistent and mainly composed of SiO2 with a trace amount of other minerals and without CaCO3.

  9. How isopolyanions self-assemble and condense into a 2D tungsten oxide crystal: HRTEM imaging of atomic arrangement in an intermediate new hexagonal phase

    SciTech Connect

    Chemseddine, A. Bloeck, U.

    2008-10-15

    The structure and structural evolution of tungstic acid solutions, sols and gels are investigated by high-resolution electron microscopy (HRTEM). Acidification of sodium tungstate solutions, through a proton exchange resin, is achieved in a way that ensures homogeneity in size and shape of intermediate polytungstic species. Gelation is shown to involve polycondensation followed by a self-assembling process of polytungstic building blocks leading to sheets with a layered hexagonal structure. Single layers of this new metastable phase are composed of three-, four- and six-membered rings of WO{sub 6} octahedra located in the same plane. This is the first time that a 2D oxide crystal is isolated and observed by direct atomic resolution. Further ageing and structural evolution leading to single sheets of 2D ReO{sub 3}-type structure is directly observed by HRTEM. Based on this atomic level imaging, a model for the formation of the oxide network structure involving a self-assembling process of tritungstic based polymeric chain is proposed. The presence of tritungstic groups and their packing in electrochromic WO{sub 3} films made by different techniques is discussed. - Graphical abstract: From the isopolyanion to the extended bulk tungsten oxide: HRTEM imaging.

  10. The effect of temperature on the structure and magnetic properties of Co0.5Ni0.5Fe2O4 spinel nanoferrite

    NASA Astrophysics Data System (ADS)

    Abdallah, Hafiz M. I.; Moyo, Thomas; Ngema, Nokwanda

    2015-11-01

    Nanocrystalline Co0.5Ni05Fe2O4 ferrite with average crystallite size of 7.6 nm and lattice constant of 0.8372 nm was synthesized via a glycol-thermal process. The structure parameters and morphology of the as-synthesized sample and annealed samples were characterized by XRD, EDX, FTIR, HRSEM and HRTEM. The hyperfine interactions, iron distribution on the tetrahedral and octahedral sites for the as-synthesized sample and samples annealed at 500 °C were deduced by Mössbauer spectroscopy measurements at 300 K. The magnetization measurements for the as-synthesized and annealed samples (300-900 °C) were obtained by a vibrating sample magnetometer on a cryogen free measurement system at different isothermal temperatures (4-300 K) in external applied magnetic fields of ±5 T. The temperature dependence of the magnetic properties such as coercive field, saturation magnetization, remanent magnetization and squareness of hysteresis loops were investigated. The sample transformed from single-domain to multi-domain configuration at particle size of about 31 nm. At 300 K, the sample annealed at 700 °C exhibits a maximum coercivity. The as-prepared sample shows a substantial increase in coercivity from 0.182 kOe at 300 K to 6.018 kOe at 4 K.

  11. Mirrored low-energy channel for the MiniXRD

    SciTech Connect

    Dutra, Eric; MacNeil, Lawrence; Raphaelian, Mark; Compton, Steve; Jacoby, Barry

    2015-10-08

    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, the researchers 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.

  12. Gahnite under high pressure: A XRD insitu study

    NASA Astrophysics Data System (ADS)

    Lathe, Christian; Wehber, Michael; Schilling, Frank; Mueller, Hans

    2013-06-01

    Placing P-T-t constraints on planetary differentiation Natural gahnite has the ideal formula ZnAl2O4. Together with franklinite (ZnFe2O4) it forms a limited solid solution at high temperatures an occurs as an accessory phase in magmatic and metamorphic rocks, but mainly in the Franklin marble and skarn deposits (Carvalho and Sclar 1988, Frondel and Baum 1974). A natural gahnite sample was investigated with large volume presses at the Synchrotron source DESY. Pressure was stepwise increased to 5 GPa at the MAX80 and 15 GPa at MAX200x and diffraction patterns were collected after each step. The determined volume-pressure-data are fitted to a 2nd and 3rd order Birch-Murnaghan equation of state to obtain the isothermal bulk modulus KT0 and its pressure derivative K'. Isothermal bulk modulus was derived from XRD data. Using a 2nd and 3rd order Birch-Murnaghan equation of state revealed KT02nd = 207(4) GPa KT03rd = 204(4) GPa and K' = 4.9(3), respectively. A significant change of the pressure derivatives of C11, C12 and C44 at a pressure of approximately 15 GPa indicates a 2nd order phase transition in gahnite.

  13. Sesamum indicum Plant Extracted Microwave Combustion Synthesis and Opto-Magnetic Properties of Spinel MnxCo₁₋xAl₂O₄Nano-Catalysts.

    PubMed

    Manikandan, A; Durka, M; Selvi, M Amutha; Antony, S Arul

    2016-01-01

    Spine Mn(x)Co₁₋xAl₂O₄ (x = 0, 0.3 and 0.5) nanoparticles were synthesized using Sesamum indicum (S. indicum) plant extracted microwave-assisted combustion method. S. indicum plant extract simplifies the process, provides an alternative process for a simple, economical and environment friendly synthesis. The absence of surfactant/catalysts has led to a simple, cheap and fast method of synthesis of spinel nanoparticles. The as-synthesized spinel nanoparticles were characterized by X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy, high resolution scanning electron microscopy (HR-SEM), high resolution transmission electron microscopy (HR-TEM), energy dispersive X-ray analysis (EDX), Brunauer Emmett Teller (BET) surface area analysis, UV-Visible diffuse reflectance spectroscopy (DRS), Photoluminescence (PL) spectroscopy, and vibrating sample magnetometer. The formation of spinel nanoparticles was confirmed by HR-SEM and HR-TEM and their possible formation mechanisms were also proposed. Powder XRD, FT-IR, SAED and EDX results confirmed the formation of pure and single cubic phase CoAl₂O₄ with well-defined crystalline. The optical property was determined by DRS and PL spectra. VSM measurements revealed that pure and Mn-doped CoAl₂O₄ samples have weak ferromagnetic behavior and the magnetization values increases with increasing the concentration of Mn²⁺ ions in the CoAl₂O₄ lattice. The sample Mn₀.₅Co₀.₅Al₂O₄ possessed higher surface area and smaller crystallite size than other samples, which led to enhance the performance toward the selective oxidation of benzyl alcohol into benzaldehyde.

  14. XRD studies of chitin-based polyurethane elastomers.

    PubMed

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

    2008-08-15

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

  15. Controlled synthesis and magnetic properties of monodispersed ceria nanoparticles

    SciTech Connect

    Kumar, Sumeet; Ojha, Animesh K.; Srivastava, Manish E-mail: manish-mani84@rediffmail.com; Singh, Jay; Layek, Samar; Yashpal, Madhu; Materny, Arnulf

    2015-02-15

    In the present study, monodispersed CeO{sub 2} nanoparticles (NPs) of size 8.5 ± 1.0, 11.4 ± 1.0 and 15.4 ± 1.0 nm were synthesized using the sol-gel method. Size-dependent structural, optical and magnetic properties of as-prepared samples were investigated by X-ray diffraction (XRD), field emission scanning electron microscope (FE-SEM), high resolution transmission electron microscopy (HR-TEM), ultra-violet visible (UV-VIS) spectroscopy, Raman spectroscopy and vibrating sample magnetometer (VSM) measurements. The value of optical band gap is calculated for each particle size. The decrease in the value of optical band gap with increase of particle size may be attributed to the quantum confinement, which causes to produce localized states created by the oxygen vacancies due to the conversion of Ce{sup 4+} into Ce{sup 3+} at higher calcination temperature. The Raman spectra showed a peak at ∼461 cm{sup -1} for the particle size 8.5 nm, which is attributed to the 1LO phonon mode. The shift in the Raman peak could be due to lattice strain developed due to variation in particle size. Weak ferromagnetism at room temperature is observed for each particle size. The values of saturation magnetization (Ms), coercivity (Hc) and retentivity (Mr) are increased with increase of particle size. The increase of Ms and Mr for larger particle size may be explained by increase of density of oxygen vacancies at higher calcination temperature. The latter causes high concentrations of Ce{sup 3+} ions activate more coupling between the individual magnetic moments of the Ce ions, leading to an increase of Ms value with the particle size. Moreover, the oxygen vacancies may also produce magnetic moment by polarizing spins of f electrons of cerium (Ce) ions located around oxygen vacancies, which causes ferromagnetism in pure CeO{sub 2} samples.

  16. Spectral, XRD, SEM and biological activities of transition metal complexes of polydentate ligands containing thiazole moiety

    NASA Astrophysics Data System (ADS)

    Neelakantan, M. A.; Marriappan, S. S.; Dharmaraja, J.; Jeyakumar, T.; Muthukumaran, K.

    2008-11-01

    Metal complexes of o-vanillidene-2-aminobenzothiazole have been prepared and characterized by elemental and spectral (vibrational, electronic, 1H NMR and EPR) data as well as magnetic susceptibility measurements and thermo gravimetric analysis (TG/DTA). The low molar conductance values reveal the non-electrolytic nature of these complexes. The elemental analysis suggests that the stoichiometry to be 1:2 (metal:ligand). Magnetic susceptibility data coupled with electronic spectra suggest that two ligands coordinate to each metal atom by phenolic oxygen and imino nitrogen to form high spin octahedral complex with Co(II), Mn(II) and Ni(II). The fifth and sixth position of metal ion is satisfied with water molecules. The thermal behaviour (TG/DTA) of the synthesised complexes shows that the complexes loss water molecules in the first step followed by decomposition of the ligand. Spin Hamiltonian parameters predict a distorted tetrahedral geometry for the copper complex. XRD and SEM analysis provide the crystalline nature and the morphology of the metal complexes. The in vitro biological activity of the metal chelates is tested against the Gram positive bacteria ( Bacillus amyloliquifacians) and gram negative bacteria ( Pseudomonas species), fungus ( Aspergillus niger) and yeast ( Sacchromyces cereviaceae). Most of the metal chelates exhibited higher biological activities.

  17. Synthesis and characterization of poly(divinylbenzene)-coated magnetic iron oxide nanoparticles as precursor for the formation of air-stable carbon-coated iron crystalline nanoparticles.

    PubMed

    Boguslavsky, Yonit; Margel, Shlomo

    2008-01-01

    Maghemite (gamma-Fe2O3) nanoparticles of 15 +/- 3 nm diameter were prepared by nucleation of gelatin/iron oxide followed by growth of gamma-Fe2O3 films onto these nuclei. The gamma-Fe2O3 nanoparticles were coated with polydivinylbenzene (PDVB) by emulsion polymerization of divinylbenzene (DVB) in an aqueous continuous phase containing the gamma-Fe2O3 nanoparticles. The PDVB-coated gamma-Fe2O3 nanoparticles, dispersed in water, were separated from homo-PDVB nanoparticles using the high gradient magnetic field (HGMF) technique. The influence of DVB concentration on the amount of PDVB coating, on the size and size distribution of the coated gamma-Fe2O3 nanoparticles and on their magnetic properties, has been investigated. Air-stable carbon-coated iron (alpha-Fe/C) crystalline nanoparticles of 41 +/- 12 nm diameter have been prepared by annealing the PDVB-coated gamma-Fe2O3 nanoparticles at 1050 degrees C in an inert atmosphere. These nanoparticles exhibit high saturation magnetization value (83 emu g(-1)) and excellent resistance to oxidation. Characterization of the PDVB-coated gamma-Fe2O3 and of the alpha-Fe/C nanoparticles has been accomplished by TEM, HRTEM, DLS, FTIR, XRD, thermal analysis, zeta-potential, and magnetic measurements.

  18. Effect of calcination temperature on microstructure and magnetic properties of Ni{sub 0.5}Zn{sub 0.25}Cu{sub 0.25} Fe{sub 2}O{sub 4} nanoparticles synthesized by sol-gel method

    SciTech Connect

    Pransisco, Prengki E-mail: afza@petronas.com.my; Shafie, Afza E-mail: afza@petronas.com.my; Guan, Beh Hoe

    2014-10-24

    This paper examines the effect of calcination process on the structural and magnetic properties material nanostructure composite of Ni{sub 0Ð}œ‡{sub 5}Zn{sub 0Ð}œ‡{sub 25}Cu{sub 0.25} Fe{sub 2}O{sub 4} ferrites. The samples were successfully prepared by sol-gel method at different calcination temperature, which are 600°C, 700°C, 800°C and 900°C. Morphological investigation, average crystallite size and microstructure of the material were examined by using X-ray diffraction (XRD) and confirmed by high resolution transmission electron microscope (HRTEM) and field emission scanning electron microscope (FESEM). The effects of calcination temperature on the magnetic properties were calculated by using vibrating sample magnetometer (VSM). The XRD result shows single-phase cubic spinel structure with interval average size 5.9-38 nm, and grain size microstructure of the material was increasing with temperature increases. The highest magnetization saturation was reached at a temperature 800°C with value 53.89 emu/g, and the value coercive force (Hc) was inversely with the grain size.

  19. Magnetic recoverable Fe3O4-TiO2:Eu composite nanoparticles with enhanced photocatalytic activity

    NASA Astrophysics Data System (ADS)

    Stefan, M.; Leostean, C.; Pana, O.; Toloman, D.; Popa, A.; Perhaita, I.; Senilă, M.; Marincas, O.; Barbu-Tudoran, L.

    2016-12-01

    This work refers to the influence of Eu doping on the morphologic, structural and compositional properties of magnetic separable Fe3O4-TiO2 composite nanoparticles with photocatalytic activity. In this respect, Fe3O4-TiO2:Eu nanocomposites were prepared by seed mediated growth of TiO2:Eu through a sol-gel method onto preformed magnetite resulted from co-precipitation method. Different Eu concentration precursors were used for doping. The thermal behavior and the conversion of precursors into corresponding Fe3O4-TiO2:Eu composite nanoparticles were evidenced by FT-IR spectra and thermal analysis. The XRD, XPS and HRTEM investigations results indicate that nanocomposites contain besides Fe3O4-TiO2:Eu some amounts of iron titanate. Formation of FeTiO3 is suppressed by the increase of Eu doping level. Magnetic studies also indicated that nanocomposite exhibit superparamagnetic behavior at room temperature. The large surface area and mesoporous structure of magnetic nanocomposite were confirmed by the surface area (BET) and porosity measurements. It was demonstrated that the composite nanoparticles exhibit good photocatalytic activity toward the degradation of RhB solution and they can be used as efficient and conveniently recoverable photocatalyst.

  20. Controllable synthesis, magnetism and solubility enhancement of graphene nanosheets/magnetite hybrid material by covalent bonding.

    PubMed

    Zhan, Yingqing; Yang, Xulin; Meng, Fanbin; Wei, Junji; Zhao, Rui; Liu, Xiaobo

    2011-11-01

    Hybrids of Fe(3)O(4) nanoparticles and surface-modified graphene nanosheets (GNs) were synthesized by a two-step process. First, graphene nanosheets were modified by SOCl(2) and 4-aminophenoxyphthalonitrile to introduce nitrile groups on their surface. Second, the nitrile groups of surface-modified graphene nanosheets were reacted with ferric ions on the surface of Fe(3)O(4) with the help of relatively high boiling point solvent ethylene glycol to form a GNs/Fe(3)O(4) hybrid. The covalent attachment of Fe(3)O(4) nanoparticles on the graphene nanosheet surface was confirmed by Fourier-transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), energy-dispersive X-ray spectrometer (EDS) and scanning electron microscopy (SEM). TEM and HRTEM observations indicated that the sizes of the nanoparticles and their coverage density on GNs could be easily controlled by changing the concentration of the precursor and the weight ratio to GNs. Magnetic measurements showed that magnetization of the hybrid materials is strongly influenced by the reaction conditions. Chemically bonded by phthalocyanine, the solubility of as-synthesized GNs/Fe(3)O(4) hybrid materials was greatly enhanced, which was believed to have potential for applications in the fields of composites, wastewater treatment and biomaterials.

  1. MAGNETS

    DOEpatents

    Hofacker, H.B.

    1958-09-23

    This patent relates to nmgnets used in a calutron and more particularly to means fur clamping an assembly of magnet coils and coil spacers into tightly assembled relation in a fluid-tight vessel. The magnet comprises windings made up of an assembly of alternate pan-cake type coils and spacers disposed in a fluid-tight vessel. At one end of the tank a plurality of clamping strips are held firmly against the assembly by adjustable bolts extending through the adjacent wall. The foregoing arrangement permits taking up any looseness which may develop in the assembly of coils and spacers.

  2. Fission products silver, palladium, and cadmium identification in neutron-irradiated SiC TRISO particles using a Cs-Corrected HRTEM

    NASA Astrophysics Data System (ADS)

    van Rooyen, I. J.; Olivier, E. J.; Neethling, J. H.

    2016-08-01

    Electron microscopy investigations of selected coated particles from the first advanced gas reactor experiment at Idaho National Laboratory provided important information on fission product distribution and chemical composition in the silicon-carbide (SiC) layer. Silver precipitates were nano-sized, and therefore high-resolution transmission electron microscopy (HRTEM) was used to provide more information at the atomic level. Based on gamma-ray analysis, this particle which was irradiated to an average burnup of 19.38% fissions per initial metal atom, may have released as much as 10% of its available Ag-110 m inventory during irradiation. The HRTEM investigation focused on silver, palladium, and cadmium due to interest in silver transport mechanisms and possible correlation with palladium and silver previously found. Palladium, silver, and cadmium were found to co-exist in some of the SiC grain boundaries and triple junctions. This study confirmed palladium both at inter and intragranular sites. Phosphor was identified in SiC grain boundaries and triple points.

  3. 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.

  4. Structural and magnetic properties of pristine and Fe-doped NiO nanoparticles synthesized by the co-precipitation method

    SciTech Connect

    Mishra, A.K.; Das, D.

    2012-09-15

    Highlights: ► The prepared samples were characterized by XRD, TEM, HR-TEM techniques. ► Magnetic properties of the samples were compared. ► Surface spins frozen at lower temperatures resulted a spin glass. ► The samples show enhancement of coercivity with decreased temperature. -- Abstract: Ni{sub 1−x}Fe{sub x}O (x = 0 and 0.03) nanoparticles are synthesized by a chemical route. XRD and TEM measurements confirm phase purity and crystallinity of the nanoparticles. Fe substitution in NiO reduces considerably the average particle size of the nanoparticles. The pristine NiO sample with size 14 nm and Fe-substituted sample having size 7 nm show room temperature ferromagnetism. The pristine NiO having 31 nm size and Fe-substituted sample with size 25 nm are found to be antiferromagnetic. The M–H and M–T behavior of the pristine and Fe-doped samples are explained with a core–shell model with an antiferromagnetic core and a ferromagnetic shell. The disordered spins at the shell give rise to a spin-glass like frozen state below 10 K. The obtained room temperature ferromagnetism in the pristine and Fe-doped NiO has been attributed to particle size effect.

  5. Synthesis of manganese oxide nanocrystal by ultrasonic bath: effect of external magnetic field.

    PubMed

    Bastami, Tahereh Rohani; Entezari, Mohammad H

    2012-07-01

    A novel technique was used for the synthesis of manganese oxide nanocrystal by applying an external magnetic field (EMF) on the precursor solution before sonication with ultrasonic bath. The results were compared in the presence and absence of EMF. Manganese acetate solution as precursor was circulated by a pump at constant speed (7 rpm, equal to flow rate of 51.5 mL/min) in an EMF with intensity of 0.38 T in two exposure times (t(MF), 2h and 24h). Then, the magnetized solution was irradiated indirectly by ultrasonic bath in basic and neutral media. One experiment was designed for the effect of oxygen atmosphere in the case of magnetic treated solution in neutral medium. The as prepared samples were characterized with X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, transmission electron microscopy (HRTEM, TEM), energy-dispersive spectrum (EDS), and superconducting quantum interference device (SQUID) analysis. In neutral medium, the sonication of magnetized solution (t(MF), 24h) led mainly to a mixture of Mn(3)O(4) (hausmannite) and γ-MnOOH (manganite) and sonication of unmagnetized solution led to a pure Mn(3)O(4). In point of particle size, the larger and smaller size of nanoparticles was obtained with and without magnetic treatment, respectively. In addition, the EMF was retarded the nucleation process, accelerated the growth of the crystal, and increased the amount of rod-like structure especially in oxygen atmosphere. In basic medium, a difference was observed on the composition of the products between magnetic treated and untreated solution. For these samples, the magnetic measurements as a function of temperature were exhibited a reduction in ferrimagnetic temperature to T(c)=39K, and 40K with and without magnetic treatment, respectively. The ferrimagnetic temperature was reported for the bulk at T(c)=43K. A superparamagnetic behavior was observed at room temperature without any saturation magnetization and hysteresis in the measured

  6. Equilibrium and kinetic studies on acid dye Acid Red 88 adsorption by magnetic ZnFe2O4 spinel ferrite nanoparticles.

    PubMed

    Konicki, Wojciech; Sibera, Daniel; Mijowska, Ewa; Lendzion-Bieluń, Zofia; Narkiewicz, Urszula

    2013-05-15

    A magnetic ZnFe2O4 (MNZnFe) was synthesized by microwave assisted hydrothermal method and was used as an adsorbent for the removal of acid dye Acid Red 88 (AR88) from aqueous solution. The effects of various parameters such as initial AR88 concentration (10-56 mg L(-1)), pH solution (3.2-10.7), and temperature (20-60°C) were investigated. Prepared magnetic ZnFe2O4 was characterized by XRD, SEM, HRTEM, ICP-AES, BET, FTIR, and measurements of the magnetic susceptibility. The experimental data were analyzed by the Langmuir and Freundlich models of adsorption. Equilibrium data fitted well with the Langmuir model. Pseudo-first-order and pseudo-second-order kinetic models and intraparticle diffusion model were used to examine the adsorption kinetic data. The adsorption kinetics was found to follow the pseudo-second-order kinetic model. Thermodynamics parameters, ΔG°, ΔH° and ΔS°, indicate that the adsorption of AR88 onto MNZnFe was spontaneous and exothermic in nature.

  7. Facile preparation of magnetic separable powdered-activated-carbon/Ni adsorbent and its application in removal of perfluorooctane sulfonate (PFOS) from aqueous solution.

    PubMed

    Liang, Xuanqi; Gondal, Mohammed A; Chang, Xiaofeng; Yamani, Zain H; Li, Nianwu; Lu, Hongling; Ji, Guangbin

    2011-01-01

    The main aim of this study was to synthesize magnetic separable Nickel/powdered activated carbon (Ni/PAC) and its application as an adsorbent for removal of PFOS from aqueous solution. In this work, the synthesized adsorbent using simple method was characterized by using X-ray diffractionometer (XRD), surface area and pore size analyzer, vibrating sample magnetometer (VSM), and high resolution transmission electron microscope (HRTEM). The surface area, pore volume and pore size of synthesized PAC was 1521.8 m(2)g(-1), 0.96 cm(3)g(-1), 2.54 nm, respectively. Different kinetic models: the pseudo-first-order model, the pseudo-second-order model, and three adsorption isotherms--Langmuir, Freundlich and Temkin--were applied to study the sorption kinetics and isothermal behavior of PFOS onto the surface of an as-prepared adsorbent. The rate constant using the pseudo-second-order model for removal of 150 ppm PFOS was estimated as 8.82×10(-5) and 1.64×10(-4) for PAC and 40% Ni/PAC, respectively. Our results demonstrated that the composite adsorbents exhibited a clear magnetic hysteretic behavior, indicating the potential practical application in magnetic separation of adsorbents from aqueous solution phase as well.

  8. Surfaces and their effect on the magnetic properties of polycrystalline hollow γ-Mn2O3 and MnO nanoparticles

    NASA Astrophysics Data System (ADS)

    Bah, Mohamed A.; Jaffari, G. Hassnain; Khan, F. A.; Shah, S. Ismat

    2016-07-01

    Manganese oxide nanoparticles were prepared in an inert gas condensation system. X-ray Diffraction (XRD) studies revealed presence of multiple manganese oxide phases while high resolution transmission electron microscopy (HRTEM) showed polycrystalline hollow nanoparticle morphology. The additional inner surface of the hollow nanoparticle directly affect the magnetic properties of these particles. Combined physical structure, electronic structure and magnetic susceptibility analyses led to the conclusion that the prepared nanoparticles are polycrystalline and composed of γ-Mn2O3 and MnO crystallites. Magnetic study found a sharp peak around 38 K with no frequency dependence in the AC susceptibility measurement. Large coercivity (HC) and exchange bias (HEB) fields, up to 11 kOe and 7 kOe, respectively, were observed below the order temperatures. HC and HEB were found to increase and decrease, respectively, as a function of cooling field. Both HC and HEB were found to decrease monotonically as the temperature approached paramagnetic phase transition of the ferrimagnetic component.

  9. 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.

  10. Morphology and Chemical Composition of soot particles emitted by Wood-burning Cook-Stoves: a HRTEM, XPS and Elastic backscattering Studies.

    NASA Astrophysics Data System (ADS)

    Carabali-Sandoval, G. A., Sr.; Castro, T.; Peralta, O.; De la Cruz, W.; Días, J.; Amelines, O.; Rivera-Hernández, M.; Varela, A.; Muñoz-Muñoz, F.; Policroniades, R.; Murillo, G.; Moreno, E.

    2014-12-01

    The morphology, microstructure and the chemical composition on surface of soot particles were studied by using high resolution transmission electron microscopy (HRTEM), X-ray photoelectron spectroscopy (XPS) and elastic backscattering spectrometry. In order to obtain freshly soot particles emitted by home-made wood-burning cook stoves, copper grids for Transmission Electron Microscope (TEM) were placed on the last two of an 8-stages MOUDI cascade impactor. The analysis of HRTEM micrographs revealed the nanostructure and the particle size of soot particles. The XPS survey spectra show a large carbon peak around 285 eV and the oxygen signal at 533 eV. Some differences observed in the carbon/oxygen (C/O) ratio of the particles probably depend on the combustion process efficiency of each cook-stove analyzed. The C-1s XPS spectra show an asymmetric broad peak and other with low intensity that corresponds to sp2 and sp3hybridization, which were fitted with a convolution using Gaussian functions. Elastic backscattering technique allows a chemical elemental analysis of samples and confirms the presence of C, O and Si observed by XPS. Additionally, the morphological properties of soot aggregates were analyzed calculating the border-based fractal dimension (Df). Particles exhibit complex shapes with high values of Df. Also, real-time absorption (σabs) and scattering (σsct) coefficients of fine (with aerodynamic diameter < 2.5 µm) soot particles were measured. The trend in σabs and σsct indicate that the cooking process has two important combustion stages which varied in its flaming strength, being vigorous in the first stage and soft in the second one.

  11. Characterization of collision cascade damage in Ca{sub 2}La{sub 8}(SiO{sub 4}){sub 6}O{sub 2} by HRTEM

    SciTech Connect

    Weber, W.J.; Wang, L.M.

    1994-12-01

    Ca{sub 2}La{sub 8}(SiO{sub 4}){sub 6}O{sub 2} thin crystals become amorphous under ion beam irradiation. The ion dose required for complete amorphization of the thin crystal (critical amorphization dose, D{sub c}) increased with the increasing irradiation temperature and decreased with ion mass at elevated temperatures. Samples irradiated with 1-1.5 MeV Ar{sup +}, Kr{sup +} and Xe{sup +} ions to doses much lower than Dc, in the temperature range from 20 to 498 K were used for a detailed HRTEM study to better understand the amorphization process. The residual collision cascade damage after irradiation appeared as manometer scale amorphous domains. The images of these domains are extremely sensitive to the sample thickness. Small domains of cascade size were only found at the very thin edge of the sample. In thicker regions, amorphous domains appear after higher doses as the result of cascade overlap in projection. At higher temperatures, the observed amorphous domains are smaller indicating thermal recovery at the amorphous/crystalline interface. The amorphous domains are also larger in size after irradiation with ions of higher mass at a fixed ion dose. These results are consistent with the Dc-temperature curves determined by in situ TEM with the HVEM-Tandem Facility at Argonne National Laboratory. The width of the amorphous rim along the edge of the specimen grew with increasing ion dose suggesting that amorphization also proceeds from the sample surface. Images of the collision cascade damage were compared to the cascade sizes calculated with the TRIM code. Some digitally acquired HRTEM images of the cascade damage were processed to reveal more detailed information.

  12. X-ray powder diffraction of high-absorption materials at the XRD1 beamline off the best conditions: Application to (Gd, Nd)5Si4 compounds

    NASA Astrophysics Data System (ADS)

    Carvalho, A. M. G.; Nunes, R. S.; Coelho, A. A.

    2017-03-01

    Representative compounds of the new family of magnetic materials Gd5-xNdxSi4 were analyzed by X-ray diffraction at the XRD1 beamline at LNLS. To reduce X-ray absorption, thin layers of the powder samples were mounted outside the capillaries and measured in Debye-Scherrer geometry as usual. The X-ray diffraction analyses and the magnetometry results indicate that the behavior of the magnetic transition temperature as a function of Nd content may be directly related to the average of the four smallest interatomic distances between different rare earth sites of the majority phase of each compound. The quality and consistency of the results show that the XRD1 beamline is able to perform satisfactory X-ray diffraction experiments on high-absorption materials even off the best conditions.

  13. Cobalt nanoparticles-embedded magnetic ordered mesoporous carbon for highly effective adsorption of rhodamine B

    NASA Astrophysics Data System (ADS)

    Tang, Lin; Cai, Ye; Yang, Guide; Liu, Yuanyuan; Zeng, Guangming; Zhou, Yaoyu; Li, Sisi; Wang, Jiajia; Zhang, Sheng; Fang, Yan; He, Yibin

    2014-09-01

    Cobalt nanoparticles-embedded magnetic ordered mesoporous carbon (Co/OMC), prepared through a simple method involving infusing and calcination, was used as a highly effective adsorbent for rhodamine B (Rh B) removal. Several techniques, including SEM, HRTEM, nitrogen adsorption-desorption isotherms, XRD, Raman spectra, EDX, zeta potential and VSM measurement, were applied to characterize the adsorbent. Batch tests were conducted to investigate the adsorption performance. The adsorption capacity of the resultant adsorbent was relatively high compared with raw ordered mesoporous carbon (OMC) and reached an equilibrium value of 468 mg/g at 200 mg/L initial Rh B concentration. Removal efficiency even reached 96% within 25 min at 100 mg/L initial Rh B concentration. Besides, the adsorption amount increased with the increase of solution pH, adsorbent dose and initial Rh B concentration. Kinetics study showed that the adsorption agreed well with pseudo-second-order model (R2 = 0.999) and had a significant correlation with intra-particle diffusion model in the both two adsorption periods. Furthermore, thermodynamics research indicated that the adsorption process was endothermic and spontaneous in nature. The adsorption isotherms fitted well with Langmuir model, demonstrating the formation of mono-molecular layer on the surface of Co/OMC during adsorption process. The results confirmed that Co/OMC has the potential superiority in removal of Rh B from aqueous solution.

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

    NASA Astrophysics Data System (ADS)

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

    2012-03-01

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

  15. 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.

  16. Hierarchical Fe3O4@MoS2/Ag3PO4 magnetic nanocomposites: Enhanced and stable photocatalytic performance for water purification under visible light irradiation

    NASA Astrophysics Data System (ADS)

    Guo, Na; Li, Haiyan; Xu, Xingjian; Yu, Hongwen

    2016-12-01

    Novel hierarchical Fe3O4@MoS2/Ag3PO4 magnetic nanophotocatalyst with remarkable photocatalytic capability were prepared by simply depositing the Ag3PO4 onto the surface of crumpled Fe3O4@MoS2 nanosphere. The nanocomposites were characterized by XRD, TEM, HRTEM, XPS, BET, and UV-vis DRS. The outcome of the photocatalytic experiments demonstrated that Fe3O4@MoS2/Ag3PO4 with 6 wt% content of Ag3PO4 (FM/A-6%) showed the highest photocatalytic activity upon the degradation Congo red (CR) and Rhodamine B (RhB) under both visible light and simulated sunlight irradiation. In addition, FM/A-6% possessed larger specific surface area (76.56 m2/g) and excellent optical property. The possible Z-scheme charge carriers transfer mechanism for the enhanced photocatalytic properties of the FM/A-6% was also discussed. The Z-scheme charge carriers transfer mechanism established between MoS2 and Ag3PO4 facilitate the charge separation efficiency. Moreover, FM/A-6% can be separated and collected easily by external magnetic field and maintain high activity after five times photoreaction cycles. Given the remarkable photocatalytic performance and high stability of FM/A-6% nanocomposite, it is looking forward to exhibit great potential for applications in water purification.

  17. Clay pigment structure characterisation as a guide for provenance determination--a comparison between laboratory powder micro-XRD and synchrotron radiation XRD.

    PubMed

    Švarcová, Silvie; Bezdička, Petr; Hradil, David; Hradilová, Janka; Žižak, Ivo

    2011-01-01

    Application of X-ray diffraction (XRD)-based techniques in the analysis of painted artworks is not only beneficial for indisputable identification of crystal constituents in colour layers, but it can also bring insight in material crystal structure, which can be affected by their geological formation, manufacturing procedure or secondary changes. This knowledge might be helpful for art historic evaluation of an artwork as well as for its conservation. By way of example of kaolinite, we show that classification of its crystal structure order based on XRD data is useful for estimation of its provenance. We found kaolinite in the preparation layer of a Gothic wall painting in a Czech church situated near Karlovy Vary, where there are important kaolin deposits. Comparing reference kaolin materials from eight various Czech deposits, we found that these can be differentiated just according to the kaolinite crystallinity. Within this study, we compared laboratory powder X-ray micro-diffraction (micro-XRD) with synchrotron radiation X-ray diffraction analysing the same real sample. We found that both techniques led to the same results.

  18. HRTEM/AEM study of trace metal behavior, sheet silicate reactions, and fluid/solid mass balances in porphyry copper hydrothermal systems

    SciTech Connect

    Veblen, D.R.; Ilton, E.S.

    1989-04-01

    Transmission electron microscopy has been used to investigate copper (Cu) incorporation into silicates and alteration reactions in porphyry copper deposits. High Cu in biotites results from submicroscopic inclusions of native Cu. The incorporation of Cu in low-temperature alteration lamellae suggests that Cu enrichment occurs during weathering, rather than during the hydrothermal event. Drill core from Cyprus Casa Grande, Arizona, shows systematic variation of Cu in sheet silicates as a function of depth in the weathering column. The aims of the present project are to apply the powerful techniques of transmission electron microscopy (TEM), high-resolution TEM (HRTEM), and analytical electron microscopy (AEM) to understanding the geochemical processes in porphyry copper systems at the near-atomic scale. Our primary goals are to characterize the structural state of anomalously high Cu in silicates, determine the timing and conditions of Cu enrichment in silicates such as biotite, and use these data to suggest how base metals are released and subsequently immobilized under hydrothermal or weathering conditions; and to determine the submicroscopic, atomic-level reaction mechanisms responsible for silicate alteration in porphyry-copper hydrothermal systems, which will allow us to determine reaction stoichiometries and hence mass balances between minerals and hydrothermal fluid. 19 refs., 7 figs., 3 tabs.

  19. TEM and HRTEM study of oxide particles in an Al-alloyed high-Cr oxide dispersion strengthened ferritic steel with Hf addition

    NASA Astrophysics Data System (ADS)

    Dou, Peng; Kimura, Akihiko; Kasada, Ryuta; Okuda, Takanari; Inoue, Masaki; Ukai, Shigeharu; Ohnuki, Somei; Fujisawa, Toshiharu; Abe, Fujio; Jiang, Shan; Yang, Zhigang

    2017-03-01

    The nanoparticles in an Al-alloyed high-Cr oxide dispersion strengthened (ODS) ferritic steel with Hf addition, i.e., SOC-16 (Fe-15Cr-2W-0.1Ti-4Al-0.62Hf-0.35Y2O3), have been examined by transmission electron microscopy (TEM) and high resolution transmission electron microscopy (HRTEM). Relative to an Al-alloyed high-Cr ODS ferritic steel without Hf addition, i.e., SOC-9 (Fe-15.5Cr-2W-0.1Ti-4Al-0.35Y2O3), the dispersion morphology and coherency of the oxide nanoparticles in SOC-16 were significantly improved. Almost all the small nanoparticles (diameter <10 nm) in SOC-16 were found to be consistent with cubic Y2Hf2O7 oxides with the anion-deficient fluorite structure and coherent with the bcc steel matrix. The larger particles (diameter >10 nm) were also mainly identified as cubic Y2Hf2O7 oxides with the anion-deficient fluorite structure. The results presented here are compared with those of SOC-9 with a brief discussion of the underlying mechanisms of the unusual thermal and irradiation stabilities of the oxides as well as the superior strength, excellent irradiation tolerance and extraordinary corrosion resistance of SOC-16.

  20. HRTEM and EFTEM Observations of Matrix in the Oxidized CV3 Chondrite ALH 84028: Implications for the Origins of Matrix Olivines

    NASA Technical Reports Server (NTRS)

    Abreu, Neyda M.; Brearley, Adrian J.

    2003-01-01

    The determination of the nature, distribution, and origin of organic material in carbonaceous chondrites is fundamental to understanding early solar nebular conditions and the origin of life. Using a variety of extraction techniques, followed by detailed chemical analysis, an extensive suite of organic compounds has been identified in carbonaceous chondrites. These data have provided key information on the diversity and isotopic composition of the organic component in chondrites. However, one disadvantage of extraction techniques is that all information regarding the spatial distribution of the organics on a fine scale is lost. This is especially important for the insoluble macromolecular carbon, which constitutes approximately 70% of the carbon in carbonaceous chondrites such as Murchison. The distribution and mineralogical associations may provide important constraints on the possible origins of the carbonaceous material. Our previous studies of the CV3 chondrites Allende and Vigarano have demonstrated that energy filtered transmission electron microscopy (EFTEM), combined with high resolution TEM (HRTEM) are powerful tools for the in situ characterization of insoluble organic matter in carbonaceous chondrites. In this study, we have used SEM and TEM techniques to characterize the matrix mineralogy of the CV3 chondrite ALH 84028 and examine the distribution and mineralogical associations of carbon. We are especially interested in establishing whether the occurrence of poorly graphitized carbon (PGC), observed in Allende matrix olivines, is common to all oxidized CV3 chondrites or is a unique feature of Allende.

  1. HRTEM Study of Oxide Nanoparticles in 16Cr-4Al-2W-0.3Ti-0.3Y2O3 ODS Steel

    SciTech Connect

    Hsiung, L; Fluss, M; Wall, M; Kimura, A

    2009-11-18

    Crystal and interfacial structures of oxide nanoparticles in 16Cr-4Al-2W-0.3Ti-0.3Y{sub 2}O{sub 3} ODS ferritic steel have been examined using high-resolution transmission electron microscopy (HRTEM) techniques. Oxide nanoparticles with a complex-oxide core and an amorphous shell were frequently observed. The crystal structure of complex-oxide core is identified to be mainly monoclinic Y{sub 4}Al{sub 2}O{sub 9} (YAM) oxide compound. Orientation relationships between the oxide and matrix are found to be dependent on the particle size. Large particles (> 20 nm) tend to be incoherent and have a spherical shape, whereas small particles (< 10 nm) tend to be coherent or semi-coherent and have a faceted interface. The observations of partially amorphous nanoparticles lead us to propose three-stage mechanisms to rationalize the formation of oxide nanoparticles containing core/shell structures in as-fabricated ODS steels.

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

    NASA Astrophysics Data System (ADS)

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

    2011-10-01

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

  3. Magnetically recoverable TiO2-WO3 photocatalyst to oxidize bisphenol A from model wastewater under simulated solar light.

    PubMed

    Dominguez, S; Huebra, M; Han, C; Campo, P; Nadagouda, M N; Rivero, M J; Ortiz, I; Dionysiou, D D

    2016-09-27

    A novel magnetically recoverable, visible light active TiO2-WO3 composite (Fe3O4@SiO2@TiO2-WO3) was prepared to enable the photocatalyst recovery after the degradation of bisphenol A (BPA) under simulated solar light. For comparison, the photocatalytic activity of other materials such as non-magnetic TiO2-WO3, Fe3O4@SiO2@TiO2, TiO2, and the commercial TiO2 P25 was also evaluated under the studied experimental conditions. The structure and morphology of the synthesized materials were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HR-TEM), and electron dispersion spectroscopy (EDS). Moreover, Brunauer-Emmett-Teller (BET) surface area and magnetic properties of the samples were determined. The Fe3O4@SiO2@TiO2-WO3 and TiO2-WO3 led to a BPA degradation of 17.50 and 27.92 %, respectively, after 2 h of the simulated solar light irradiation. Even though their activity was lower than that of P25, which degraded completely BPA after 1 h, our catalysts were magnetically separable for their further reuse in the treatment. Furthermore, the influence of the water matrix in the photocatalytic activity of the samples was studied in municipal wastewater. Finally, the identification of reaction intermediates was performed and a possible BPA degradation pathway was proposed to provide a better understanding of the degradation process. Graphical abstract ᅟ.

  4. Magnetically separable Cu2O/chitosan-Fe3O4 nanocomposites: Preparation, characterization and visible-light photocatalytic performance

    NASA Astrophysics Data System (ADS)

    Cao, Chunhua; Xiao, Ling; Chen, Chunhua; Cao, Qihua

    2015-04-01

    A novel magnetically-separable visible-light-induced photocatalyst, Cu2O/chitosan-Fe3O4 nanocomposite (Cu2O/CS-Fe3O4 NC), was prepared via a facile one-step precipitation-reduction process by using magnetic chitosan chelating copper ions as precursor. The structure and properties of Cu2O/CS-Fe3O4 NCs were characterized by XRD, FT-IR, SEM, HRTEM, SAED, EDS, BET, VSM, XPS and UV-vis/DRS. The photocatalytic activity of Cu2O/CS-Fe3O4 NCs was evaluated by decolorization of reactive brilliant red X-3B (X-3B) under visible light irradiation. The characterization results indicated that Cu2O/CS-Fe3O4 NCs exhibited relatively large specific surface areas and special dimodal pore structure because Cu2O was wrapped in chitosan matrix embedded with Fe3O4 nanoparticles. The tight combination of magnetic Fe3O4 and semiconductor Cu2O through chitosan made the nanocomposites show good superparamagnetism and photocatalytic activity. It was found that X-3B could be decolorized more efficiently in acidic media than in neutral or alkaline media. The decolorization of X-3B was ascribed to the synergistic effect of photocatalysis and adsorption. Cu2O/CS-Fe3O4 NCs could be easily separated from the solution by an external magnet, and the decolorization rates of X-3B were still above 87% after five reaction cycles, indicating that Cu2O/CS-Fe3O4 NCs had excellent reusability and stability.

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

    NASA Astrophysics Data System (ADS)

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

    2016-01-01

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

  6. XRD measurement and EXAFS study using synchrotron radiation of Ni (II) complexes of macro cyclic ligand

    NASA Astrophysics Data System (ADS)

    Mishra, Ashutosh; Ninama, Samrath

    2013-06-01

    Nickel (II) tetra-aza macro cyclic complexes compound were synthesis by chemical rout method. X-ray diffraction (XRD) and Extended X-ray absorption fine structure (EXAFS) measurement were carried out. XRD analysis shows that sample is crystalline in nature and having particle size in the range of few micrometers. The EXAFS technique used to determine the bond lengths by three different methods, namely, Levy's, Lytle's and Lytle, Sayers and Stern's (LSS) methods. The phase uncorrected bond lengths have also been obtained from Fourier transformation (F.T.) method and the results obtained have been compared with the results obtained from LSS method, which also gives phase uncorrected bond lengths.

  7. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2016-05-01

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

  9. Raman and XRD Field Characterisation of Sulfate Efflorescences at Rio Tinto (Spain)

    NASA Astrophysics Data System (ADS)

    Rull, F.; Sansano, A.; Sobron, P.; Lafuente, B.; Sarrazin, P.; Gailhanou, M.; Blake, D.

    2009-03-01

    In this work a comparative in-situ analysis of evaporate minerals from Rio Tinto (Spain) is undertaken using two techniques selected for Mars exploration: Raman spectrometer and CheMin XRD both selected as part of the ExoMars and MSL missions respectively.

  10. 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

  11. Characterization of diamond-like carbon films by SEM, XRD and Raman spectroscopy

    NASA Astrophysics Data System (ADS)

    Pang, Hua; Wang, Xingquan; Zhang, Guling; Chen, Huan; Lv, Guohua; Yang, Size

    2010-08-01

    Diamond-like carbon films were deposited by electrolysis of a water-ethanol solution on Cu at low voltages (60-100 V) at 2 mm interelectrode separation. The films were characterized by scanning electron microscopy (SEM), X-ray diffractometer (XRD) and Raman spectroscopy. The films were found to be continuous and compact with uniform grain distribution. Raman spectroscopy analysis revealed two broad bands at ˜1350 and ˜1580 cm -1. The downshift of the G band of graphite is indicative of the presence of DLC. For XRD analysis, the three strong peaks located at 2 θ values of 43.2°, 74.06° and 89.9° can be identified with reflections form (1 1 1), (2 2 0) and (3 1 1) plane of diamond.

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

    SciTech Connect

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

    2014-12-15

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

  13. Mössbauer and XRD study of Al-Sn linished steel bimetal alloy

    NASA Astrophysics Data System (ADS)

    Kuzmann, E.; Silva, L. da; Stichleutner, S.; El-Sharif, M.; Homonnay, Z.; Klencsár, Z.; Sziráki, L.; Chisholm, C. U.; Lak, B.

    2016-12-01

    Aluminium alloy free CS1 type steel (0.06 wt% C, 0.45 wt% Mn) and samples of cold roll bonded steel bimetal alloys (MAS15 and MAS16) were fabricated and investigated by X-ray diffraction (XRD), 57Fe conversion electron Mössbauer spectroscopy (CEMS) at room temperature. XRD has revealed only the existence of the alpha iron solid solution (steel) phase in the steel only sample, while identified steel and metallic Al and Sn constituent phases in the bimetallic alloys. 57Fe Mössbauer spectroscopy revealed the presence of 4 % secondary iron-bearing phase attributed mainly to iron oxide/ oxyhydroxides (ferrihydrite) besides the steel matrix on the surface of the steel sample. A significant difference between the occurrences of the secondary phase of differently prepared bimetal alloys found in their 57Fe CEM spectra allowed to identify the main phase of debris as different iron oxide/ oxyhydroxides.

  14. 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.

  15. Understanding changes in cellulose crystalline structure of lignocellulosic biomass during ionic liquid pretreatment by XRD.

    PubMed

    Zhang, Jiafu; Wang, Yixun; Zhang, Liye; Zhang, Ruihong; Liu, Guangqing; Cheng, Gang

    2014-01-01

    X-ray diffraction (XRD) was used to understand the interactions of cellulose in lignocellulosic biomass with ionic liquids (ILs). The experiment was designed in such a way that the process of swelling and solubilization of crystalline cellulose in plant cell walls was followed by XRD. Three different feedstocks, switchgrass, corn stover and rice husk, were pretreated using 1-butyl-3-methylimidazolium acetate ([C4mim][OAc]) at temperatures of 50-130°C for 6h. At a 5 wt.% biomass loading, increasing pretreatment temperature led to a drop in biomass crystallinity index (CrI), which was due to swelling of crystalline cellulose. After most of the crystalline cellulose was swollen with IL molecules, a low-order structure was found in the pretreated samples. Upon further increasing temperature, cellulose II structure started to form in the pretreated biomass samples as a result of solubilization of cellulose in [C4mim][OAc] and subsequent regeneration.

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

    SciTech Connect

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

    2012-01-03

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

  17. 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.

  18. 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.

  19. Study the oxidation kinetics of uranium using XRD and Rietveld method

    NASA Astrophysics Data System (ADS)

    Zhang, Yanzhi; Guan, Weijun; Wang, Qinguo; Wang, Xiaolin; Lai, Xinchun; Shuai, Maobing

    2010-03-01

    The surface oxidation of uranium metal has been studied by X-ray diffraction (XRD) and Rietveld method in the range of 50~300°C in air. The oxidation processes are analyzed by XRD to determine the extent of surface oxidation and the oxide structure. The dynamics expression for the formation of UO2 was derived. At the beginning, the dynamic expression was nonlinear, but switched to linear subsequently for uranium in air and humid oxygen. That is, the growth kinetics of UO2 can be divided into two stages: nonlinear portion and linear portion. Using the kinetic data of linear portion, the activation energy of reaction between uranium and air was calculated about 46.0 kJ/mol. However the content of oxide as a function of time was linear in humid helium ambience. Contrast the dynamics results, it prove that the absence of oxygen would accelerate the corrosion rate of uranium in the humid gas. We can find that the XRD and Rietveld method are a useful convenient method to estimate the kinetics and thermodynamics of solid-gas reaction.

  20. [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.

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

    NASA Astrophysics Data System (ADS)

    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. 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.

  3. 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.

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

    NASA Astrophysics Data System (ADS)

    Ostrooumov, Mikhail

    2007-12-01

    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 α-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 Å) 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.

  5. Quantitative XRD HW-IR plot for clay mineral domain size and lattice strain analyses

    NASA Astrophysics Data System (ADS)

    Wang, H. J.; Chen, D. Z.; Zhou, J.; Chen, T.; Wang, H.; Zhang, Z. Q.

    2003-04-01

    Based on integral-breadth method, the one of three basic XRD methods (Klug &Alexander, 1974), authors (2000) proposed a qualitative half width (HW)-intensity ratio (IR) plot for clay mineral domain size and lattice strain analyses. In this study, the quantitative HW-IR plot is further developed on the basis of i) the curve relation between the Voigt function and the Pearson VII function; ii) the relationship between the Kübler index and the Weaver index. By numerical simulating, it is derived a curve relation between shape indexes k of the Voigt function and u of the Pearson VII function. With this curve relation, k and u can be converted each other in an accuracy of ten thousandth and therefore the domain size and the lattice strain contributions can be precisely separated from an XRD peak according to Langford's (1978) formula. For micaceous minerals, the HW-IR plot requires only a pair of values of the Kübler index and the Weaver index from 1nm reflection. For other clay minerals, the plot needs a pair of values of the (00l) peak's half width and intensity ratio IR. IR is a ratio of peak maximum to the intensity at the position of maximum minus 0.422oΔ2Θ in CuKα radiation. This quantitative plot renders a mean dimension of clay particles perpendicular to the reflection plane (00l) and an approximate upper limit strain normal to d001. The accuracy for domain size analysis reaches one tenth of nanometre and that for the lattice strain analysis is in ten thousandth respectively. This plot method can be widely used with any digital X-ray diffractometer, whose XRD data can be converted into text format. Excel 5.0 or latter versions in both English and Chinese can well support the HW-IR plot. This study was supported by NNSFC (Grant No 40272022)

  6. [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.

  7. 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

  8. Hydration Characteristics of Metakaolin Admixtured Cement using DTA, XRD and SEM Techniques

    NASA Astrophysics Data System (ADS)

    Govindarajan, D.; Gopalakrishnan, R.

    2008-04-01

    The paper aims to investigate hydration and pozzolanic reaction in Portland cement paste with different replacement percentages (0%, 10%, 20% and 30%) of metakaolin. The compressive strength of the metakaolin admixtured cement was measured at 1 day, 1 week and 4 weeks. The compressive strength developments of the metakaolin admixtured cement are compared with Portland cement. It is found that metakaolin contributes significantly to strength development as an accelerating admixture for Portland cement. The pozzolanic reactions and the reaction products were determined by DTA, XRD and SEM.

  9. 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

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

    SciTech Connect

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

    2014-02-12

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

  11. 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.

  12. 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.

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

    SciTech Connect

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

    2012-11-19

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

  14. Application of quantitative XRD on the precipitation of struvite from Brine Water

    NASA Astrophysics Data System (ADS)

    Heraldy, E.; Rahmawati, F.; Heryanto; Putra, D. P.

    2017-02-01

    The present studies have been conducted to quantify the varied phases in struvite formation from brine water as the magnesium source. The quantitative X-ray Diffraction (QXRD) method was performed to quantitatively determine the crystal phases and amorphous content of struvite samples. Substantial phase samples were employed quantitative analysis to calibrate against known phase composition information by Rietveld refinement on powder XRD data. The results showed that brine water could be considered as magnesium source the formation of struvite products. The study demonstrated that in general, the high N:P molar ratio (both pH 9 and 10) might lead to the significant formation of struvite.

  15. XRD studies of cement embedding matrices containing complexing reagents from decontamination practices

    SciTech Connect

    Ionascu, L.; Nicu, M.; Turcanu, M.; Dragolici, F.; Rotarescu, Ghe.

    2013-07-01

    The study of embedding matrix of radioactive waste is an important issue concerning the need to assure the radiological safety requirements for final disposal. The conditioning of the radioactive wastes by cementation process involves also a structural investigation by X-ray diffraction (XRD) of the samples prepared with cement and complexing agents at different concentration. This paper gives useful information about the influence of complexing agents related to damages produced in concrete microstructures. The experimental data obtained on samples kept in real repository environment for a period up to 15 years, offer structural information regarding the interaction between the different decontamination agents with the major components of the matrix. (authors)

  16. 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.

  17. Investigation of Mg and Zn doped 45S5 bioactive materials by XRD, FTIR and SEM techniques

    NASA Astrophysics Data System (ADS)

    Anand, Vikas; Singh, K. J.; Kaur, Kulwinder

    2014-04-01

    Magnesium and zinc doped 45S5 samples were prepared in the laboratory by sol gel technique., Structural properties of the samples have been studied by XRD, FTIR and SEM techniques. Both FTIR and XRD data indicate the primary bioactive behavior of the samples. Presented results may be useful to improve the antibacterial as well as osteoblast properties of the currently available bioactive materials.

  18. Investigation of NaCl deliquescence in porous substrates using RH-XRD

    NASA Astrophysics Data System (ADS)

    Linnow, Kirsten; Juling, Herbert; Steiger, Michael

    2007-03-01

    We report on the use of X-ray diffractometry under controlled conditions of temperature and relative humidity (RH-XRD) for the investigation of NaCl deliquescence in the pore space of glass filter frits, which were used as model substrates. The study confirms that RH-XRD is an appropriate experimental technique for the in situ observation of phase transformation in porous materials. It is used for an investigation of both the deliquescence kinetics and the deliquescence humidity within pores of different median pore diameter. Several major influences affecting deliquescence rates in the pore space close to the surface of a porous material are discussed. It appears that quite short-term variation of ambient relative humidity, e.g., typical daily fluctuations, might induce damaging deliquescence-crystallization cycles within the pore space of building materials. In agreement with theoretical considerations it was found that confinement of NaCl crystals in pores with median diameters in the range 1.4-70 μm does not affect the deliquescence humidity of the salt.

  19. Determination of equilibrium humidities using temperature and humidity controlled X-ray diffraction (RH-XRD).

    PubMed

    Linnow, Kirsten; Steiger, Michael

    2007-01-30

    Confined growth of crystals in porous building materials is generally considered to be a major cause of damage. We report on the use of X-ray diffraction under controlled conditions of temperature and relative humidity (RH-XRD) for the investigation of potentially deleterious phase transition reactions. An improved procedure based on rate measurements is used for the accurate and reproducible determination of equilibrium humidities of deliquescence and hydration reactions. The deliquescence humidities of NaCl (75.4+/-0.5% RH) and Ca(NO3)2 x 4 H2O (50.8+/-0.7% RH) at 25 degrees C determined with this improved RH-XRD technique are in excellent agreement with available literature data. Measurement of the hydration of anhydrous Ca(NO3)2 to form Ca(NO3)2 x 2 H2O revealed an equilibrium humidity of 10.2+/-0.3%, which is also in reasonable agreement with available data. In conclusion, dynamic X-ray diffraction measurements are an appropriate method for the accurate and precise determination of equilibrium humidities with a number of interesting future applications.

  20. Crystal growth in Se70Te30 thin films followed by SEM and in situ XRD

    NASA Astrophysics Data System (ADS)

    Martinková, Simona; Barták, Jaroslav; Málek, Jiri; Segawa, Hiroyo

    2016-10-01

    The isothermal crystal growth kinetics in Se70Te30 thin films was investigated using the microscopy and in situ X-ray diffraction (XRD) measurements. Plate-like crystals grew linearly with time which is the sign of liquid-crystal interface kinetics. In the studied temperature range, from 68 °C to 88 °C, crystal growth rates exhibit simple exponential behavior with an activation energy of crystal growth EG = 168 ± 12 kJ mol-1. The growth data obtained from the microscopy measurements were combined with viscosity data, melting parameters and the appropriate crystal growth model was assessed. The relation between the kinetic coefficient of crystal growth and viscosity (u∝η-ξ) is described in detail, and a correction of the standard growth model is suggested. The crystal growth data obtained from the in situ XRD measurements were described using the Johnson-Mehl-Avrami nucleation-growth model with the Avrami exponent m = 2.2 ± 0.2. The activation energy of the overall crystallization process EA was estimated and its value is 171 ± 11 kJ mol-1.

  1. 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.

  2. 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.

  3. Mössbauer and XRD study of hot dip galvanized alloy

    NASA Astrophysics Data System (ADS)

    Kuzmann, E.; Speakman, R.; El-Sharif, M.; Stichleutner, S.; Homonnay, Z.; Klencsár, Z.; Sziráki, L.; Chisholm, C. U.; Lak, Gy. B.

    2016-12-01

    Mössbauer spectroscopy has been used to investigate the nature of the Zinc-Iron alloys present within the Hot Dip Galvanized (HDG) layers of steel with a silicon content of 0.35 %. The investigation also studied the impact of the powder coating pretreatment on the nature of the alloy layers. The acid etching process within the pretreatment process in particular would be expected to have a significant impact on the HDG layer. This study utilized 57Fe Mössbauer spectroscopy to examine identically processed samples prior to and post pre treatment. XRD and 57Fe CEMS measurements were performed on hot galvanized S355J2 + N samples, forming sandwiched structure. Both XRD and CEMS reveal the presence of dominant steel phase in accordance with its estimated occurrence on the surface of the sandwiched samples. Minor Γ-Fe3Zn10, ζ-FeZn15 and solid solution Fe-Zn as well as minor Fe-Si phases could also be identified.

  4. 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.

  5. FTIR, XRD and DSC studies of nanochitosan, cellulose acetate and polyethylene glycol blend ultrafiltration membranes.

    PubMed

    Vinodhini, P Angelin; K, Sangeetha; Thandapani, Gomathi; P N, Sudha; Jayachandran, Venkatesan; Sukumaran, Anil

    2017-03-29

    In the present work, a series of novel nanochitosan/cellulose acetate/polyethylene glycol (NCS/CA/PEG) blend flat sheet membranes were fabricated in different ratios (1:1:1, 1:1:2, 2:1:1, 2:1:2, 1:2:1, 2:2:1) in a polar solvent of N,N'-dimethylformamide (DMF) using the most popular phase inversion method. Nanochitosan was prepared by the ionotropic gelation method and its average particle size has been analyzed using Dynamic Light Scattering (DLS) method. The effect of blending of the three polymers was investigated using FTIR and XRD studies. FTIR results confirmed the formation of well-blended membranes and the XRD analysis revealed enhanced amorphous nature of the membrane ratio 2:1:2. DSC study was conducted to find out the thermal behavior of the blend membranes and the results clearly indicated good thermal stability and single glass transition temperature (Tg) of all the prepared membranes. Asymmetric nature and rough surface morphology was confirmed using SEM analysis. From the results it was evident that the blending of the polymers with higher concentration of nanochitosan can alter the nature of the resulting membranes to a greater extent and thus amorphous membranes were obtained with good miscibility and compatibility.

  6. Luminescence and magnetic properties of novel nanoparticle-sheathed 3D Micro-Architectures of Fe0.5R0.5(MoO4)1.5:Ln3+ (R = Gd3+, La3+), (Ln = Eu, Tb, Dy) for bifunctional application

    NASA Astrophysics Data System (ADS)

    Krishnan, Rajagopalan; Thirumalai, Jagannathan; Kathiravan, Arunkumar

    2015-01-01

    For the first time, we report the successful synthesis of novel nanoparticle-sheathed bipyramid-like and almond-like Fe0.5R0.5(MoO4)1.5:Ln3+ (R = Gd3+, La3+), (Ln = Eu, Tb, Dy) 3D hierarchical microstructures through a simple disodium ethylenediaminetetraacetic acid (Na2EDTA) facilitated hydrothermal method. Interestingly, time-dependent experiments confirm that the assembly-disassembly process is responsible for the formation of self-aggregated 3D architectures via Ostwald ripening phenomena. The resultant products are characterized by x-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), high resolution transmission electron microscopy (HRTEM), photoluminescence (PL), and magnetic measurements. The growth and formation mechanisms of the self-assembled 3D micro structures are discussed in detail. To confirm the presence of all the elements in the microstructure, the energy loss induced by the K, L shell electron ionization is observed in order to map the Fe, Gd, Mo, O, and Eu components. The photo luminescence properties of Fe0.5R0.5(MoO4)1.5 doped with Eu3+, Tb3+, Dy3+ are investigated. The room temperature and low temperature magnetic properties suggest that the interaction between the local-fields introduced by the magnetic Fe3+ ions and the R3+ (La, Gd) ions in the dodecahedral sites determine the magnetism in Fe0.5R0.5(MoO4)1.5:Eu3+. This work provides a new approach to synthesizing the novel Fe0.5R0.5(MoO4)1.5:Ln3+ for bi-functional magnetic and luminescence applications.

  7. The high - low-p clinoenstatite transition: in situ xrd and ultrasonic study

    NASA Astrophysics Data System (ADS)

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

    2003-04-01

    Using single-crystal X-ray diffraction analyses in a diamond anvil cell Angel et al. (1992) published the transformation of MgSiO_3 from LCEn to a C2/c-polymorph (HCEn) at around 5.5 - 8.0 GPa and room-T (RT)conditions. This LCEn - HCEn-transition is not quenchable. However, the knowledge of the exact phase boundary positions for the MgSiO_3-transitions is essential as pyroxene is an important component of the Earth's mantle and will significantly influence elastic properties (e.g. v_p, v_s) of the mantle. We determined the HCEn - LCEn-transition by in-situ XRD experiments under high P, T using the multi-anvil appar atus MAX80 at the synchrotron facility HASYLAB, Hamburg. Our preliminary results only represent the minimum P-conditions of the HCEn - LCEn phase boundary, which is approximated by equation P (GPa) = 0.0021T (/C) + 6.06. Nevertheless, our results are in good agreement to data published by Angel & Hugh-Jones (1994). The invariant point defined by the intersection of the HCEn - LCEn equilibrium determined within this study and the OEn - LCEn reaction after Angel &Hugh-Jones (1994) lies at about 7.9 GPa and 875/C. This is in contrast to earlier experimental results of Kanzaki (1991) and Ulmer &Stalder (2001). The samples for the ultrasonic interferometry experiments were prepared by hot-isostatic pressing also using the MAX80. Adjacent XRD ruled out any phase transition during the hip-process. For the ultrasonic measurements one of the six anvils of MAX80 were exchanged by an anvil equipped with lithium niobate p- and s-wave transducers of 33.3 MHz natural frequency (Mueller et al., 2002). Corresponding to the XRD experiments HCEn was formed by increasing the pressure at RT. The velocities of elastic compressional and shear waves were measured under in situ conditions using the classical digital sweep technique. After the phase transition to LCEn as a result of rising the temperature at given pressure the measurements were repeated. The newly developed

  8. 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.

  9. 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.

  10. 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.

  11. Formation of nickel-manganese oxide thermistors studied by XRD, SEM and auger spectroscopy

    NASA Astrophysics Data System (ADS)

    Azimi-Nam, S.; Golestani-Fard, F.; Hashemi, T.

    1987-03-01

    This paper describes the formation of nickel-manganeses oxide thermistor bodies at 1000 1340° C, employing analytical techniques of XRD, SEM/EPMA and AES. The micro-structural studies revealed that the main phase of nickel manganite coexists with a solid solution of NiO in Mn3O4 in the final product. The optimum firing conditions to achieve the necessary electrical properties as well as the development of the desired microstructure could be selected around 1200° C, for 4 hrs in an ambient atmosphere. Above this temperature, the density begins to decrease while the resistivity increases. These anomalous electrical resistivity variations could be partly attributed to the trapped oxygen which was evolved from the decomposition of the unreacted α-Mn2O3. At-lower temperatures, unreacted nickel oxide residuals as well as a high porosity of the samples would yield specimens with high resistivity.

  12. EXAFS and XRD characterization of palladium sorbents for high temperature mercury capture from fuel gas.

    PubMed

    Poulston, Stephen; Hyde, Timothy I; Hamilton, Hugh; Mathon, Olivier; Prestipino, Carmelo; Sankar, Gopinathan; Smith, Andrew W J

    2010-01-14

    Removal of pollutants such as mercury at elevated temperatures provides improvements in the overall thermal efficiency during the process of coal gasification. The two high temperature sorbents studied were 5 wt% Pd/Al(2)O(3) and 5 wt% Pd/SiO(2): materials shown to have significantly different Hg adsorption capacities. A combination of XRD and EXAFS has been used to characterize the Pd-Hg alloy formed when these Pd-based sorbents were exposed to fuel gas (CO, CO(2), H(2)) containing Hg vapour at 204 degrees C. Significant differences were found in the nature of the alloy formed on the two sorbents following Hg exposure. The Pd/Al(2)O(3) sorbent produced a single homogeneous solid solution of Pd-Hg whilst the silica-supported Pd produced an alloy of varying composition.

  13. 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.

  14. 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.

  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.

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

    NASA Astrophysics Data System (ADS)

    Xu, Hongwu; Guo, Xiaofeng; Bai, Jianming

    2017-02-01

    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. Synchrotron-based XRD from rat bone of different age groups.

    PubMed

    Rao, D V; Gigante, G E; Cesareo, R; Brunetti, A; Schiavon, N; Akatsuka, T; Yuasa, T; Takeda, T

    2017-05-01

    Synchrotron-based XRD spectra from rat bone of different age groups (w, 56 w and 78w), lumber vertebra at early stages of bone formation, Calcium hydroxyapatite (HAp) [Ca10(PO4)6(OH)2] bone fill with varying composition (60% and 70%) and bone cream (35-48%), has been acquired with 15keV synchrotron X-rays. Experiments were performed at Desy, Hamburg, Germany, utilizing the Resonant and Diffraction beamline (P9), with 15keV X-rays (λ=0.82666 A(0)). Diffraction data were quantitatively analyzed using the Rietveld refinement approach, which allowed us to characterize the structure of these samples in their early stages. Hydroxyapatite, received considerable attention in medical and materials sciences, since these materials are the hard tissues, such as bone and teeth. Higher bioactivity of these samples gained reasonable interest for biological application and for bone tissue repair in oral surgery and orthopedics. The results obtained from these samples, such as phase data, crystalline size of the phases, as well as the degree of crystallinity, confirm the apatite family crystallizing in a hexagonal system, space group P63/m with the lattice parameters of a=9.4328Å and c=6.8842Å (JCPDS card #09-0432). Synchrotron-based XRD patterns are relatively sharp and well resolved and can be attributed to the hexagonal crystal form of hydroxyapatite. All the samples were examined with scanning electron microscope at an accelerating voltage of 15kV. The presence of large globules of different sizes is observed, in small age groups of the rat bone (8w) and lumber vertebra (LV), as distinguished from, large age groups (56 and 78w) in all samples with different magnification, reflects an amorphous phase without significant traces of crystalline phases. Scanning electron microscopy (SEM) was used to characterize the morphology and crystalline properties of Hap, for all the samples, from 2 to 100μm resolution.

  18. Spectroscopic, DFT, and XRD Studies of Hydrogen Bonds in N-Unsubstituted 2-Aminobenzamides.

    PubMed

    Mphahlele, Malose Jack; Maluleka, Marole Maria; Rhyman, Lydia; Ramasami, Ponnadurai; Mampa, Richard Mokome

    2017-01-04

    The structures of the mono- and the dihalogenated N-unsubstituted 2-aminobenzamides were characterized by means of the spectroscopic (¹H-NMR, UV-Vis, FT-IR, and FT-Raman) and X-ray crystallographic techniques complemented with a density functional theory (DFT) method. The hindered rotation of the C(O)-NH₂ single bond resulted in non-equivalence of the amide protons and therefore two distinct resonances of different chemical shift values in the ¹H-NMR spectra of these compounds were observed. 2-Amino-5-bromobenzamide (ABB) as a model confirmed the presence of strong intramolecular hydrogen bonds between oxygen and the amine hydrogen. However, intramolecular hydrogen bonding between the carbonyl oxygen and the amine protons was not observed in the solution phase due to a rapid exchange of these two protons with the solvent and fast rotation of the Ar-NH₂ single bond. XRD also revealed the ability of the amide unit of these compounds to function as a hydrogen bond donor and acceptor simultaneously to form strong intermolecular hydrogen bonding between oxygen of one molecule and the NH moiety of the amine or amide group of the other molecule and between the amine nitrogen and the amide hydrogen of different molecules. DFT calculations using the B3LYP/6-311++G(d,p) basis set revealed that the conformer (A) with oxygen and 2-amine on the same side predominates possibly due to the formation of a six-membered intramolecular ring, which is assisted by hydrogen bonding as observed in the single crystal XRD structure.

  19. 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.

  20. 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.

  1. Influence of microstructure and interfacial strain on the magnetic properties of epitaxial Mn3O4/La0.7Sr0.3MnO3 layered-composite thin films

    NASA Astrophysics Data System (ADS)

    Mukherjee, Devajyoti; Bingham, Nicholas; Hordagoda, Mahesh; Phan, Manh-Huong; Srikanth, Hariharan; Witanachchi, Sarath; Mukherjee, Pritish

    2012-10-01

    Epitaxial Mn3O4/La0.7Sr0.3MnO3 (Mn3O4/LSMO) bilayer thin films were grown on lattice-matched single crystal substrates of SrTiO3 (STO) (100) and MgO (100), with Mn3O4 as the top layer, using a pulsed laser deposition technique. X-ray diffraction (XRD) patterns revealed the single crystalline nature and epitaxial relationship between the layers. A detailed analysis of strains using XRD asymmetric/symmetric scans indicated an increasing in-plane compressive strain in the LSMO layer with increasing thicknesses of the Mn3O4 layer, resulting in a tetragonal distortion of the LSMO lattice in the Mn3O4/LSMO films in comparison to the tensile strains in LSMO single-layer films grown on both STO and MgO substrates. Cross-sectional high resolution transmission electron microscope (HRTEM) images showed atomically sharp interfaces in all films. However, as opposed to a flat interface between LSMO and STO, the Mn3O4 and LSMO interface was undulating and irregular in the bilayer films. Magnetic measurements revealed that relative to LSMO, the presence of Mn3O4 in Mn3O4/LSMO reduced the saturation magnetization at T > 50 K (the ferrimagnetic ordering temperature of Mn3O4) but enhanced it at T < 50 K. The decrease of the saturation magnetization in Mn3O4/LSMO for T > 50 K was associated with the appearance and increase of the compressive strain with the increase in Mn3O4 thickness. These observations point to the importance of a ferromagnetic-ferrimagnetic interfacial coupling between the LSMO and Mn3O4 layers in enhancing the surface magnetism of LSMO in the Mn3O4/LSMO bilayers. Our study provides useful information regarding the development of manganite composite thin films with improved magnetic properties for a wide range of technological applications, such as in spintronics and sensor devices.

  2. Photocatalytic degradation of methylene blue dye and magneto-optical studies of magnetically recyclable spinel NixMn1-xFe2O4 (x = 0.0-1.0) nanoparticles

    NASA Astrophysics Data System (ADS)

    Mathubala, G.; Manikandan, A.; Arul Antony, S.; Ramar, P.

    2016-06-01

    Nickel doped spinel manganese ferrite (NixMn1-xFe2O4: x = 0.0-1.0) nanoparticles were prepared successfully by a superficial microwave irradiation technique using urea as the fuel. Powder X-ray diffraction (XRD) analysis was recognized the configuration of single phase spinel structure of NixMn1-xFe2O4. Debye Sherrer's formula was used to calculate the average crystallite size of the samples, which were found in the range of 15-20 nm. High resolution scanning electron microscopy (HR-SEM) was used to analyze the surface morphology of the samples, which showed the particle like-morphology with smaller agglomeration, and it was also confirmed by high resolution transmission electron microscopy (HR-TEM). Energy dispersive X-ray (EDX) analysis confirmed the elemental composition, which also evidence for the formation of single pure phase. Microwave heating method produced well crystalline nature of the products, which was confirmed by selected area electron diffraction (SAED) analysis. UV-Visible diffuse reflectance spectra (DRS) were used to calculate the energy band gap and the observed values are increased slightly from 2.05 eV to 2.44 eV with increasing the Ni-dapant. Magnetic characterization of the samples were analyzed by room temperature vibrating sample magnetometer (VSM) technique and the observed magnetization (Ms) values are decreased with increasing Ni content, due to the different magnetic moments of Mn2+ and Ni2+ cations. Photocatalytic degradation (PCD) of methylene blue dye was carried out by self designed photo-catalytic reactor. It was observed that PCD efficiency is increased with increase in concentration of Ni and the sample Ni0.6Mn0.4Fe2O4 shows better photocatalytic activity (96.73%) than other samples.

  3. 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

  4. 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.

  5. Structures And Magnetization Of Defect-Associated Sites In Silicon

    SciTech Connect

    Chow, L.; Gonzalez-Pons, J. C.; Barco, E. del; Vanfleet, R.; Misiuk, A.; Chai, G.

    2008-04-24

    To better understand the mechanism of the reported 'quasi-ferromagnetism' observed in Si ions self-implanted or irradiated silicon, we carry out high resolution transmission electron microscopy (HRTEM), magnetization measurements using superconducting quantum interference device (SQUID) magnetometer, and ferromagnetic resonance (FMR) measurements of the magnetic interaction of the defect-associated sites in silicon damaged by silicon self-implantation or energetic particle beams. The SQUID measurements showed that the silicon self-implanted sample has paramagnetic ordering. FMR measurements indicated the He{sup ++} irradiated sample has a ferromagnetic interaction and yields a Lande g-factor of 2.35.

  6. 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

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

    PubMed

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

    2004-03-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2004-03-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2010-09-01

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

  10. 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

  11. 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

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

    PubMed

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

    2013-12-16

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

  13. 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.

  14. [Spectroscopic analysis of the crystallization mechanism of synthesized zeolite with XRD and FTIR approaches].

    PubMed

    Fan, Chun-hui; Ma, Hong-rui; Hua, Li

    2012-04-01

    Zeolites were synthesized from fly ash using modified one-stage method. The changes in cation exchange capacity (CEC) and chemical elements of zeolite were investigated during the synthesis process to reveal the materials and elements transformation in solid-liquid system. The approaches of XRD, SEM and FTIR were used to indicate the crystallization characteristics and mechanism. The zeolite NaP1 was synthesized, and the CEC value reached to the maximum of 135 mmol/100g at 24 h. After the hydrothermal reaction for 12 h, the characteristic peak and metastable crystalline structure of zeolite NaP1 appeared, then the hydroxy sodalite products formed at 48 h. The crystallization process was the result of materials transformation: the elements of fly ash released into the liquid system for the melting effect of alkali solution, and the solid system played the role of skeleton in crystallization process, being the "source" and the "sink" of the reaction, respectively, and the achievements presented the crystallization mechanism of liquid-phase and solid-phase transformation.

  15. XRD and XANES study of some Cu-doped MnBi materials

    NASA Astrophysics Data System (ADS)

    Mishra, Ashutosh; Patil, Harsha

    2016-10-01

    High purity MnBi low temperature phase has been prepared and analyzed using X- ray diffraction (XRD) and X-ray absorption near edge structure (XANES) measurements. The X-ray diffraction measurements were carried out using Bruker D8 Advance X-ray diffractometer. The X-rays were produced using a sealed tube and the wavelength of X-ray was 154 nm (Cu K-alpha). and X-rays were detected using a fast counting detector based on Silicon strip technology (Bruker LynxEye detector)[1]. and the X-ray absorption spectra has emerged as a powerful technique for local structure determination, which can be applied to any type of material. The X-ray absorption measurements of two Cu-doped MnBi alloys have been performed at the recently developed BL-8 Dispersive EXAFS beam line at 2.5 GeV Indus-2 synchrotron at RRCAT, Indore, India[2]. The X-ray absorption near edge structure (XANES) data obtained has been processed using data analysis program Athena. The energies of the K absorption edge, chemical shifts, edge-widths, shifts of the principal absorption maximum in the alloys have been determined.

  16. 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.

  17. Void-species nanostructure of chalcogenide glasses studied with FSDP-related XRD

    NASA Astrophysics Data System (ADS)

    Kavetskyy, T. S.; Shpotyuk, O. I.; Boyko, V. T.

    2007-05-01

    Void-species nanostructure is studied in glassy arsenic selenide g-As2Se3 and sulphide g-As2S3 using X-ray diffraction in respect to the first sharp diffraction peak (FSDP-related XRD) treated within Elliott's void-based model. It is shown that the previously established analytical relationship between the FSDP position Q1 and nanovoid diameter D in the form of Q1=2.3·π/D seems to be close to ones reported by Gaskell [Medium-range structure in glasses and low-Q structure in neutron and X-ray scattering data, J. Non-Cryst. Solids 351 (2005) 1003 1013] and Rachek [X-ray diffraction study of amorphous alloys Al Ni Ce Sc with using Ehrenfest's formula, J. Non-Cryst. Solids 352 (2006) 3781 3786]. Following to this correlation, it is concluded that internal nanostructural voids in chalcogenide glasses are responsible for low-Q structure observed in X-ray scattering.

  18. 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.

  19. 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.

  20. 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.

  1. 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.

  2. 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)

  3. 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.

  4. Development Of Magnetic Fe-C Nanocomposites Obtained Via The Laser Pyrolysis: Structural And Disaggregation Properties

    SciTech Connect

    Morjan, Ion; Alexandrescu, R.; Dumitrache, F.; Fleaca, C.; Birjega, R.; Soare, I.; Luculescu, C.-R.; Prodan, V.; Kuncser, V.; Filoti, G.; Xu, H.; Wang, D.

    2010-10-06

    Fe-C) nanoparticles have been successfully synthesized using the laser pyrolysis method and variable nozzle geometries. At large nozzle diameters, XRD and SAED analysis clearly identified distinct {alpha}-Fe and Fe{sub 3}C phases. TEM and HRTEM indicated that these Fe-based nanoparticles have an average grain size of 3.5-10.2 nm. Temperature dependent Moessbauer spectra further confirm their distinct nanophases. By using a multi-step reduction procedure, Fe-C powders can be disaggregated into stable, water soluble nanoparticles.

  5. 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.

  6. Characterization of various magnesium oxides by XRD and {sup 1}H MAS NMR spectroscopy

    SciTech Connect

    Aramendia, M.A.; Benitez, J.A.; Borau, V.; Jimenez, C.; Marinas, J.M.; Ruiz, J.R.; Urbano, F.

    1999-04-01

    A magnesium oxide obtained by thermal decomposition of commercially available magnesium hydroxide was refluxed in water and acetone in order to improve its chemical and textural properties with the purpose of using it as a support for metals in heterogeneous catalysts. X-ray diffraction, CO{sub 2} chemisorption, and {sup 1}H magic-angle spinning nuclear magnetic resonance were used to identify crystal phases, the number of basic sites, and the nature of OH groups in the oxide, respectively.

  7. 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

  8. 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.

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

    PubMed

    Finck, Nicolas; Dardenne, Kathy

    2016-05-01

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

  10. FT-IR and XRD analysis of natural Na-bentonite and Cu(II)-loaded Na-bentonite.

    PubMed

    Zhirong, Liu; Azhar Uddin, Md; Zhanxue, Sun

    2011-09-01

    Na-bentonite has been studied extensively because of its strong adsorption capacity and complexation ability. In this work, surface area, total pore volume, mean pore diameter, TG, DTA, FT-IR and XRD were carried out in order to reveal the characteristics of natural Na-bentonite. XRD and FT-IR of natural Na-bentonite (China) and Cu-loaded Na-bentonite as a function of Na-bentonite dosage and temperature using batch technique were characterized in detail, respectively.

  11. FT-IR and XRD analysis of natural Na-bentonite and Cu(II)-loaded Na-bentonite

    NASA Astrophysics Data System (ADS)

    Zhirong, Liu; Azhar Uddin, Md.; Zhanxue, Sun

    2011-09-01

    Na-bentonite has been studied extensively because of its strong adsorption capacity and complexation ability. In this work, surface area, total pore volume, mean pore diameter, TG, DTA, FT-IR and XRD were carried out in order to reveal the characteristics of natural Na-bentonite. XRD and FT-IR of natural Na-bentonite (China) and Cu-loaded Na-bentonite as a function of Na-bentonite dosage and temperature using batch technique were characterized in detail, respectively.

  12. Friedel's salt formation in sulfoaluminate cements: A combined XRD and {sup 27}Al MAS NMR study

    SciTech Connect

    Paul, G.; Boccaleri, E.; Buzzi, L.; Canonico, F.; Gastaldi, D.

    2015-01-15

    Four different binders based on calcium sulfoaluminate cements have been submitted to accelerated chlorination through ionic exchange on hydrated pastes, in order to investigate their ability to chemically bind chloride ions that might reduce chloride penetration. The composition of hydrated cements before and after the treatment was evaluated by means of an X-Ray Diffraction–{sup 27}Al Magic Angle Spinning Nuclear Magnetic Resonance Spectroscopy combined study, allowing to take into account even partially amorphous phases and to make quantitative assumption on the relative abundance of the different aluminium-containing phases. It was found that low SO{sub 3} Sulfoaluminate–Portland ternary systems are the most effective in binding chloride ions and the active role played by different members of the AFm family in chloride uptake was confirmed. Moreover, a peculiar behavior related to the formation of Friedel's salt in different pH conditions was also established for the different cements.

  13. Structural characterization and molecular order of rodlike mesogens with three- and four-ring core by XRD and 13C NMR spectroscopy.

    PubMed

    Reddy, M Kesava; Reddy, K Subramanyam; Yoga, K; Prakash, M; Narasimhaswamy, T; Mandal, A B; Lobo, Nitin P; Ramanathan, K V; Rao, D S Shankar; Prasad, S Krishna

    2013-05-09

    Structural characterizations using XRD and (13)C NMR spectroscopy of two rodlike mesogens consisting of (i) three phenyl ring core with a polar cyano terminal and (ii) four phenyl ring core with flexible dodecyl terminal chain are presented. The three-ring-core mesogen with cyano terminal exhibits enantiotropic smectic A phase while the four-ring mesogen reveals polymesomorphism and shows enantiotropic nematic, smectic C, and tilted hexatic phases. The molecular organization in the three-ring mesogen is found to be partial bilayer smectic Ad type, and the interdigitation of the molecules in the neighboring layers is attributed to the presence of the polar terminal group. For the four-ring mesogen, the XRD results confirm the existence of the smectic C and the tilted hexatic mesophases. A thermal variation of the layer spacing across the smectic C phase followed by a discrete jump at the transition to the tilted hexatic phase is also observed. The tilt angles have been estimated to be about 45° in the smectic C phase and about 40° in tilted hexatic phase. (13)C NMR results indicate that in the mesophase the molecules are aligned parallel to the magnetic field. From the (13)C-(1)H dipolar couplings determined from the 2D experiments, the overall order parameter for the three-ring mesogen in its smectic A phase has been estimated to be 0.72 while values ranging from 0.88 to 0.44 have been obtained for the four-ring mesogen as it passes from the tilted hexatic to the nematic phase. The orientations of the different rings of the core unit with respect to each other and also with respect to the long axis of the molecule have also been obtained.

  14. Mossbauer and XRD characterization of the phase transformations in a Fe-Mn-Al-C-Mo-Si-Cu as cast alloy during tribology test

    NASA Astrophysics Data System (ADS)

    Ramos, J.; Piamba, J. F.; Sánchez, H.; Alcazar, G. A. Pérez

    2015-06-01

    In present study Fe-29.0Mn-6Al-0.9C-1.8Mo-1.6Si-0.4Cu (%w) alloy was obtained after melted in an induction furnace, and then molded as an ingot. From the as cast ingot it were cut samples for the different characterization measurements. The microstructure of the as-cast sample is of dendritic type and its XRD pattern was refined with the lines of the austenite, with a big volumetric fraction, and the lines of the martensite, with small volumetric fraction. The Mössbauer spectrum of the sample was fitted with a broad singlet which corresponds to disordered austenite. After the tribology test, its XRD pattern was refined with the lines of two austenite phases, one similar to the previous one and other with bigger lattice parameter. The total volumetric fraction of the austenite is smaller than that obtained for sample without wear. It was added the lines of the martensite phase with bigger volumetric fraction than that of the previous sample. The Mössbauer spectrum of the weared sample was fitted with two paramagnetic sites which correspond to the two Fe austenite phases and a hyperfine magnetic field distribution which is associated to the disordered original martensite and the new one which appears in the surface as a consequence of the wear process. These results show that during wear process the original austenite phase is transformed in martensite and in a new austenite phase. The increases of the martensitic phase improves mechanical properties and wear behavior.

  15. Intrinsic magnetic properties of bimetallic nanoparticles elaborated by cluster beam deposition.

    PubMed

    Dupuis, V; Khadra, G; Hillion, A; Tamion, A; Tuaillon-Combes, J; Bardotti, L; Tournus, F

    2015-11-14

    In this paper, we present some specific chemical and magnetic order obtained very recently on characteristic bimetallic nanoalloys prepared by mass-selected Low Energy Cluster Beam Deposition (LECBD). We study how the competition between d-atom hybridization, complex structure, morphology and chemical affinity affects their intrinsic magnetic properties at the nanoscale. The structural and magnetic properties of these nanoalloys were investigated using various experimental techniques that include High Resolution Transmission Electron Microscopy (HRTEM), Superconducting Quantum Interference Device (SQUID) magnetometry, as well as synchrotron techniques such as Extended X-ray Absorption Fine Structure (EXAFS) and X-ray Magnetic Circular Dichroism (XMCD). Depending on the chemical nature of the nanoalloys we observe different magnetic responses compared to their bulk counterparts. In particular, we show how specific relaxation in nanoalloys impacts their magnetic anisotropy; and how finite size effects (size reduction) inversely enhance their magnetic moment.

  16. Tuning the magnetic properties of L a0.67S r0.33Co O3-δ films by oxygen pressure

    NASA Astrophysics Data System (ADS)

    Liu, Bin; Wang, Yiqian; Liu, Guiju; Feng, Honglei; Yang, Huaiwen; Xue, Xuyan; Sun, Jirong

    2016-03-01

    In this paper, oxygen-deficient L a0.67S r0.33Co O3 (LSCO) thin films are prepared by adjusting the oxygen pressure during the deposition. As oxygen vacancies are introduced into the LSCO films, the out-of-plane lattices are elongated, as revealed by x-ray diffraction and high-resolution transmission electron microscopy (HRTEM). Modulated bright and dark stripes observed in the HRTEM images of the oxygen-deficient LSCO films are induced by cation ordering and oxygen vacancy ordering, respectively. Magnetic measurements and first-principles calculations show that the oxygen vacancies depress the magnetism of the LSCO films greatly. We also demonstrate that doping Sr into LaCo O3 and removing oxygen from LSCO have a similar effect on the magnetic properties, which is correlated with a derived formula.

  17. Mössbauer and XRD studies of Roman amphorae buried in the sea for two millennia

    NASA Astrophysics Data System (ADS)

    Wagner, F. E.; Wagner, U.; Häusler, W.; Costa, B. F. O.; Blot, J.-Y.; Silva, A. J. M.; Bombico, S.

    2016-12-01

    During the years 2004-2007 many Roman amphora sherds were found in the sea near Cortiçais, off the southern coast of the Peniche peninsula on the Atlantic coast of Portugal. The amphorae are of the Haltern 70 type and stem from a shipwreck that has been dated to the time of the emperor Augustus, between about 15 BC and 15 AD. They were produced in the Roman Province of Baetica in the south of Spain and used to transport wine and other staple foods by sea to other Roman settlements. We have studied several fragments of these amphorae by 57Fe Mössbauer spectroscopy and X-ray diffraction in order to look for changes in the ceramic material caused by two millennia of exposure to sea water. For comparison Mössbauer data on a Haltern 70 type amphora handle excavated on land at the site of Castro do Vieito in the north of Portugal were used. The fragments on which we report here are a body sherd and two handles. The sherds show a visible layer structure. The different layers were studied separately. The Mössbauer spectra of the buff surface layers indicate that up to about 60 % of the iron is present as very fine goethite particles, which are superparamagnetic at RT but exhibit magnetically split spectra at 4.2 K. Their blocking temperature is around or even below 50 K. The goethite is too fine grained to be detected by X-ray diffraction. Re-firing experiments confirm the presence of goethite, which is found to convert to hematite between 300 and 600 ∘C. The results show that the iron in the silicate matrix of the ceramic material converts to goethite under the prolonged influence of the sea water, mainly in the outermost several millimetres and apparently depending on the nature of the ceramic material.

  18. 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.

  19. Petrography, XRD and Wet Chemistry os Sassanid Rock Reliefs at Khan Tahkti (230 a.d.), Iran : A Case Study.

    NASA Astrophysics Data System (ADS)

    Samaniana, Kouros; Shirvanib, Maryam; Bakhshaeia, Hooman

    At Khan Takhti at North West of Iran a sculpted monument commemorating a war waged against the Romans by Shapour I, the second Sassanid king, has been archaeometrically studied. This relief monument carved into the rock in the mountains has faced a considerable destruction process. Petrography, wet chemistry experiments and X-ray diffraction (XRD) analysis were performed to identify rock samples for conservation and preservation purposes. The rock used in this monument is limestone and dolomite. According to XRD analysis, a significant amount of quartz is present in the stone structure. The results of analysis and stone type identification show that a significant quantity of surface sediments and dissolved sulphate, chloride and nitrate salts have been deposited on the surface of the monument due to its proximity to the salty Urmia Lake, which is considered an important factor in the destruction process.

  20. 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.

  1. 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.

  2. Doxorubicin loaded PEG-b-poly(4-vinylbenzylphosphonate) coated magnetic iron oxide nanoparticles for targeted drug delivery

    NASA Astrophysics Data System (ADS)

    Hałupka-Bryl, Magdalena; Bednarowicz, Magdalena; Dobosz, Bernadeta; Krzyminiewski, Ryszard; Zalewski, Tomasz; Wereszczyńska, Beata; Nowaczyk, Grzegorz; Jarek, Marcin; Nagasaki, Yukio

    2015-06-01

    Due to their unique physical properties, superparamagnetic iron oxide nanoparticles are increasingly used in medical applications. They are very useful carriers for delivering antitumor drugs in targeted cancer treatment. Magnetic nanoparticles with chemiotherapeutic were synthesized by coprecipitation method followed by coating with biocompatible polymer. The aim of this work is to characterize physical and magnetic properties of synthesized nanoparicles. Characterization was carried out using EPR, HRTEM, X-ray diffraction, SQUID and NMR methods. The present findings show that synthesized nanosystem is promising tool for potential magnetic drug delivery.

  3. Vacancy ordered γ-Fe2O3 nanoparticles functionalized with nanohydroxyapatite: XRD, FTIR, TEM, XPS and Mössbauer studies

    NASA Astrophysics Data System (ADS)

    Ramos Guivar, Juan A.; Sanches, Edgar A.; Bruns, Florian; Sadrollahi, Elaheh; Morales, M. A.; López, Elvis O.; Litterst, F. Jochen

    2016-12-01

    Vacancy ordered maghemite (γ-Fe2O3) nanoparticles functionalized with nanohydroxyapatite (HAp - Ca10(PO4) 6(OH)2) have been successfully synthesized using an inexpensive co-precipitation chemical route. Evidence for the presence of vacancy order in maghemite was shown by the superstructure lines observed in X-ray diffraction. The adsorption of carboxyl groups of citric acid (C6H8O7) onto γ-Fe2O3 nanoparticles was investigated by FTIR, XPS and Mössbauer spectroscopy. From XPS surface analysis, two binding energies related to oxygen were attributed to bindings between C6H8O7/γ- Fe2O3 and C6H8O7/HAp from an interfacial reaction promoted by strongly adsorbed H2O molecules at the surface of these nanomaterials. Le Bail refinement of the XRD patterns showed the formation of well-crystallized pure tetragonal maghemite before and after functionalization with nanoHAp. The temperature dependence of hyperfine parameters of pure and functionalized γ-Fe2O3 nanoparticles was investigated via Mössbauer spectroscopy. TEM revealed the formation of quasi-spherical γ- Fe2O3 nanoparticles with an average diameter of ca. 12 nm and 16 nm before and after functionalization with nanoHAp in agreement with Le Bail refinement. Magnetometry measurements showed a saturation magnetization of 12 emu/g and a blocking temperature of 340 K for the functionalized γ- Fe2O3 nanoparticles.

  4. 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

  5. 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

  6. Sorption processes and XRD analysis of a natural zeolite exchanged with Pb(2+), Cd(2+) and Zn(2+) cations.

    PubMed

    Castaldi, Paola; Santona, Laura; Enzo, Stefano; Melis, Pietro

    2008-08-15

    In this study the Pb(2+), Cd(2+) and Zn(2+) adsorption capacity of a natural zeolite was evaluated in batch tests at a constant pH of 5.5 by polluting this mineral with solutions containing increasing concentrations of the three cations to obtain adsorption isotherms. In addition X-ray powder diffraction (XRD) was used to investigate the changes of zeolite structure caused by the exchange with cations of different ionic radius. The zeolite adsorption capacity for the three cations was Zn>Pb>Cd. Moreover a sequential extraction procedure [H(2)O, 0.05 M Ca(NO(3))(2) and 0.02 M EDTA] was applied to zeolite samples used in the adsorption experiments to determine the chemical form of the cations bound to the sorbent. Using this approach it was shown that low concentrations of Pb(2+), Cd(2+) and Zn(2+) were present as water-soluble and exchangeable fractions (<25% of the Me adsorbed), while EDTA extracted most of the adsorbed cations from the zeolite (>27% of the Me adsorbed). The XRD pattern of zeolite, analysed according to the Rietveld method, showed that the main mineralogical phase involved in the adsorption process was clinoptilolite. Besides structure information showed that the incorporation of Pb(2+), Cd(2+) and Zn(2+), into the zeolite frameworks changed slightly but appreciably the lattice parameters. XRD analysis also showed the occurrence of some isomorphic substitution phenomena where the Al(3+) ions of the clinoptilolite framework were replaced by exchanged Pb(2+) cations in the course of the ion exchange reaction. This mechanism was instead less evident in the patterns of the samples doped with Cd(2+) and Zn(2+) cations.

  7. 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.

  8. [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.

  9. 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.

  10. Rapid characterisation of archaeological midden components using FT-IR spectroscopy, SEM-EDX and micro-XRD.

    PubMed

    Shillito, Lisa-Marie; Almond, Matthew J; Nicholson, James; Pantos, Manolis; Matthews, Wendy

    2009-07-01

    Samples taken from middens at the Neolithic site of Catalhöyük in Turkey have been analysed using IR spectroscopy backed up by powder XRD and SEM-EDX. Microcomponents studied include fossil hackberries (providing evidence of ancient diet and seasonality), mineral nodules (providing evidence of post-depositional change) and phytoliths (mineralised plant cells, providing evidence of usage of plant species). Finely laminated ashy deposits have also been investigated allowing chemical and mineralogical variations to be explored. It is found that many layers which appear visually to be quite distinctive have, in fact, very similar mineralogy.

  11. 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...

  12. The phase relations in Earth's mid-lower mantle: constraints from in-situ XRD and quantitative chemical analysis

    NASA Astrophysics Data System (ADS)

    Zhang, L.; Meng, Y.; Prakapenka, V.; Mao, W. L.

    2011-12-01

    Determining the phase relations in the system MgO-FeO-SiO2 at high pressure (P) and high temperature (T) is of fundamental importance for understanding the geochemical and geophysical properties of Earth's deep interior. The phase relations in the upper lower mantle have been investigated both in a diamond anvil cell (DAC) [1] and a multi-anvil apparatus [2]. In this study, we investigated the phase relations in (Mg0.6Fe0.4)SiO3 at elevated P-T conditions (up to 80 GPa and 3000 K) by in-situ X-ray diffraction (XRD) measurements in a DAC. Each sample was compressed to the P of interest and then heated to high T. In-situ XRD data were collected at high P-T and then the sample was quenched to preserve the high P-T chemical composition. Samples were recovered and phase chemistry was obtained by scanning electron microscope (SEM) and energy dispersive X-ray spectroscopy (EDS) analysis. Fe solubility in Pv phase increases with increasing P up to 80 GPa. (Mg0.6Fe0.4)SiO3 Pv formed at 80 GPa and its unit-cell volume is 1.8 % larger than that of Fe-free Pv (Lundin et al., 1991). Our improved knowledge of the phase relations in the mid-lower mantle and related geophysical implications will be discussed.

  13. 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.

  14. 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.

  15. 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.

  16. 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.

  17. The Crystal Structure of Micro- and Nanopowders of ZnS Studied by EPR of Mn2+ and XRD

    NASA Astrophysics Data System (ADS)

    Nosenko, Valentyna; Vorona, Igor; Grachev, Valentyn; Ishchenko, Stanislav; Baran, Nikolai; Becherikov, Yurii; Zhuk, Anton; Polishchuk, Yuliya; Kladko, Vasyl; Selishchev, Alexander

    2016-11-01

    The crystal structure of micro- and nanopowders of ZnS doped with different impurities was analyzed by the electron paramagnetic resonance (EPR) of Mn2+ and XRD methods. The powders of ZnS:Cu, ZnS:Mn, ZnS:Co, and ZnS:Eu with the particle sizes of 5-7 μm, 50-200 nm, 7-10 μm, and 5-7 nm, respectively, were studied. Manganese was incorporated in the crystal lattice of all the samples as uncontrolled impurity or by doping. The Mn2+ ions were used as EPR structural probes. It is found that the ZnS:Cu has the cubic structure, the ZnS:Mn has the hexagonal structure with a rhombic distortion, the ZnS:Co is the mixture of the cubic and hexagonal phases in the ratio of 1:10, and the ZnS:Eu has the cubic structure and a distorted cubic structure with stacking defects in the ratio 3:1. The EPR technique is shown to be a powerful tool in the determination of the crystal structure for mixed-polytype ZnS powders and powders with small nanoparticles. It allows observation of the stacking defects, which is revealed in the XRD spectra.

  18. A study on the extent of exchange coupling between (Ba0.5Sr0.5Fe12O19)1-x(CoFe2O4)x magnetic nanocomposites synthesized by solgel combustion method

    NASA Astrophysics Data System (ADS)

    Harikrishnan, V.; Ezhil Vizhi, R.

    2016-11-01

    One step citrate gel combustion method followed by high temperature annealing was employed for preparing (Ba0.5Sr0.5Fe12O19)1-x(CoFe2O4)x (x=0.1, 0.2, and 0.3) composite ferrite powders. The powders were subjected to annealing at 800 °C in order to decisively study the phase evolution of the combined hard and soft ferrites. Thermogravitry (TGA)/differential scanning calorimetry (DSC) analysis exhibited three stages of decomposition in the precursor gels combined with an exothermic peak at 210 °C. X-ray diffraction (XRD) analysis confirmed that the diffraction peaks were perfectly indexed to the hexagonal magnetoplumbite structure of Ba0.5Sr0.5Fe12O19 and the cubic spinel structure of CoFe2O4. Fourier transform infrared spectroscopy (FT-IR) analysis for the samples showed a Co-O stretching vibration accompanied with Co-O-Co or Fe-O-Fe bands at 1220 cm-1. The morphology of the samples were examined by field emission scanning electron microscope (FE-SEM) and transmission electron microscope (TEM). The crystallinity of a selected sample was evaluated by using the high resolution transmission electron microscope (HR-TEM) and selected area electron diffraction (SAED) pattern. It confirmed the presence of planes comprising the hard and soft phases in the synthesized nanocomposites. The magnetic parameters like saturation magnetization MS, remanent magnetization MR, squareness ratio SR, coercivity HC and magnetic moment μB were evaluated using hysteresis by employing vibrating sample magnetometer (VSM). Maximum HC of 4.7 kOe and MS of 60.4 emu/g were obtained for (Ba0.5Sr0.5Fe12O19)0.9(CoFe2O4)0.1. Switching field distribution curves were analysed by using the demagnetization curve. The exchange coupling between the hard and soft phases were analysed by the dM/dH plots and it indicated the exchange coupling first increased with the increase in the concentration of spinels and then decreased. The possible comparison of exchange coupling between the hard and soft phases

  19. Copper nanoparticles functionalized PE: Preparation, characterization and magnetic properties

    NASA Astrophysics Data System (ADS)

    Reznickova, A.; Orendac, M.; Kolska, Z.; Cizmar, E.; Dendisova, M.; Svorcik, V.

    2016-12-01

    We report grafting of copper nanoparticles (CuNP) on plasma activated high density polyethylene (HDPE) via dithiol interlayer pointing out to the structural and magnetic properties of those composites. The as-synthesized Cu nanoparticles have been characterized by high-resolution transmission electron microscopy (HRTEM/TEM) and UV-vis spectroscopy. Properties of pristine PE and their plasma treated counterparts were studied by different experimental techniques: X-ray photoelectron spectroscopy (XPS), UV-vis spectroscopy, energy dispersive X-ray spectroscopy (EDS), zeta potential, electron spin resonance (ESR) and SQUID magnetometry. From TEM and HRTEM analyses, it is found that the size of high purity Cu nanoparticles is (12.2 ± 5.2) nm. It was determined that in the CuNPs, the copper atoms are arranged mostly in the (111) and (200) planes. Absorption in UV-vis region by these nanoparticles is ranging from 570 to 670 nm. EDS revealed that after 1 h of grafting are Cu nanoparticles homogeneously distributed over the whole surface and after 24 h of grafting Cu nanoparticles tend to aggregate slightly. The combined investigation of magnetic properties using ESR spectrometry and SQUID magnetometry confirmed the presence of copper nanoparticles anchored on PE substrate and indicated ferromagnetic interactions.

  20. 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

  1. 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.

  2. 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.

  3. Investigation of structural resorption behavior of biphasic bioceramics with help of gravimetry, μCT, SEM, and XRD.

    PubMed

    de Wild, Michael; Amacher, Fabienne; Bradbury, Christopher R; Molenberg, Aart

    2016-04-01

    Resorbable bone substitute materials are widely used for bone augmentation after tumor resection, parallel to implant placement, or in critical size bone defects. In this study, the structural dissolution of a biphasic calcium phosphate bone substitute material with a hydroxyapatite (HA)/tricalcium phosphate (β-TCP) ratio of 60/40 was investigated by repeatedly placing porous blocks in EDTA solution at 37 °C. At several time points, the blocks were investigated by SEM, µCT, and gravimetry. It was found that always complete 2-3 µm sized grains were removed from the structure and that the β-TCP is dissolved more rapidly. This selective dissolution of the β-TCP grains was confirmed by XRD measurements. The blocks were eroded from the outside toward the center. The structure remained mechanically stable because the central part showed a delayed degradation and because the slower dissolving HA grains preserved the integrity of the structure.

  4. 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.

  5. 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.

  6. Degradation of dental ZrO2-based materials after hydrothermal fatigue. Part I: XRD, XRF, and FESEM analyses.

    PubMed

    Perdigão, Jorge; Pinto, Ana M; Monteiro, Regina C C; Braz Fernandes, Francisco M; Laranjeira, Pedro; Veiga, João P

    2012-01-01

    The aim was to investigate the effect of simulated low-temperature degradation (s-LTD) and hydrothermal fatigue on the degradation of three ZrO(2)-based dental materials. Lava, IPS, and NanoZr discs were randomly assigned to (1) Control-Storage in distilled water at 37°C; (2) Aging at 134°C for 5 h (s-LTD); (3) Thermocycling in saliva for 30,000 cycles (TF). XRD revealed that ZrO(2) m phase was identified in all groups but TF increased the m phase only for Lava. Under the FESEM, Lava showed no alterations under s-LTD, but displayed corrosion areas up to 60 µm wide after TF. We conclude that TF accelerated the degradation of Lava through an increase in the m phase and grain pull-out from the material surface.

  7. 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.

  8. Identification of reaction compounds in micrometric layers from gothic paintings using combined SR-XRD and SR-FTIR.

    PubMed

    Salvadó, Nati; Butí, Salvador; Nicholson, James; Emerich, Hermann; Labrador, Ana; Pradell, Trinitat

    2009-07-15

    Synchrotron radiation X-ray diffraction (micro-SR-XRD) and Fourier transform infrared spectroscopy (micro-SR-FTIR) are used in the non-destructive identification of reaction and aging compounds from micrometric ancient painting layers. The combination of the micrometer size and non-destructive nature of the techniques together with the high resolution and brilliance of the synchrotron radiation has proved to be a procedure most advantageous for the study of reaction, aging and degradation processes. Copper, lead and calcium carboxylates and oxalates are determined in the chromatic, preparation and alteration layers from 15th century egg tempera and oil paintings. Their nature and crystallinity have been assessed. Some hypothesis about the mechanisms of development of both carboxylates and oxalates are presented.

  9. Fe3O4/salicylic acid nanoparticles versatility in magnetic mediated vascular nanoblockage

    NASA Astrophysics Data System (ADS)

    Mîndrilă, I.; Buteică, S. A.; Mihaiescu, D. E.; Badea, G.; Fudulu, A.; Mărgăritescu, D. N.

    2016-01-01

    An aqueous dispersion of Fe3O4/salicylic acid magnetic nanoparticles (SaMNPs) was synthesized by a modified Massart method, characterized by Inductively Coupled Plasma-Optic Emission Spectrometry (ICP-OES), High-Resolution Transmission Electron Microscopy (HRTEM) and Dynamic Light Scattering (DLS) methods, and tested on the chick chorioallantoic membrane (CAM) model to evaluate biocompatibility, biodistribution, intravascular time persistence, and ability to be magnetically target driven in order to block the blood supply into a tumor xenograft. ICP-OES, DLS, and HRTEM SaMNPs sample analyses showed a 0.356 mg/mL Fe concentration, a good stability in water (average Zeta potential of 39.3 mV), a hydrodynamic diameter around 52 nm and a core diameter in the 7-15 nm range for the Fe3O4 nanoparticles. In vivo CAM assay showed that SaMNPs were biocompatible with the chick embryo, were fixed almost completely by the liver, had no embolic potential, and a threshold-dose-dependent intravascular magnetic targeting time. Study on the CAM tumor model showed that SaMNPs could be used for long-term magnetically mediated nanoblocking of the capillary networks and 70-µm smaller arterioles.

  10. Magnetite and magnetite/silver core/shell nanoparticles with diluted magnet-like behavior

    SciTech Connect

    Garza-Navarro, Marco; Gonzalez, Virgilio; Ortiz, Ubaldo; De la Rosa, Elder

    2010-01-15

    In the present work is reported the use of the biopolymer chitosan as template for the preparation of magnetite and magnetite/silver core/shell nanoparticles systems, following a two step procedure of magnetite nanoparticles in situ precipitation and subsequent silver ions reduction. The crystalline and morphological characteristics of both magnetite and magnetite/silver core/shell nanoparticles systems were analyzed by high resolution transmission electron microscopy (HRTEM) and nanobeam diffraction patterns (NBD). The results of these studies corroborate the core/shell morphology and the crystalline structure of the magnetite core and the silver shell. Moreover, magnetization temperature dependent, M(T), measurements show an unusual diluted magnetic behavior attributed to the dilution of the magnetic ordering in the magnetite and magnetite/silver core/shell nanoparticles systems. - Graphical abstract: Biopolymer chitosan was used as stabilization media to synthesize both magnetite and magnetite/silver core/shell nanoparticles. Results of HRTEM and NBD patterns confirm core/shell morphology of the obtained nanoparticles. It was found that the composites show diluted magnet-like behavior.

  11. 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

  12. Multivariate analysis of DSC-XRD simultaneous measurement data: a study of multistage crystalline structure changes in a linear poly(ethylene imine) thin film.

    PubMed

    Kakuda, Hiroyuki; Okada, Tetsuo; Otsuka, Makoto; Katsumoto, Yukiteru; Hasegawa, Takeshi

    2009-01-01

    A multivariate analytical technique has been applied to the analysis of simultaneous measurement data from differential scanning calorimetry (DSC) and X-ray diffraction (XRD) in order to study thermal changes in crystalline structure of a linear poly(ethylene imine) (LPEI) film. A large number of XRD patterns generated from the simultaneous measurements were subjected to an augmented alternative least-squares (ALS) regression analysis, and the XRD patterns were readily decomposed into chemically independent XRD patterns and their thermal profiles were also obtained at the same time. The decomposed XRD patterns and the profiles were useful in discussing the minute peaks in the DSC. The analytical results revealed the following changes of polymorphisms in detail: An LPEI film prepared by casting an aqueous solution was composed of sesquihydrate and hemihydrate crystals. The sesquihydrate one was lost at an early stage of heating, and the film changed into an amorphous state. Once the sesquihydrate was lost by heating, it was not recovered even when it was cooled back to room temperature. When the sample was heated again, structural changes were found between the hemihydrate and the amorphous components. In this manner, the simultaneous DSC-XRD measurements combined with ALS analysis proved to be powerful for obtaining a better understanding of the thermally induced changes of the crystalline structure in a polymer film.

  13. Synthesis and magnetic properties of nickel nanoparticles

    NASA Astrophysics Data System (ADS)

    Singh, Jaiveer; Patel, Tarachand; Kaurav, Netram; Okram, Gunadhor S.

    2016-05-01

    Monodisperse nickel nanoparticles (Ni-NPs) were synthesized via a thermal decomposition process. The NPs were characterized by X-ray diffraction (XRD) and transmission electron microscopy (TEM). They were spherical with mean diameter of 4 nm. Zero field cooled (ZFC) and field cooled (FC) magnetization versus temperature data displayed interesting magnetic interactions. ZFC showed a peak at 4.49 K, indicating the super paramagnetic behavior. Magnetic anisotropic constant was estimated to be 4.62×105 erg/cm3 and coercive field was 168 Oe at 3 K.

  14. 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.

  15. Diagnosis of the heating effect on the electrical resistivity of Ouargla (Algeria) dunes sand using XRD patterns and FTIR spectra

    NASA Astrophysics Data System (ADS)

    Mechri, Mohammed Laïd; Chihi, Smaïl; Mahdadi, Naouia; Beddiaf, Samiha

    2017-01-01

    XRD patterns and FTIR spectra have shown that dunes sand of Ouargla's region, in its natural state, is formed of a high percentage of quartz, gypsum and very low percentage of kaolinite and hematite, in addition to some organic compounds. The electrical resistivity of the natural sand has been measured, it was 6 × 1014 Ω cm. Six samples of the sand were heated separately at 200, 400, 600, 800, 1000 and 1200 °C. The XRD patterns and FTIR spectra of these samples were carried out. On the other hand, the electrical resistivities of these samples have been measured. The change of the electrical resistivity with heat shows a nonlinear behavior. The heated sample of sand at 200 °C has lost some water. Most of the gypsum in the 200 °C heated sample has transformed into anhydrite, and the rest has transformed into bassanite, and its electrical resistivity has fallen down to 3.5 × 1014 Ω cm. By heating at 400 °C, the gypsum has lost all its water and it has transformed entirely to anhydrite, and its electrical resistivity became 6.75 × 1012 Ω cm, it has the lowest measured resistivity. At 600 °C and 800 °C, in addition to anhydrite, the kaolinite transformed to meta-kaolin due to the continuous breaking of OH bond and formation of water vapor, and the electrical resistivity increased to (1.5-1.9) × 1014 Ω cm. Heating at 1000 °C leads to the initiation of the interaction between anhydrite and quartz, the wollastonite appears, and the meta-kaolin transforms to aluminum-silicon and cristobalite. The wollastonite is a good electrical insulator. It raises the electrical resistivity of sand to 2.6 × 1014 Ω cm. The heating at 1200 °C makes all anhydrite to interact with quartz due to the increasing of volume of wollastonite, the anhydrite disappears completely, the quartz transforms into cristobalite. The cristobalite increases due to the dissociation of aluminium-silicon into mullite and cristobalite, as well as the transformation of quartz into cristobalite at

  16. Single crystal XRD structure and theoretical analysis of the chiral Au30S(S-t-Bu)18 cluster.

    PubMed

    Crasto, David; Malola, Sami; Brosofsky, Grace; Dass, Amala; Häkkinen, Hannu

    2014-04-02

    Au30S(S-t-Bu)18 cluster, related closely to the recently isolated "green gold" compound Au30(S-t-Bu)18, has been structurally solved via single-crystal XRD and analyzed by density functional theory calculations. The molecular protecting layer shows a combination of monomeric (RS-Au-SR) and trimeric (RS-Au-SR-Au-SR-Au-SR) gold-thiolate units, bridging thiolates, and a single sulfur (sulfide) in a novel μ3-coordinating position. The chiral gold core has a geometrical component that is identical to the core of the recently reported Au28(SPh-t-Bu)20. Both enantiomers of Au30S(S-t-Bu)18 are found in the crystal unit cell. The calculated CD spectrum bears a close resemblance to that of Au28(SPh-t-Bu)20. This is the first time when two structurally characterized thiol-stabilized gold clusters are found to have such closely related metal core structures and the results may increase understanding of the formation of gold clusters when stabilized by bulky thiolates.

  17. Influence of temperature on layer growth as measured by in situ XRD observation of nitriding of austenitic stainless steel

    NASA Astrophysics Data System (ADS)

    Manova, D.; Günther, C.; Bergmann, A.; Mändl, S.; Neumann, H.; Rauschenbach, B.

    2013-07-01

    Investigating the formation of expanded austenite has resulted in several, different models trying to explain the particular diffusion and phase formation behaviour. However, only ex situ information, influenced by cooling and annealing processes of the samples after ion implantation has been available until now. Here, the time and temperature dependent layer growth is reported using in situ XRD measurements obtained from low energy broadbeam nitrogen ion implantation into polycrystalline austenitic stainless steel 304 in the temperature range from 300 to 500 °C for a process time of up to 1 h. Expanded austenite was observed at all temperatures without any CrN, in agreement with already published lifetime data for this metastable phase. The layer growth was derived from the time evolution of the substrate peak intensity. Using the temperature dependence of the layer growth, an activation energy of nearly 0.8 eV was estimated for the nitrogen diffusion. In contrast, a complex behaviour was observed for the lattice expansion and peak width of the expanded peak, indicating additional dynamic annealing during implantation.

  18. 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.

  19. 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.

  20. Mechanical properties and XRD studies of silicon carbide inert matrix fuel fabricated by a low temperature polymer precursor route

    NASA Astrophysics Data System (ADS)

    Shih, Chunghao; Rohbeck, Nadia; Gopalakrishnan, Karthik; Tulenko, James S.; Baney, Ronald H.

    2013-01-01

    The mechanical properties of silicon carbide (SiC) inert matrix fuel (IMF) pellets fabricated by a low temperature (1050 °C) polymer precursor route were evaluated at room temperature. The Vickers hardness was mainly related to the chemical bonding strength between the amorphous SiC phase and the β-SiC particles. The biaxial fracture strength with pre-notch and fracture toughness were found to be mostly controlled by the pellet density. The maximum Vickers hardness, biaxial fracture strength with pre-notch and fracture toughness achieved were 5.6 GPa, 201 MPa and 2.9 MPa m1/2 respectively. These values appear to be superior to the reference MOX or UO2 fuels. Excellent thermal shock resistance for the fabricated SiC IMF was proven and the values were compared to conventional UO2 pellets. XRD studies showed that ceria (PuO2 surrogate) chemically reacted with the polymer precursor during sintering, forming cerium oxysilicate. Whether PuO2 will chemically react in a similar manner remains unclear.

  1. Composite uranium carbide targets at TRIUMF: Development and characterization with SEM, XRD, XRF and L-edge densitometry

    NASA Astrophysics Data System (ADS)

    Kunz, Peter; Bricault, Pierre; Dombsky, Marik; Erdmann, Nicole; Hanemaayer, Vicky; Wong, John; Lützenkirchen, Klaus

    2013-09-01

    The production of radioactive ion beams (RIB) from spallation targets by irradiation with a continuous 500 MeV proton beam, has been routine at TRIUMF for several years. Based on the experience with composite refractory carbide targets a procedure for the fabrication of UC2/C targets was developed. It includes the preparation of UC2 by carbothermal reduction of UO2, the slip-casting of fine-grained UC2/C slurry on graphite foil under inert gas atmosphere and the cutting of composite target discs which are stacked up to a lamellar structure. The thermal properties of such an arrangement are adequate to withstand the high power deposition of an intense, continuous proton beam and also beneficial for the fast release of short-lived radioactive isotopes. Molecular structure, particle size and the impact of sintering of the target discs were investigated via XRD and SEM. Thickness and mass distribution were measured with position-sensitive LIII-edge densitometry. The results confirm that the properties of the UC2/C target material are well suited for RIB production at TRIUMF while there is still room for improvement with regard to uniformity of mass distribution in target disc thickness.

  2. Simplified Procedure for Estimating Epitaxy of La2Zr2O7-Buffered NiW RABITS Using XRD

    SciTech Connect

    Rikel, Mark O.; Isfort, Dirk; Klein, Marcel; Ehrenberg, Jurgen; Bock, Joachim; Specht, Eliot D; Sun-Wagener, Ming; Weber, Oxana; Sporn, Dieter; Engel, Sebastian; de Haas, Oliver; Semerad, Robert; Schubert, Margitta; Holzapfel, Bernhard

    2009-01-01

    Abstract A procedure is developed for assessing the epitaxy of La(2-x)Zr(2+x)O(7) (LZO) layers on NiW RABITS. Comparing XRD patterns (theta / 2-theta scans and 2D rocking curves) of LZO films of known thickness (ellipsometry or reflectometry measurements) with those of standard samples (100% epitaxial LZO film and an isotropic LZO pellet of known density), we estimate the epitaxial (EF), and polycrystalline (PF) fractions of LZO within the layer. The procedure was tested using MOD-LZO(100 nm)/NiW tape samples with varied from 3 to 90% (reproducibly prepared by varying the humidity of Ar-5%H2 gas during heat treatment). A qualitative agreement with RHEED and quantitative (within 10%) agreement with the EBSD results was shown. Correlation between EF and Jc in 600 nm thick YBCO layer deposited on MOD-LZO/NiW using thermal coevaporation enables us to impose the EF=80% margin on the quality of LZO layer for the particular conductor architecture.

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

    NASA Astrophysics Data System (ADS)

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

    2010-03-01

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

  4. Magnetic properties of cobalt ferrite synthesized by hydrothermal method

    NASA Astrophysics Data System (ADS)

    Allaedini, Ghazaleh; Tasirin, Siti Masrinda; Aminayi, Payam

    2015-05-01

    In this study, the magnetic properties of nanocrystalline cobalt ferrite synthesized via the hydrothermal method have been investigated. The structural properties of the produced powders were investigated using X-ray diffraction (XRD) and scanning electron microscopy (SEM). The observed XRD pattern confirmed the spinel/cubic structure of the prepared cobalt ferrite. The SEM pictures show that the simple hydrothermal method produces uniform sphere-shaped nanopowders. Moreover, infrared spectroscopy was used to confirm the formation of cobalt ferrite particles. Magnetic hysteresis was measured using a vibrating sample magnetometer in a maximum field of 10 kOe. The magnetization of the prepared nanoparticles was investigated, and the saturation magnetization ( M s), remanence ( M r), and coercivity ( H c) were derived from the hysteresis loops. The results revealed that the cobalt ferrite nanoparticles synthesized via the simple hydrothermal method exhibit superior magnetic properties.

  5. Characterization of magnetic material in the mound-building termite Macrotermes gilvus in Southeast Asia

    NASA Astrophysics Data System (ADS)

    Esa, Mohammad Faris Mohammad; Rahim, Faszly; Hassan, Ibrahim Haji; Hanifah, Sharina Abu

    2015-09-01

    Magnetic material such as magnetite are known as particles that respond to external magnetic field with their ferromagnetic properties as they are believed contribute to in responding to the geomagnetic field. These particles are used by terrestrial animals such as termites for navigation and orientation. Since our earth react as giant magnetic bar, the magnitude of this magnetic field present by intensity and direction (inclination and direction). The magnetic properties and presence of magnetite in termites Macrotermes gilvus, common mound-building termite were tested. M. gilvus termites was tested with a Vibrating Sample Magnetometer VSM to determine the magnetic properties of specimen. The crushed body sample was characterized with X-Ray Diffraction XRD to show the existent of magnetic material (magnetite) in the specimens. Results from VSM indicate that M. gilvus has diamagnetism properties. The characterization by XRD shows the existent of magnetic material in our specimen in low concentration.

  6. Characterization of magnetic material in the mound-building termite Macrotermes gilvus in Southeast Asia

    SciTech Connect

    Esa, Mohammad Faris Mohammad; Hassan, Ibrahim Haji; Rahim, Faszly; Hanifah, Sharina Abu

    2015-09-25

    Magnetic material such as magnetite are known as particles that respond to external magnetic field with their ferromagnetic properties as they are believed contribute to in responding to the geomagnetic field. These particles are used by terrestrial animals such as termites for navigation and orientation. Since our earth react as giant magnetic bar, the magnitude of this magnetic field present by intensity and direction (inclination and direction). The magnetic properties and presence of magnetite in termites Macrotermes gilvus, common mound-building termite were tested. M. gilvus termites was tested with a Vibrating Sample Magnetometer VSM to determine the magnetic properties of specimen. The crushed body sample was characterized with X-Ray Diffraction XRD to show the existent of magnetic material (magnetite) in the specimens. Results from VSM indicate that M. gilvus has diamagnetism properties. The characterization by XRD shows the existent of magnetic material in our specimen in low concentration.

  7. Magnetic hardening of high-energy ball-milled nanocrystalline LaMn 2Si 2

    NASA Astrophysics Data System (ADS)

    Elmali, Ayhan; Tekerek, Simsek; Dincer, Ilker; Elerman, Yalcin; Theissmann, Ralf; Ehrenberg, Helmut; Fuess, Hartmut

    Nanocrystalline LaMn 2Si 2 powders have been obtained by high-energy ball milling for 30 min from bulk alloys. After milling a high coercivity about 6 kOe is observed at 10 K in contrast to neglectable coercivity for the bulk LaMn 2Si 2 at 5 K. The average grain size of the optimum particles which is obtained from X-ray diffraction pattern and HRTEM picture is about 20 nm. The magnetic hardening is observed for the nanocrystalline LaMn 2Si 2, reflected in the coercivity field strength of 6 kOe at 10 K.

  8. Specialty magnets

    SciTech Connect

    Halbach, K.

    1986-07-01

    A number of basic conceptual designs are explained for magnet systems that use permanent magnet materials. Included are iron free multipoles and hybrid magnets. Also appended is a discussion of the manufacturing process and magnetic properties of some permanent magnet materials. (LEW)

  9. 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.

  10. Influence of a silica interlayer on the structural and magnetic properties of sol-gel TiO₂-coated magnetic nanoparticles.

    PubMed

    De Matteis, Laura; Fernández-Pacheco, Rodrigo; Custardoy, Laura; García-Martín, María L; de la Fuente, Jesús M; Marquina, Clara; Ibarra, M Ricardo

    2014-05-13

    Superparamagnetic iron oxide nanoparticles coated with titanium dioxide have been synthesized, growing the titanium dioxide directly either on the magnetic nuclei or on magnetic nanoparticles previously coated with a semihydrophobic silica layer. Both coatings have been obtained by sol-gel. Since it is well-known that the existence of the intermediate silica layer influences the physicochemical properties of the material, a detailed characterization of both types of coatings has been carried out. The morphology, structure, and composition of the synthesized nanomatrices have been locally analyzed with subangstrom spatial resolution, by means of aberration corrected transmission electron microscopy (HRTEM and STEM-HAADF). Besides magnetization measurements, proton relaxivity experiments have been also performed on water suspensions of the as-synthesized nanoparticles to investigate the role of the silica interlayer in the relaxometric properties. The silica interlayer leads to nanoparticles with much higher water stability and to higher relaxivity of the suspensions.

  11. Mercury in polluted soils: speciation using micro-XRF, micro-XRD, and micro- and bulk XAFS.

    NASA Astrophysics Data System (ADS)

    Terzano, R.; Santoro, A.; Spagnuolo, M.; Vekemans, B.; Medici, L.; Janssens, K.; Goettlicher, J.; Denecke, M. A.; Mangold, S.; Ruggiero, P.

    2009-04-01

    In this research, mercury speciation was assessed for soil samples collected inside and outside an industrial polluted area of National environmental interest located in "Val Basento" (Basilicata, Italy). Hg concentration in these soil samples ranged from 12 up to 240 mg/kg. Mercury chemical forms in these samples were identified by a combination of sequential extraction procedures, thermal desorption analyses, and different bulk- and micro-analytical techniques exploiting high intensity synchrotron generated X-rays. Bulk XANES (X-ray Absorption Near Edge Structure) and EXAFS (Extended X-ray Absorption Fine Structure) spectra were collected for direct Hg-speciation in soil samples sieved at 2mm as well as in the clay fraction (<2um), where the highest amount of mercury was concentrated. The interpretation of the complex mixture of Hg-chemical forms in the soil samples was made simpler by performing, beside bulk XAS investigations, microanalyses on soil thin sections by combined u-XRF/u-XRD (micro X-ray Fluorescence/micro X-ray Diffraction) and u-XANES, with a resolution of 20 um. The information deriving from the micro-scale was then used to understand the bulk data. m-XRF maps were collected to localize microscopic Hg-containing particles in areas of several hundreds of mm2. Simultaneous to u-XRF spectra, microdiffraction patterns were collected in each point of the map, to identify possible crystalline Hg-mineral forms or mineral associations. Once points of interest were localized, u-XANES spectra were also collected. In general, two main representative XANES spectra (S1 and S2) were observed from Hg-rich spots at the microscopic level. Interestingly, all the bulk XANES spectra from all soil samples could be fitted by a linear combination of the microscopic S1 and S2 spectra. Therefore, by fitting the S1 and S2 spectra by means of known standard spectra it was then possible to decipher Hg-speciation for all the soil samples. In conclusion, the main constituents

  12. Magnetic testing

    NASA Technical Reports Server (NTRS)

    Pasley, R. L.; Barton, J. R.

    1973-01-01

    Magnetic techniques are described for the nondestructive evaluation of defects in materials. The physical principles, and the magnetic-particle method are discussed along with magnetic-hysteresis measurements and electric current perturbations.

  13. 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.

  14. 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.

  15. Synthesis, dynamic NMR characterization and XRD studies of novel N,N’-substituted piperazines for bioorthogonal labeling

    PubMed Central

    Pretze, Marc; Gott, Matthew; Köckerling, Martin

    2016-01-01

    Novel, functionalized piperazine derivatives were successfully synthesized and fully characterized by 1H/13C/19F NMR, MS, elemental analysis and lipophilicity. All piperazine compounds occur as conformers resulting from the partial amide double bond. Furthermore, a second conformational shape was observed for all nitro derivatives due to the limited change of the piperazine chair conformation. Therefore, two coalescence points were determined and their resulting activation energy barriers were calculated using 1H NMR. To support this result, single crystals of 1-(4-nitrobenzoyl)piperazine (3a, monoclinic, space group C2/c, a = 24.587(2), b = 7.0726(6), c = 14.171(1) Å, β = 119.257(8)°, V = 2149.9(4) Å3, Z = 4, D obs = 1.454 g/cm3) and the alkyne derivative 4-(but-3-yn-1-yl)-1-(4-fluorobenzoyl)piperazine (4b, monoclinic, space group P21/n, a = 10.5982(2), b = 8.4705(1), c = 14.8929(3) Å, β = 97.430(1)°, V = 1325.74(4) Å3, Z = 4, D obs = 1.304 g/cm3) were obtained from a saturated ethyl acetate solution. The rotational conformation of these compounds was also verified by XRD. As proof of concept for future labeling purposes, both nitropiperazines were reacted with [18F]F–. To test the applicability of these compounds as possible 18F-building blocks, two biomolecules were modified and chosen for conjugation either using the Huisgen-click reaction or the traceless Staudinger ligation. PMID:28144316

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

    PubMed Central

    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) × 10-5 s-1 for a solution:solid of 10:1 and 1.6 (± 0.8) × 10-4 s-1 for a solution:solid of 5:1 (batch mode; T = 150°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 δiso = 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

  17. Structural and magnetic properties of L10 -FePt nanoparticles aligned by external magnetic field

    NASA Astrophysics Data System (ADS)

    Tamada, Yoshinori; Yamamoto, Shinpei; Nasu, Saburo; Ono, Teruo

    2008-12-01

    We investigated structural and magnetic properties of the easy-axis aligned L10 -FePt nanoparticles by the combined use of x-ray diffraction (XRD), magnetization, and F57e Mössbauer measurements. The L10 -FePt nanoparticles were fixed in a polystyrene matrix by performing free radical polymerization of styrene under an aligning external magnetic field. Mössbauer spectrum of the L10 -FePt nanoparticles/polystyrene composite showed tremendous decrease in the second and fifth absorption lines under the condition that the incident γ ray was parallel to the aligning field. This result indicates that the easy axes of the L10 -FePt nanoparticles in the composite have a strong preferred orientation with a finite distribution. We estimated the distribution of easy-axis orientation by using the Mössbauer hyperfine parameters, which is in good agreement with that determined by the XRD rocking curve.

  18. Magnetic measurements on α−CS{sub 2}U{sub 4}O{sub 12}

    SciTech Connect

    Kanrar, Buddhadev Misra, N. L.; Sastry, P. U.; Dube, V.; Ravikumar, G.

    2014-04-24

    Magnetic and XRD measurements on α−CS{sub 2}U{sub 4}O{sub 12} having uranium in mixed valent states of U (V) and U (VI) have been made. The study reveals that the compound undergoes an antiferromagnetic transition below 25K and an anomalous magnetic behavior was seen around 75K. This anomalous behavior indicates towards a structural phase transition. However, the low temperature XRD could not confirm this observation.

  19. Exchange bias in ferrite hollow nanoparticles originated by complex internal magnetic structure

    NASA Astrophysics Data System (ADS)

    De Biasi, Emilio; Lima, Enio, Jr.; Vargas, Jose M.; Zysler, Roberto D.; Arbiol, Jordi; Ibarra, Alfonso; Goya, Gerardo F.; Ibarra, M. Ricardo

    2015-10-01

    Iron-oxide hollow nanospheres (HNS) may present unusual magnetic behavior as a consequence of their unique morphology. Here, we report the unusual magnetic behavior of HNS that are 9 nm in diameter. The magnetic properties of HNS originate in their complex magnetic structure, as evidenced by Mössbauer spectroscopy and magnetization measurements. We observe a bias in the hysteresis when measured at very low temperature in the field cooling protocol (10 kOe). In addition, dc (static) and ac (dynamic) magnetization measurements against temperature and applied field reveal a frustrated order of the system below 10 K. High-resolution transmission electron microscopy (HRTEM) studies reveal that the HNS are composed of small crystalline clusters of about 2 nm in diameter, which behave as individual magnetic entities. Micromagnetic simulations (using conjugate gradient in order to minimize the total energy of the system) reproduce the experimentally observed magnetic behavior. The model considers the hollow particles as constituted by small ordered clusters embedded in an antiferromagnetic environment (spins localized outside the clusters). In addition, the surface spins (in both inner and outer surfaces of the HNS) are affected by a local surface anisotropy. The strong effective magnetic anisotropy field of the clusters induces the bias observed when the system is cooled in the presence of a magnetic external field. This effect propagates through the exchange interaction into the entire particle.

  20. Neodymium Magnets.

    ERIC Educational Resources Information Center

    Wida, Sam

    1992-01-01

    Uses extremely strong neodymium magnets to demonstrate several principles of physics including electromagnetic induction, Lenz's Law, domain theory, demagnetization, the Curie point, and magnetic flux lines. (MDH)

  1. 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.

  2. Following the Formation of Active Co(III) Sites in Cobalt Substituted Aluminophosphates Catalysts by In-Situ Combined UV-VIS/XAFS/XRD Technique

    SciTech Connect

    Sankar, Gopinathan; Fiddy, Steven; Harvey, Ian; Hayama, Shusaku; Bushnell-Wye, Graham; Beale, Andrew M.

    2007-02-02

    Cobalt substituted aluminophosphates, CoAlPO-34 (Chabazite structure) and DAF-8 (Phillipsite structure) were investigated by in situ combined XRD/EXAFS/UV-VIS technique. In-situ combined XRD, Co K-edge EXAFS and UV-Vis measurements carried out during the calcination process reveal that CoAlPO-34 containing 10 wt percent cobalt is stable and the cobalt ions are converted from Co(II) in the as synthesised form to Co(III); DAF-8 containing about 25 percent cobalt is not stable and does not show change in oxidation state.

  3. Synthesis, characterization and magnetic properties of Fe3O4 doped chitosan polymer

    NASA Astrophysics Data System (ADS)

    Karaca, E.; Şatır, M.; Kazan, S.; Açıkgöz, M.; Öztürk, E.; Gürdağ, G.; Ulutaş, D.

    2015-01-01

    Fe3O4 nanoparticles doped into chitosan films were prepared by the solution casting technique. Various samples were synthesized in atmospheric medium and in vacuum. The morphological properties of the samples were characterized by high resolution transmission electron microscopy (HR-TEM) and Scanning Electron Microscopy (SEM). The structural, magnetic, and microwave absorption properties of magnetic chitosan films have been carried out using the Vibrating Sample Magnetometer (VSM) and Ferromagnetic Resonance (FMR). It is shown that the composite polymer behaves like a superparamagnetic material with high blocking temperature. The effective magnetization shows gradual increments with the concentration of dopant Fe3O4 nanoparticles. The microwave absorption characteristic of superparamagnetic composite polymer shows low reflection loss.

  4. Magnetic Levitation.

    ERIC Educational Resources Information Center

    Rossing, Thomas D.; Hull, John R.

    1991-01-01

    Discusses the principles of magnetic levitation presented in the physics classroom and applied to transportation systems. Topics discussed include three classroom demonstrations to illustrate magnetic levitation, the concept of eddy currents, lift and drag forces on a moving magnet, magnetic levitation vehicles, levitation with permanent magnets…

  5. Magnetic Spinner

    ERIC Educational Resources Information Center

    Ouseph, P. J.

    2006-01-01

    A science toy sometimes called the "magnetic spinner" is an interesting class demonstration to illustrate the principles of magnetic levitation. It can also be used to demonstrate Faraday's law and a horizontally suspended physical pendulum. The levitated part contains two circular magnets encased in a plastic housing. Each magnet stays…

  6. Magnetic interaction in oxygenated alpha Fe-phthalocyanines

    SciTech Connect

    Kuzmann, Ernő Homonnay, Zoltán; Horváth, Attila; Pechousek, Jiri; Cuda, Jan; Machala, Libor; Zoppellaro, Giorgio; Zboril, Radek; Klencsár, Zoltán; Kubuki, Shiro; Nath, Amar

    2014-10-27

    Alpha iron phthalocyanines (α-FePc) oxygenated at low temperatures were investigated with the help of {sup 57}Fe Mössbauer spectroscopy, magnetization measurements (SQUID) and X-ray diffractometry (XRD). Mössbauer spectroscopy revealed that upon oxygenation of α-FePc, new species were formed which could be associated with Fe{sup III}Pc oxygen adducts. Unexpectedly, magnetically split spectrum of oxygenated α-FePc was observed below 20 K. In-field Mössbauer spectra in a 5 T external magnetic field at 5K and magnetization measurements indicate antiferromagnetic coupling in oxygenated α-FePc.

  7. Interplay of structural, optical and magnetic properties in Gd doped CeO{sub 2}

    SciTech Connect

    Soni, S.; Dalela, S.; Kumar, Sudish; Meena, R. S.; Vats, V. S.

    2015-06-24

    In this research wok systematic investigation on the synthesis, characterization, optical and magnetic properties of Ce{sub 1-x}Gd{sub x}O{sub 2} (where x=0.02, 0.04, 0.06, and 0.10) synthesized using the Solid-state method. Structural, Optical and Magnetic properties of the samples were investigated by X-ray diffraction (XRD), UV-VIS-NIR spectroscopy and VSM. Fluorite structure is confirmed from the XRD measurement on Gd doped CeO{sub 2} samples. Magnetic studies showed that the Gd doped polycrystalline samples display room temperature ferromagnetism and the ferromagnetic ordering strengthens with the Gd concentration.

  8. Comparative Study by MS and XRD of Fe50Al50 Alloys Produced by Mechanical Alloying, Using Different Ball Mills

    NASA Astrophysics Data System (ADS)

    Rojas Martínez, Y.; Pérez Alcázar, G. A.; Bustos Rodríguez, H.; Oyola Lozano, D.

    2005-02-01

    In this work we report a comparative study of the magnetic and structural properties of Fe50Al50 alloys produced by mechanical alloying using two different planetary ball mills with the same ball mass to powder mass relation. The Fe50Al50 sample milled during 48 h using the Fritsch planetary ball mill pulverisette 5 and balls of 20 mm, presents only a bcc alloy phase with a majority of paramagnetic sites, whereas that sample milled during the same time using the Fritsch planetary ball mill pulverisette 7 with balls of 15 mm, presents a bcc alloy phase with paramagnetic site (doublet) and a majority of ferromagnetic sites which include pure Fe. However for 72 h of milling this sample presents a bcc paramagnetic phase, very similar to that prepared with the first system during 48 h. These results show that the conditions used in the first ball mill equipment make more efficient the milling process.

  9. Cooperative use of VCD and XRD for the determination of tetrahydrobenzoisoquinolines absolute configuration: a reliable proof of memory of chirality and retention of configuration in enediyne rearrangements.

    PubMed

    Mondal, Shovan; Naubron, Jean-Valère; Campolo, Damien; Giorgi, Michel; Bertrand, Michéle P; Nechab, Malek

    2013-12-01

    The absolute configurations (AC) of azaheterocylic compounds resulting from the cascade rearrangement of enediynes involving only light atoms were unambiguously assigned by the joint use of vibrational circular dichroism (VCD) and copper radiation single crystal X-ray diffraction (XRD). These AC determinations proved that the rearrangements of enediynes proceeded with memory of chirality and retention of configuration.

  10. Mineralogical In-Situ Investigation of Acid-Sulfate Samples from the Rio Tinto River, Spain, with a Portable XRD/XRF Instrument

    NASA Astrophysics Data System (ADS)

    Sarrazin, P.; Ming, D. W.; Morris, R. V.; Fernández-Remolar, D.; Amils, R.; Arvidson, R. E.; Blake, D.; Bish, D. L.

    2007-03-01

    The CheMin 4 XRD/XRF prototype was deployed in Rio Tinto, Spain, for a field campaign to study river bed sediments and test the potential of an instrument suite in an astrobiological investigation context for future Mars surface robotic missions.

  11. Correlation of cation distribution with the hyperfine and magnetic behaviour of Ni0.3Zn0.4Co0.2Cu0.1Fe2O4 nanoparticles and their microwave absorption properties when encapsulated in multi-walled carbon nanotubes

    NASA Astrophysics Data System (ADS)

    Dalal, Madhumita; Mallick, Ayan; Greneche, Jean-Marc; Das, Dipankar; Chakrabarti, Pabitra K.

    2017-03-01

    Nanocrystalline samples of Ni0.3Zn0.4Co0.2Cu0.1Fe2O4 (NZCCF) are prepared by a simple co-precipitation method. To obtain nanoparticles of different sizes, the as prepared sample is annealed at 400, 600, 800 and 1000 °C. Nanoparticles of the sample annealed at 600 °C are encapsulated in multi-walled carbon nanotubes (MWCNT). To confirm the crystallographic phase, x-ray diffraction (XRD) patterns are analyzed by the Rietveld method and cation distribution in A- and B-sites is estimated from the analysis. Occupancy of Zn2+ ions in A-site and that of Fe3+ ions in B-site increase with the increase of annealing temperature (T A) and lattice parameters lie within 8.365-8.398 Å. Morphology of the encapsulated sample is examined by taking micrographs in high resolution transmission electron microscope (HRTEM). Hyperfine behaviour of the prepared samples is studied by analyzing Mössbauer spectra recorded at room temperature (RT) and 77 K. Average values of isomer shift (IS) are found to decrease with the increase of crystallite size. Static and dynamic magnetic hysteresis loops are recorded to analyze the magnetic properties of the sample. Maximum saturation magnetization of ~75 emu g-1 is obtained for the sample of NZCCF annealed at 800 °C with crystallite size of ~48 nm. Microwave absorption capability of the encapsulated sample is measured by recording the reflection loss in X and K u bands of microwave region of frequency. Maximum value of reflection loss is  -25.71 dB observed at 15.24 GHz for a sample layer thickness of 1 mm. Moreover, the reflection loss is less than  -10 dB for the entire range of observation (8-18 GHz) which shows that MWCNT encapsulated NZCCF could be considered as a potential candidate for applications in microwave devices.

  12. Magnetic properties of Ni and Cu-Ni nanoparticles

    NASA Astrophysics Data System (ADS)

    Ganga, B. G.; Santhosh, P. N.; Thomas, P. John

    2012-06-01

    Ni and Cu-Ni nanoparticles were prepared by solution phase method and crystal phase was identified by XRD. SEM and EDX were used to analyze morphology and elemental composition of nanoparticles. Magnetic measurements indicate that Ni nanoparticles are superparamagnetic at room temperature and blocking temperature is around 103 K. Ferromagnetism is observed in the case of Cu-Ni nanoparticles with decrease in magnetization compared to Ni nanoparticles.

  13. Conduction and magnetization improvement of BiFeO{sub 3} multiferroic nanoparticles by Ag{sup +} doping

    SciTech Connect

    Ahmed, M.A.; Mansour, S.F.; El-Dek, S.I.; Abu-Abdeen, M.

    2014-01-01

    Graphical abstract: HRTEM micrographs of the samples BiFeO{sub 3}. - Highlights: • Flash auto combustion method was successful in the preparation of Ag doped BiFeO{sub 3} in nanosize. • Ag doping results in hexagonal platelet shapes up to x = 0.10, at x ≥ 0.15 needle shape predominates. • Mixed conduction is obtained in Ag doped samples. • This nanometric multiferroic could be recommended as attractive cathode for solid oxide fuel cell. - Abstract: Nanometric multiferroic namely Ag doped (BiFeO{sub 3}) was synthesized using flash auto combustion technique and glycine as a fuel. Single phase rhombohedral–hexagonal perovskite structure was obtained by annealing at 550 °C, as determined from XRD. High resolution transmission electron microscope (HRTEM) clarifies the hexagonal platelet shape with size 17.9 nm. Maximum room temperature AC conductivity was obtained at Ag content of x = 0.10. The results of this study promote the use of such multiferroic in solid oxide fuel cell applications.

  14. 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

  15. 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.

  16. The Role of Mn(2+)-Doping on Structural, Morphological, Optical, Magnetic and Catalytic Properties of Spinel ZnFe2O4 Nanoparticles.

    PubMed

    Hema, E; Manikandan, A; Gayathri, M; Durka, M; Antony, S Arul; Venkatraman, B R

    2016-06-01

    Spinel Mn(x)Zn(1-x)Fe2O4 (0.0 ≤ x ≤ 1.0) nanoparticles (NPs) were successfully synthesized by a facile one-pot microwave combustion method using urea as the fuel. The formation of single phase cubic spinel structure was confirmed by powder X-ray diffraction (XRD), Rietveld analysis and Fourier transform infrared (FT-IR) spectroscopy and the calculated average crystallite size is in the range of 37.57 nm to 25.43 nm. The high resolution scanning electron microscopy (HR-SEM) and high resolution transmission electron microscopy (HR-TEM) results indicated that the as-prepared spinel Mn(x)Zn(1-x)Fe2O4 NPs showed high crystallinity and uniform size distribution with particles-like morphologies. The energy dispersive X-ray (EDX) analysis was confirmed the elemental composition and purity of the samples. The estimated band gap energy from UV-Visible diffuse reflectance spectroscopy (UV-Vis. DRS) is about 1.88 eV to 2.35 eV. The broad visible emission band is observed in the entire photoluminescence (PL) spectroscopy for all compositions. The variation of magnetization (M(s)) value of the samples was studied by vibrating sample magnetometer (VSM) and the lower compositions (x = 0.0, 0.2 and 0.4) show a superparamagnetism and the higher composition (x = 0.6, 0.8 and 1.0) show a ferromagnetic behavior with hysteresis and that the M(s) values increased with increasing Mn2+ content to reach a maximum value of 60.99 emu/g for MnFe2O4. All composition of spinel Mn(x)Zn(1-x)Fe2O4 NPs were successfully tested as catalyst for the oxidation of benzyl alcohol into benzaldehyde, which has resulted 83.29 and 96.51% conversion efficiency of ZnFe2O4 and Mn0.6Zn0.4Fe2O4 respectively.

  17. Large scale continuous synthesis of carbon-encapsulated magnetic nanoparticles

    NASA Astrophysics Data System (ADS)

    Bystrzejewski, M.; Huczko, A.; Lange, H.; Baranowski, P.; Cota-Sanchez, G.; Soucy, G.; Szczytko, J.; Twardowski, A.

    2007-04-01

    Fe, Fe3C and NdC2 nanoparticles, encapsulated within carbon cages, were continuously produced during the induction thermal plasma processing of Fe14Nd2B, in the presence of methane or acetylene. The product morphology was studied by means of SEM. Further structural details were obtained from TEM, HRTEM, Raman spectroscopy and x-ray powder diffraction studies. The so-produced nanostructures have core-shell structure, with inner cavity diameters varying between 10 and 30 nm. The carbon coatings were composed of between 5 and 25 graphene layers. The carbon cages were built from sp2 carbon atoms, which protected the encapsulated nanoparticles from both oxidation and agglomeration. The plasma generated products were ferromagnetic, with maximum values of coercivity field of 600 G s, and saturation magnetization values of up to 40 emu g-1.

  18. Silica-encapsulated magnetic nanoparticles: enzyme immobilization and cytotoxic study.

    PubMed

    Ashtari, Khadijeh; Khajeh, Khosro; Fasihi, Javad; Ashtari, Parviz; Ramazani, Ali; Vali, Hojatollah

    2012-05-01

    Silica-encapsulated magnetic nanoparticles (MNPs) were prepared via microemulsion method. The products were characterized by high resolution transmission electron microscopy (HRTEM) and energy-dispersive X-ray spectrum (EDS). MNPs with no observed cytotoxic activity against human lung carcinoma cell and brine shrimp lethality were used as suitable support for glucose oxidase (GOD) immobilization. Binding of GOD onto the support was confirmed by the FTIR spectra. The amount of immobilized GODs was 95 mg/g. Storage stability study showed that the immobilized GOD retained 98% of its initial activity after 45 days and 90% of the activity was also remained after 12 repeated uses. Considerable enhancements in thermal stabilities were observed for the immobilized GOD at elevated temperatures up to 80°C and the activity of immobilized enzyme was less sensitive to pH changes in solution.

  19. Microstructure Of Multistage Annealed Nanocrystalline SmCo2Fe2B Alloy With Enhanced Magnetic Properties

    SciTech Connect

    Jiang, Xiujuan; Devaraj, Arun; Balamurugan, B.; Cui, Jun; Shield, Jeffrey E.

    2014-02-11

    The microstructure and chemistry of SmCo2Fe2B melt-spun alloy after multistage annealing was investigated using high resolution transmission electron microscopy (HRTEM) and 3D atom probe tomography. The multistage annealing resulted in an increase in both the coercivity and magnetization. The presence of Sm(Co,Fe)4B (1:4:1) and Sm2(Co,Fe)17Bx (2:17:x) magnetic phases were confirmed using both techniques. Fe2B at a scale of ~ 5 nm was found by HRTEM precipitating within the 1:4:1 phase after the second-stage annealing. Ordering within the 2:17:x phase was directly identified both by the presence of antiphase boundaries observed by TEM and the interconnected isocomposition surface network found in 3D atom probe results in addition to radial distribution function analysis. The variations in the local chemistry after the secondary annealing were considered pivotal in improving the magnetic properties.

  20. Microstructure of multistage annealed nanocrystalline SmCo{sub 2}Fe{sub 2}B alloy with enhanced magnetic properties

    SciTech Connect

    Jiang, Xiujuan Shield, Jeffrey E.; Devaraj, Arun; Balamurugan, B.; Cui, Jun

    2014-02-14

    The microstructure and chemistry of SmCo{sub 2}Fe{sub 2}B melt-spun alloy after multistage annealing was investigated using high resolution transmission electron microscopy (HRTEM) and 3D atom probe tomography. The multistage annealing resulted in an increase in both the coercivity and magnetization. The presence of Sm(Co,Fe){sub 4}B (1:4:1) and Sm{sub 2}(Co,Fe){sub 17}B{sub x} (2:17:x) magnetic phases were confirmed using both techniques. Fe{sub 2}B at a scale of ∼5 nm was found by HRTEM precipitating within the 1:4:1 phase after the second-stage annealing. Ordering within the 2:17:x phase was directly identified both by the presence of antiphase boundaries observed by TEM and the interconnected isocomposition surface network found in 3D atom probe results in addition to radial distribution function analysis. The variations in the local chemistry after the secondary annealing were considered pivotal in improving the magnetic properties.

  1. Synthesis, characterisation, spectral, thermal, XRD, molecular modelling and potential antibacterial study of metal complexes containing octadentate azodye ligands

    NASA Astrophysics Data System (ADS)

    Mahapatra, Bipin Bihari; Chaulia, Satyanarayan; Sarangi, Ashish Kumar; Dehury, Satyanarayan; Panda, Jnyanaranjan

    2015-05-01

    Twelve tetrametallic complexes of Co(II), Ni(II), Cu(II), Zn(II), Cd(II) and Hg(II) with two new octadentate azodye ligands, 4,4‧-bis(2‧,4‧-dihydroxy-5‧carboxyphenylazo) diphenylether (LH6) and 4,4‧-bis(2‧,4‧-dihydroxy-5‧-acylphenylazo) diphenylether (L‧H4) have been synthesised. The structural elucidation of the complexes was made basing upon analytical, conductance, magnetic susceptibility, IR, electronic spectra, ESR, NMR, ESI-MS, TG, DTG, DTA and X-ray diffraction (powder pattern) data. The cobalt (II) and nickel (II) complexes are found to be octahedral, copper (II) complexes are distorted octahedral and a tetrahedral stereochemistry has been suggested to zinc (II), cadmium (II) and mercury (II) complexes. The thermal analysis data provided the kinetic parameters as order of decomposition reaction, activation energy and frequency factor. The geometry of the ligands and their Co(II), Ni(II), Cu(II) and Zn(II) complexes were optimised and their physicochemical properties were calculated by using molecular modelling procedure. The ESI-MS determination supports the molecular formula and molecular weight of the ligands and the complexes. The Ni(II) complex is found to have a triclinic crystal system. The potential antibacterial study of the two ligands and eight metal complexes was made by cup-plate method against one gram positive and one gram negative bacteria. The results showed increase in the activity of some metal complexes as compare with azodye ligands.

  2. 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

  3. Planetary magnetism

    NASA Technical Reports Server (NTRS)

    Russell, C. T.

    1981-01-01

    A synoptic view of early and recent data on the planetary magnetism of Mercury, Venus, the moon, Mars, Jupiter, and Saturn is presented. The data on Mercury from Mariner 10 are synthesized with various other sources, while data for Venus obtained from 120 orbits of Pioneer Venus give the upper limit of the magnetic dipole. Explorer 35 Lunar Orbiter data provided the first evidence of lunar magnetization, but it was the Apollo subsatellite data that measured accurately the magnetic dipole of the moon. A complete magnetic survey of Mars is still needed, and only some preliminary data are given on the magnetic dipole of the planet. Figures on the magnetic dipoles of Jupiter and Saturn are also suggested. It is concluded that if the magnetic field data are to be used to infer the interior properties of the planets, good measures of the multiple harmonics in the field are needed, which may be obtained only through low altitude polar orbits.

  4. Magnetic characterization of dual phase FeZrB soft magnetic alloy

    NASA Astrophysics Data System (ADS)

    Kong, L. H.; Chen, R. R.; Song, T. T.; Gao, Y. L.; Zhai, Q. J.

    2011-12-01

    The magnetic properties and the annealing process of Fe78Zr7B15 amorphous ribbons are investigated by X-ray diffraction (XRD), differential scanning calorimetry, and vibrating sample magnetometer. The fully amorphous structure of the as-quenched ribbons is confirmed by the XRD pattern. The Curie temperature and the saturation magnetization Ms of the ribbons are 305 °C and 124.3 emu/g, respectively. Annealing at 550 °C can result in an increase in Ms with annealing time due to the increasing crystallized volume fraction of α-Fe phase. The optimized annealing process is established at 550 °C for 20-30 min with maximum Ms of 146.6 emu/g. The morphology of the ribbons annealed at 550 °C is observed by scanning electron microscopy, showing that nanocrystalline α-Fe grains are dispersed in an amorphous matrix.

  5. Measurement of 2-5 keV x-ray emission from laser-target interactions by using fluor-MCP and CsI-XRD detectors

    SciTech Connect

    Lee, P.H.Y.; Tirsell, K.G.; Leipelt, G.R.; Laird, W.B.

    1981-09-29

    For inertial confinement fusion plasma diagnostics, x-ray diode (XRD) detectors using conventional cathodes are not sensitive enough to measure x-rays above approx. 1.5 keV. However, for laser driver fusion targets, x-rays in the range of 2 to 5 keV are important because of their mobility in the target. We have successfully used fluor-microchannel plate (MCP) detectors to obtain absolute x-ray measurements in the 2 to 5 keV range. Recent data obtained from experiments on the Shiva laser system are presented. In addition, designs for a variety of channels in the range using fluor-MCP and CsI-XRD's above 1.5 keV will be discussed.

  6. 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.

  7. 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.

  8. 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.

  9. 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.

  10. XRD and TEM characterization of cathodic MnO{sub 2} and discharge products in the Li-MnO{sub 2} cell

    SciTech Connect

    Shao, Y.; Hackney, S.A.; Cornilsen, B.C.

    1995-12-31

    The crystal structures of the undischarged, heat-treated electrolytic manganese dioxide (HEMD) and discharge products are characterized by high spatial resolution convergent beam electron diffraction (CBED). The results are compared with the x-ray diffraction (XRD) patterns characterized by broad, diffuse peaks. The CBED results for HEMD show that the starting cathodic material has the pyrolusite space group, but with a range of c/a ratios. The variability of the lattice parameter from grain to grain is found to coincide with the broadening on the low angle side of the XRD peaks. The CBED patterns of discharge products suggest a reduction range in c/a ratios and the formation of another phase.

  11. Laser Raman, XRD, DSC and Ac-Impedance Analysis of Polymer Blend Electrolyte Based on Eco-Friendly Pva-Pvp Blend with NH4NO3

    NASA Astrophysics Data System (ADS)

    Rajeswari, N.; Selvasekarapandian, S.; Prabaharan, S. R. S.; Kawamura, J.; Iwai, Y.; Karthikeyan, S.

    2013-07-01

    Proton conducting polymer blend electrolytes have attractive interest because of their advantages such as processability, flexibility, electrochemical stability, easy handling and their applications to a variety of electrochemical devices such as fuel cells, chemical sensor and electrochemical displays. In the present work, the films of 50PVA-50PVP blend with different MWt% concentrations of NH4NO3 have been prepared by solution casting techniques using distilled water as a solvent. The prepared films have been investigated by different techniques such as XRD, DSC, Laser Raman and AC Impedance spectroscopy. XRD studies reveal the amorphous nature of the polymer blend-salt complexes. The glass transition temperature has been calculated from the DSC analysis. From the AC Impedance spectroscopy, the high conductivity of the 30MWt% of NH4NO3 doped 50PVA-50PVP polymer complex has been found to be the order of 1.41 × 10-3S cm-1 at room temperature.

  12. 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.

  13. Instrumental Characterization Of Coir PITH By XRD, FTIR and SEM After Radium Adsorption From Aqueous Solution Under The Presence Of Humic Acids

    NASA Astrophysics Data System (ADS)

    Laili, Zalina; Omar, Muhamat; Yasir, Muhamad Samudi; Ibrahim, Mohd Zaidi; Yahaya, Mohd Yusri; Murshidi, Julie Andrianny

    2010-01-01

    Adsorption interactions of radium (Ra) ions onto coir pith (CP) under the presence of humic acid (HA) in the aqueous solution were investigated using X-ray diffraction (XRD), Fourier Transform Infrared Spectrophotometer (FTIR) and Scanning Electron Microscopy (SEM) techniques. XRD, IR and SEM characterization of the CP has revealed differences in the native CP and Ra ions loaded CP under the presence of HA in the aqueous solution. The X-Ray patterns showed that crystalline structure of the loaded CP exhibited a decrease in crystalline structure at around 49°-51° compared with unloaded CP. Characterization by IR revealed that participation of some surface functional groups during the Ra adsorption. SEM images for the morphological studies showed that there were slightly changes of the CP surfaces after the adsorption process.

  14. Studies on the intercalation of naproxen into layered double hydroxide and its thermal decomposition by in situ FT-IR and in situ HT-XRD

    NASA Astrophysics Data System (ADS)

    Wei, Min; Shi, Shuxian; Wang, Ji; Li, Yong; Duan, Xue

    2004-07-01

    Layered double hydroxides, novel anionic clay, meet the first requirement as inorganic matrices for encapsulating functional drugs or biomolecules with negative charge in aqueous media. In this study, naproxen has been intercalated into Mg-Al layered double hydroxide by the methods of ion exchange. The structure and composition of the intercalated material have been studied by X-ray diffraction (XRD), UV-vis spectroscopy and inductively coupled plasma emission spectroscopy. A schematic model has been proposed. Furthermore, in situ Fourier transform infrared spectroscopy, in situ high-temperature XRD, and thermogravimetry (TG) have been used to characterize the thermal decomposition of the hybrid material. It has been found that the thermal stability of the intercalated naproxen is significantly enhanced compared with the pure form before intercalation, which suggests that this drug-inorganic layered material may have prospective application as the basis of a novel drug delivery system.

  15. Magnetizing of permanent magnets using HTS bulk magnets

    NASA Astrophysics Data System (ADS)

    Oka, Tetsuo; Muraya, Tomoki; Kawasaki, Nobutaka; Fukui, Satoshi; Ogawa, Jun; Sato, Takao; Terasawa, Toshihisa

    2012-01-01

    A demagnetized Nd-Fe-B permanent magnet was scanned just above the magnetic pole which contains the HTS bulk magnet generating a magnetic field of 3.27 T. The magnet sample was subsequently found to be fully magnetized in the open space of the static magnetic fields. We examined the magnetic field distributions when the magnetic poles were scanned twice to activate the magnet plate inversely with various overlap distances between the tracks of the bulk magnet. The magnetic field of the "rewritten" magnet reached the values of the magnetically saturated region of the material, showing steep gradients at the border of each magnetic pole. As a replacement for conventional pulse field magnetizing methods, this technique is proposed to expand the degree of freedom in the design of electromagnetic devices, and is proposed as a novel practical method for magnetizing rare-earth magnets, which have excellent magnetic performance and require intense fields of more than 3 T to be activated.

  16. [Study on the damage of SiO2 thin films on LiNbO3 crystal in optical parametric oscillator by XRD spectrometry].

    PubMed

    Niu, Rui-Hua; Han, Jing-Hua; Luo, Jin; Lu, Feng; Zhu, Qi-Hua; Li, Tong; Yang, Li-Ming; Feng, Guo-Ying; Zhou, Shou-Huan

    2010-12-01

    In an attempt to elucidate the damage in high transmission thin films on LiNbO3 crystal in optical parametric oscillator, the authors employed XRD spectrometry to investigate the spectrum of laser-induced damage in thin film as well as the morphology of the damage. The authors observed that the damage of thin film was characterized by the depressions/craters in the surface of the films, which were surrounded by a deposition layer with the deceasing thickness from the center of the craters. The XRD measurements indicate that the film was crystallized. The authors analyzed the causes of morphologies and the mechanism of crystallization with the aid of the model for impurity-induced damage in thin solid films. The crystallization was due to the solidification of liquid and gaseous mixtures that result from the strong absorbing to the incident laser. The crater was generated because the mixtures were ejected under the extensive pressure of the laser plasma shock wave. During the process that the mixtures deposit around the craters, the density of the mixtures will decrease and crystallization takes place. As a result, the color of the deposition layer becomes lighter from inside to outside, and the crystallization of the thin film materials was observed by XRD spectrometry.

  17. Magnetic Properties of Nanocrystalline Nickel-Cobalt Ferrites

    NASA Astrophysics Data System (ADS)

    Tiwari, D. K.; Villaseñor-Cendejas, L. M.; Thakur, A. K.

    2013-09-01

    In this study, the nanocrystalline nickel-cobalt ferrites were prepared via the citrate route method at . The samples were calcined at for 3 h. The crystalline structure and the single-phase formations were confirmed by X-ray diffraction (XRD) measurements. Prepared materials showed the cubic spinel structure with m3m symmetry and Fd3m space group. The analyses of XRD patterns were carried out using POWD software. It gave an estimation of lattice constant “” of 8.3584 Å, which was in good agreement with the results reported in JCPDS file no. 742081. The crystal size of the prepared materials calculated by Scherer’s formula was 27.6 nm and the electrical conductivity was around . The permeability component variations with frequency were realized. The magnetic properties of the prepared materials were analyzed by a vibrating sample magnetometer (VSM). It showed a saturation magnetization of and the behavior of a hard magnet.

  18. Magnetite/CdTe magnetic-fluorescent composite nanosystem for magnetic separation and bio-imaging.

    PubMed

    Kale, Anup; Kale, Sonia; Yadav, Prasad; Gholap, Haribhau; Pasricha, Renu; Jog, J P; Lefez, Benoit; Hannoyer, Béatrice; Shastry, Padma; Ogale, Satishchandra

    2011-06-03

    A new synthesis protocol is described to obtain a CdTe decorated magnetite bifunctional nanosystem via dodecylamine (DDA) as cross linker. High resolution transmission electron microscopy (HRTEM), energy-dispersive x-ray spectroscopy (EDAX), vibrating sample magnetometry (VSM), Fourier transform infrared spectroscopy (FTIR), diffuse reflectance spectroscopy (DRS) and fluorescence microscopy are used to characterize the constitution, size, composition and physical properties of these superparamagnetic-fluorescent nanoparticles. These CdTe decorated magnetite nanoparticles were then functionalized with anti-epidermal growth factor receptor (EGFR) antibody to specifically target cells expressing this receptor. The EGFR is a transmembrane glycoprotein and is expressed on tumor cells from different tissue origins including human leukemic cell line Molt-4 cells. The magnetite-CdTe composite nanosystem is shown to perform excellently for specific selection, magnetic separation and fluorescent detection of EGFR positive Molt-4 cells from a mixed population. Flow cytometry and confocal laser scanning microscopy results show that this composite nanosystem has great potential in antibody functionalized magnetic separation and imaging of cells using cell surface receptor antibody.

  19. Magnetite/CdTe magnetic-fluorescent composite nanosystem for magnetic separation and bio-imaging

    NASA Astrophysics Data System (ADS)

    Kale, Anup; Kale, Sonia; Yadav, Prasad; Gholap, Haribhau; Pasricha, Renu; Jog, J. P.; Lefez, Benoit; Hannoyer, Béatrice; Shastry, Padma; Ogale, Satishchandra

    2011-06-01

    A new synthesis protocol is described to obtain a CdTe decorated magnetite bifunctional nanosystem via dodecylamine (DDA) as cross linker. High resolution transmission electron microscopy (HRTEM), energy-dispersive x-ray spectroscopy (EDAX), vibrating sample magnetometry (VSM), Fourier transform infrared spectroscopy (FTIR), diffuse reflectance spectroscopy (DRS) and fluorescence microscopy are used to characterize the constitution, size, composition and physical properties of these superparamagnetic-fluorescent nanoparticles. These CdTe decorated magnetite nanoparticles were then functionalized with anti-epidermal growth factor receptor (EGFR) antibody to specifically target cells expressing this receptor. The EGFR is a transmembrane glycoprotein and is expressed on tumor cells from different tissue origins including human leukemic cell line Molt-4 cells. The magnetite-CdTe composite nanosystem is shown to perform excellently for specific selection, magnetic separation and fluorescent detection of EGFR positive Molt-4 cells from a mixed population. Flow cytometry and confocal laser scanning microscopy results show that this composite nanosystem has great potential in antibody functionalized magnetic separation and imaging of cells using cell surface receptor antibody.

  20. CONDENSED MATTER: STRUCTURE, MECHANICAL AND THERMAL PROPERTIES: Synthesis and Properties of Magnetic Composites of Carbon Nanotubes/Fe Nanoparticle

    NASA Astrophysics Data System (ADS)

    Xu, Mei-Hua; Qi, Xiao-Si; Zhong, Wei; Ye, Xiao-Juan; Deng, Yu; Au, Chaktong; Jin, Chang-Qing; Yang, Zai-Xing; Du, You-Wei

    2009-11-01

    Magnetic composites of carbon nanotubes (CNTs) are synthesized by the in situ catalytic decomposition of benzene at temperatures as low as 400°C over Fe nanoparticles (mean grain size = 26 nm) produced by sol-gel fabrication and hydrogen reduction. The yield of CNT composite is up to about 3025% in a run of 6 h. FESEM and HRTEM investigations reveal that one-dimensional carbon species are produced in a large quantity. A relatively high value of magnetization is observed for the composite due to the encapsulation of ferromagnetic Fe3C and/or α-Fe. The method is suitable for the mass-production of CNT composites that contain magnetic nanoparticles.

  1. 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

  2. Synthesis, characterization and magnetic evaluation of praseodymium modified cerium oxide

    NASA Astrophysics Data System (ADS)

    Cruz Pacheco, A. F.; Gómez Cuaspud, J. A.; Parra Vargas, C. A.

    2017-01-01

    This paper report the synthesis, characterization and magnetic evaluation of Ce0.6Pr0.4O2 system using a chemical route that involves the combustion of citrate species. The precursors were characterized by Fourier transform infrared spectroscopy (FTIR), to identify, the main vibrational bands associated with the organic material after combustion process. The structural analysis by X-ray diffraction (XRD) revealed the obtaining of an Fm-3m (225) cubic phase with a particle size around 10nm. Finally, the measurement of the magnetization as a function of applied magnetic field and of susceptibility showed a perfect paramagnetic behaviour.

  3. Synthesis, Structural, Electrical and Magnetic Studies of Ni- Ferrite Nanoparticles

    NASA Astrophysics Data System (ADS)

    Godbole, Bhavana; Badera, Nitu; Shrivastava, S. B.; Jain, Deepti; Chandra, L. S. Sharath; Ganesan, V.

    Mono-dispersed NiFe2O4 nanoparticles have been synthesized using a stable ferric salt of FeCl3 with co-precipitation technique, for study of their structural, morphological and magnetic properties. The XRD pattern conforms the formation of FCC structure with the lattice constant 8.31Ao. The crystallite size was found to increase with the bath temperature ranging from 33 nm to 55 nm. The AFM results revealed that uniform disc shaped particles were obtained. The resistivity measurements show a metal like to semiconductor transition, which depends on the size of the grains. The magnetic study reveals that saturation magnetization increases with the grain thickness.

  4. Magnetic investigations

    SciTech Connect

    Bath, G.D.; Jahren, C.E.; Rosenbaum, J.G.; Baldwin, M.J.

    1983-12-31

    Air and ground magnetic anomalies in the Climax stock area of the NTS help define the gross configuration of the stock and detailed configuration of magnetized rocks at the Boundary and Tippinip faults that border the stock. Magnetizations of geologic units were evaluated by measurements of magnetic properties of drill core, minimum estimates of magnetizations from ground magnetic anomalies for near surface rocks, and comparisons of measured anomalies with anomalies computed by a three-dimensional forward program. Alluvial deposits and most sedimentary rocks are nonmagnetic, but drill core measurements reveal large and irregular changes in magnetization for some quartzites and marbles. The magnetizations of quartz monzonite and granodiorite near the stock surface are weak, about 0.15 A/m, and increase at a rate of 0.00196 A/m/m to 1.55 A/m, at depths greater than 700 m (2300 ft). The volcanic rocks of the area are weakly magnetized. Aeromagnetic anomalies 850 m (2800 ft) above the stock are explained by a model consisting of five vertical prisms. Prisms 1, 2, and 3 represent the near surface outline of the stock, prism 4 is one of the models developed by Whitehill (1973), and prism 5 is modified from the model developed by Allingham and Zietz (1962). Most of the anomaly comes from unsampled and strongly-magnetized deep sources that could be either granite or metamorphosed sedimentary rocks. 48 refs., 23 figs., 3 tabs.

  5. Observation of dimension dependent magnetic ordering in bismuth ferrite particulate and fiber nanostructures

    SciTech Connect

    Sakar, M.; Bharathkumar, S.; Balakumar, S.; Saravanan, P.

    2015-06-24

    Nanoparticles and nanofibers of bismuth ferrite were fabricated by sol-gel and electrospinning methods respectively. The structural and morphological analysis was carried out by XRD and FESEM techniques respectively. The magnetic measurements were carried out by SQUID magnetometer. The BFO nanofibers showed an enhanced magnetic property compared to nanoparticles. The observed magnetic properties were found to be associated with their magnetic ordering in the system where the antiferromagnetic/ferromagnetic core/shell like nature and ‘canted’ spin structure ordering was found to be the magnetic origin in the particulate and fiber nanostructures respectively.

  6. Transmission electron microscopy and ab initio calculations to relate interfacial intermixing and the magnetism of core/shell nanoparticles

    SciTech Connect

    Chi, C.-C.; Hsiao, C.-H.; Ouyang, Chuenhou; Skoropata, E.; Lierop, J. van

    2015-05-07

    Significant efforts towards understanding bi-magnetic core-shell nanoparticles are underway currently as they provide a pathway towards properties unavailable with single-phased systems. Recently, we have demonstrated that the magnetism of γ-Fe2O3/CoO core-shell nanoparticles, in particular, at high temperatures, originates essentially from an interfacial doped iron-oxide layer that is formed by the migration of Co{sup 2+} from the CoO shell into the surface layers of the γ-Fe2O3 core [Skoropata et al., Phys. Rev. B 89, 024410 (2014)]. To examine directly the nature of the intermixed layer, we have used high-resolution transmission electron microscopy (HRTEM) and first-principles calculations to examine the impact of the core-shell intermixing at the atomic level. By analyzing the HRTEM images and energy dispersive spectra, the level and nature of intermixing was confirmed, mainly as doping of Co into the octahedral site vacancies of γ-Fe2O3. The average Co doping depths for different processing temperatures (150 °C and 235 °C) were 0.56 nm and 0.78 nm (determined to within 5% through simulation), respectively, establishing that the amount of core-shell intermixing can be altered purposefully with an appropriate change in synthesis conditions. Through first-principles calculations, we find that the intermixing phase of γ-Fe2O3 with Co doping is ferromagnetic, with even higher magnetization as compared to that of pure γ-Fe2O3. In addition, we show that Co doping into different octahedral sites can cause different magnetizations. This was reflected in a change in overall nanoparticle magnetization, where we observed a 25% reduction in magnetization for the 235 °C versus the 150 °C sample, despite a thicker intermixed layer.

  7. Planetary Magnetism

    NASA Technical Reports Server (NTRS)

    Connerney, J. E. P.

    2007-01-01

    The chapter on Planetary Magnetism by Connerney describes the magnetic fields of the planets, from Mercury to Neptune, including the large satellites (Moon, Ganymede) that have or once had active dynamos. The chapter describes the spacecraft missions and observations that, along with select remote observations, form the basis of our knowledge of planetary magnetic fields. Connerney describes the methods of analysis used to characterize planetary magnetic fields, and the models used to represent the main field (due to dynamo action in the planet's interior) and/or remnant magnetic fields locked in the planet's crust, where appropriate. These observations provide valuable insights into dynamo generation of magnetic fields, the structure and composition of planetary interiors, and the evolution of planets.

  8. Magnetization and Magnetocaloric Effect in Sol-Gel Derived Nanocrystalline Copper-Zinc Ferrite.

    PubMed

    Anwar, M S; Ahmed, Faheem; Koo, Bon Heun

    2015-02-01

    We report the sol-gel synthesis and magnetocaloric effect in nanocrystalline copper-zinc ferrite (Cu0.5Zn0.5Fe2O4). The synthesized powder was characterized by using X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), energy dispersive X-ray spectroscopy (EDX) and magnetization measurements. The XRD results confirm the formation of single phase spinel structure. The average particle size was found to be ~58 nm. FE-SEM results suggested that the nanoparticles are agglomerated and spherical in shape. Magnetization measurement reveals that Cu0.5Zn0.5Fe2O4 nanoparticles exhibit transition temperature (Tc) above room temperature. The maximum magnetic entropy change (ΔSM)max shows interesting behaviour and was found to vary with the applied magnetic field. This nanopowder can be considered as potential material for magnetic refrigeration above room temperature.

  9. Planetary magnetism

    NASA Technical Reports Server (NTRS)

    Russell, C. T.

    1980-01-01

    Planetary spacecraft have now probed the magnetic fields of all the terrestrial planets, the moon, Jupiter, and Saturn. These measurements reveal that dynamos are active in at least four of the planets, Mercury, the earth, Jupiter, and Saturn but that Venus and Mars appear to have at most only very weak planetary magnetic fields. The moon may have once possessed an internal dynamo, for the surface rocks are magnetized. The large satellites of the outer solar system are candidates for dynamo action in addition to the large planets themselves. Of these satellites the one most likely to generate its own internal magnetic field is Io.

  10. Magnetic shielding

    DOEpatents

    Kerns, J.A.; Stone, R.R.; Fabyan, J.

    1987-10-06

    A magnetically-conductive filler material bridges the gap between a multi-part magnetic shield structure which substantially encloses a predetermined volume so as to minimize the ingress or egress of magnetic fields with respect to that volume. The filler material includes a heavy concentration of single-magnetic-domain-sized particles of a magnetically conductive material (e.g. soft iron, carbon steel or the like) dispersed throughout a carrier material which is generally a non-magnetic material that is at least sometimes in a plastic or liquid state. The maximum cross-sectional particle dimension is substantially less than the nominal dimension of the gap to be filled. An epoxy base material (i.e. without any hardening additive) low volatility vacuum greases or the like may be used for the carrier material. The structure is preferably exposed to the expected ambient magnetic field while the carrier is in a plastic or liquid state so as to facilitate alignment of the single-magnetic-domain-sized particles with the expected magnetic field lines. 3 figs.

  11. Magnetic shielding

    DOEpatents

    Kerns, John A.; Stone, Roger R.; Fabyan, Joseph

    1987-01-01

    A magnetically-conductive filler material bridges the gap between a multi-part magnetic shield structure which substantially encloses a predetermined volume so as to minimize the ingress or egress of magnetic fields with respect to that volume. The filler material includes a heavy concentration of single-magnetic-domain-sized particles of a magnetically conductive material (e.g. soft iron, carbon steel or the like) dispersed throughout a carrier material which is generally a non-magnetic material that is at least sometimes in a plastic or liquid state. The maximum cross-sectional particle dimension is substantially less than the nominal dimension of the gap to be filled. An epoxy base material (i.e. without any hardening additive) low volatility vacuum greases or the like may be used for the carrier material. The structure is preferably exposed to the expected ambient magnetic field while the carrier is in a plastic or liquid state so as to facilitate alignment of the single-magnetic-domain-sized particles with the expected magnetic field lines.

  12. PyXRD v0.6.2: a FOSS program to quantify disordered, layered minerals using multi-specimen X-ray diffraction profile fitting

    NASA Astrophysics Data System (ADS)

    Dumon, M.; Van Ranst, E.

    2015-03-01

    This paper presents a free and open-source model called PyXRD (short for Python X-ray diffraction) to improve the quantification of complex, poly-phasic mixed-layer phyllosilicate assemblages. The novelty of this model is the ab initio incorporation of the multi-specimen method, making it possible to share phases and (a selection of) their parameters across multiple specimens. By effectively reducing the number of parameters and increasing the number of observations, this approach speeds up the manual refinement process significantly when automated algorithms are used. To check the hypothesis that the multi-specimen set-up can improve automatic parameter refinement, we calculated X-ray diffraction patterns for four theoretical mineral assemblages. These patterns were then used as input for a refinement employing the multi-specimen set-up and one employing the single-pattern set-ups. For all of the assemblages, PyXRD was able to reproduce or approximate the input parameters with the multi-specimen approach. Diverging solutions only occurred in single-pattern set-ups which do not contain enough information (e.g. patterns of heated samples) to discern all the different minerals. Assuming a correct qualitative interpretation was made and a single pattern exists in which all phases are sufficiently discernible, the obtained results indicate a good quantification can often be obtained with just that pattern. For naturally occurring samples, this could mean modelling air-dry and/or ethylene-glycolated patterns might be sufficient. However, these results from theoretical experiments cannot automatically be extrapolated to all real-life experiments. In any case, PyXRD has proven to be very useful when X-ray diffraction patterns are modelled for complex mineral assemblages containing mixed-layer phyllosilicates with a multi-specimen approach.

  13. Synthetic spinels in the (Mg, Fe2+)(Cr, Fe3+)2O4 join: Mossbauer, optical absorption, single crystal XRD and electron microprobe analyses

    NASA Astrophysics Data System (ADS)

    Lenaz, D.; Skogby, H.; Princivalle, F.; Halenius, U.

    2003-04-01

    Single crystals along the Mg-chromite -- Mg-ferrite and Mg-chromite -- chromite joins were synthesized using a flux-growth method (24 hours at 1200^oC and 4^oC/h cooling rate to 900^oC in air and gas-controlled atmosphere) in order to evaluate the influence of composition on structure and cation distribution using optical absorption (OAS), Mössbauer (MS), single-crystal X-ray diffraction (XRD) and microprobe analyses (EPMA). At present, most of the analyses were carried out on the (Mg,Fe2+)Cr_2O_4 series. MgCr_2O_4 end-member: OAS shows prominent absorption bands at 23,700 and 17,300 cm-1. XRD analyses on three single crystals show a_0 equal to 8.3329 (1) Å and u (oxygen positional parameter) equal to 0.2612 (1), close to the values reported by O'Neill and Dollase (1994) as determined by powder diffraction on samples annealed at 900 to 1400^oC. The T-O and M-O calculated bond distances are equal to 1.965 and 1.995, respectively. These results are consistent with the set of optimised bond distances for Mg and Cr proposed by Lavina et al. (2002). (Mg,Fe2+)Cr_2O_4 series: Mössbauer spectra were measured at room temperature on different samples with nominal chromite components in the 10 to 70 mol % range. All the spectra show a single absorption line. For compositions close to the Mg-chromite end-member the line is narrow, however, for intermediate compositions the line broadens progressively and is best fitted with a quadrupole doublet (dq=0.22 for 50 mol % chromite). Towards the chromite end-member the peak becomes narrower again. XRD data shows that there is a linear positive correlation between a_0 and u with increasing Fe2+.

  14. Evaluating mineralogy at terrestrial analogs for early Mars: Detection and characterization of clays with XRD and investigation of iron substitution in natroalunite

    NASA Astrophysics Data System (ADS)

    Beckerman, Laura Grace

    The Mars Science Laboratory (MSL) Curiosity rover is equipped with CheMin, the first x-ray diffraction (XRD) instrument on Mars, for in situ mineralogy as part of its mission to seek evidence of past habitability at Gale Crater. Detection and characterization of hydrated minerals like clays and sulfates provides crucial insight into Mars' early geochemistry. For example, clays are often interpreted as having formed in lacustrine environments at neutral pHs, while sulfates such as jarosite are evidence of acid sulfate alteration. However, CheMin's inability to remove non-clay minerals and to preferentially orient samples may pose significant challenges to clay detection and characterization at Gale Crater. To evaluate the effect of particle size separation (<0.2 microm), removal of non-clay minerals, preferred orientation, and ethylene glycol solvation on XRD analyses of clays, we used both a CheMin analog instrument and a traditional laboratory XRD to identify clays in acid sulfate altered basalt from Mars analog sites in Costa Rica. We detected kaolinite in four of the fourteen samples studied, one of which also contained montmorillonite. Kaolinite was not detected in two samples with the analog instrument prior to clay isolation. These results suggest that CheMin may miss detection of some clays at Gale Crater, which could affect interpretations of early Mars' habitability. Mistaking iron-rich natroalunite (Na[Al,Fe]3(SO4) 2(OH)6) for jarosite (KFe3(SO4) 2(OH)6) could also impact interpretations of early Mars, as natroalunite can form over a broader range of pH, water:rock ratios, and redox conditions than can jarosite. To determine if iron-rich natroalunite is a common alteration product at Mars analog sites, we assessed iron content in natroalunite from Costa Rica. We detected up to 30% iron substitution in natroalunite at diverse geochemical settings. We also evaluated the feasibility of using XRD or Raman spectroscopy for in situ iron-rich natroalunite

  15. 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

  16. XRD and xanes studies of copper complexes using (diethyl 4-amino-1-phenyl-1H-pyrazole-3,5 dicarboxylate) as ligand

    NASA Astrophysics Data System (ADS)

    Mishra, Ashutosh; Jain, Garima

    2013-06-01

    X-ray diffraction (XRD) and X-ray absorption spectroscopic (XAS) studies have been done on three copper complexes using (diethyl 4-amino-1-phenyl-1H-pyrazole-3,5 dicarboxylate) as ligand. The X-ray diffraction studies of copper complexes have been recorded using Rigaku RINT-2000 X-ray diffractometer equipped with a rotating anode with tube voltage of 40 kV and current of 100 mA. The X-ray absorption spectra of the complexes have been recorded at Raja Ramanna Centre for Advanced Technology (RRCAT), Indore and is called beamline.

  17. Magnetic Recording.

    ERIC Educational Resources Information Center

    Lowman, Charles E.

    A guide to the technology of magnetic recorders used in such fields as audio recording, broadcast and closed-circuit television, instrumentation recording, and computer data systems is presented. Included are discussions of applications, advantages, and limitations of magnetic recording, its basic principles and theory of operation, and its…

  18. Magnetic shielding

    DOEpatents

    Kerns, J.A.; Stone, R.R.; Fabyan, J.

    1985-02-12

    A magnetically-conductive filler material bridges the gap between a multi-part magnetic shield structure which substantially encloses a predetermined volume so as to minimize the ingress or egress of magnetic fields with respect to that volume. The filler material includes a heavy concentration of single-magnetic-domain-sized particles of a magnetically conductive material (e.g. soft iron, carbon steel or the like) dispersed throughout a carrier material which is generally a non-magnetic material that is at least sometimes in a plastic or liquid state. The maximum cross-sectional particle dimension is substantially less than the nominal dimension of the gap to be filled. An epoxy base material (i.e. without any hardening additive) low volatility vacuum greases or the like may be used for the carrier material. The structure is preferably exposed to the expected ambient field while the carrier is in a plastic or liquid state so as to facilitate alignment of the single-magnetic-domain-sized particles with the expected magnetic field lines.

  19. Microstructure of Multistage Annealed Nanocrystalline SmCo2Fe2B Alloy with Enhanced Magnetic Properties

    SciTech Connect

    Jiang, Xiujuan; Devaraj, Arun; Balamurugan, B.; Cui, Jun; Shield, Jeffrey E.

    2014-02-01

    The microstructure and chemistry of SmCo2Fe2B melt-spun alloy after multistage annealing was investigated using high resolution transmission electron microscopy (HRTEM) and 3D atom probe tomography. The multistage annealing resulted in an increase in both the coercivity and magnetization. The presence of Sm(Co,Fe)4B (1:4:1) and Sm2(Co,Fe)17Bx (2:17:x) magnetic phases were confirmed using both techniques. Fe2B at a scale of -5 nm was found by HRTEM precipitating within the 1:4:1 phase after the second-stage annealing. Ordering within the 2:17:x phase was directly identified both by the presence of antiphase boundaries observed by TEM and the interconnected isocomposition surface network found in 3D atom probe results in addition to radial distribution function analysis. The variations in the local chemistry after the secondary annealing were considered pivotal in improving the magnetic properties.

  20. Microstructure of multistage annealed nanocrystalline SmCo2Fe2B alloy with enhanced magnetic properties

    SciTech Connect

    Jiang, Xiujuan; Devaraj, Arun; Balamurugan, B.; Cui, Jun; Shield, Jeffrey E.

    2014-07-30

    The microstructure and chemistry of SmCo2Fe2B melt-spun alloy after multistage annealing was investigated using high resolution transmission electron microscopy (HRTEM) and 3D atom probe tomography. The multistage annealing resulted in an increase in both the coercivity and magnetization. The presence of Sm(Co,Fe)4B (1:4:1) and Sm2(Co,Fe)17Bx (2:17:x) magnetic phases were confirmed using both techniques. Fe2B at a scale of -5 nm was found by HRTEM precipitating within the 1:4:1 phase after the second-stage annealing. Ordering within the 2:17:x phase was directly identified both by the presence of antiphase boundaries observed by TEM and the interconnected isocomposition surface network found in 3D atom probe results in addition to radial distribution function analysis. The variations in the local chemistry after the secondary annealing were considered pivotal in improving the magnetic properties.

  1. Magnetic nanotubes

    DOEpatents

    Matsui, Hiroshi; Matsunaga, Tadashi

    2010-11-16

    A magnetic nanotube includes bacterial magnetic nanocrystals contacted onto a nanotube which absorbs the nanocrystals. The nanocrystals are contacted on at least one surface of the nanotube. A method of fabricating a magnetic nanotube includes synthesizing the bacterial magnetic nanocrystals, which have an outer layer of proteins. A nanotube provided is capable of absorbing the nanocrystals and contacting the nanotube with the nanocrystals. The nanotube is preferably a peptide bolaamphiphile. A nanotube solution and a nanocrystal solution including a buffer and a concentration of nanocrystals are mixed. The concentration of nanocrystals is optimized, resulting in a nanocrystal to nanotube ratio for which bacterial magnetic nanocrystals are immobilized on at least one surface of the nanotubes. The ratio controls whether the nanocrystals bind only to the interior or to the exterior surfaces of the nanotubes. Uses include cell manipulation and separation, biological assay, enzyme recovery, and biosensors.

  2. Investigating α-particle radiation damage in phyllosilicates using synchrotron microfocus-XRD/XAS: implications for geological disposal of nuclear waste

    NASA Astrophysics Data System (ADS)

    Bower, W. R.; Pearce, C. I.; Pimblott, S. M.; Haigh, S. J.; Mosselmans, J. F. W.; Pattrick, R. A. D.

    2014-12-01

    The response of mineral phases to the radiation fields that will be experienced in a geological disposal facility (GDF) for nuclear waste is poorly understood. Phyllosilicates are critical phases in a GDF with bentonite clay as the backfill of choice surrounding high level wastes in the engineered barrier, and clays and micas forming the most important reactive component of potential host rocks. It is essential that we understand changes in mineral properties and behaviour as a result of damage from both α and γ radiation over long timescales. Radiation damage has been demonstrated to affect the physical integrity and oxidation state1 of minerals which will also influence their ability to react with radionuclides. Using the University of Manchester's newly commissioned particle accelerator at the Dalton Cumbrian Facility, UK, model phyllosilicate minerals (e.g. biotite, chlorite) were irradiated with high energy (5MeV) alpha particles at controlled dose rates. This has been compared alongside radiation damage found in naturally formed 'radiohalos' - spherical areas of discolouration in minerals surrounding radioactive inclusions, resulting from alpha particle penetration, providing a natural analogue to study lattice damage under long term bombardment1,2. Both natural and artificially irradiated samples have been analysed using microfocus X-ray absorption spectroscopy and high resolution X-ray diffraction mapping on Beamline I18 at Diamond Light Source; samples were probed for redox changes and long/short range disorder. This was combined with lattice scale imaging of damage using HR-TEM (TitanTM Transmission Electron Microscope). The results show aberrations in lattice parameters as a result of irradiation, with multiple damage-induced 'domains' surrounded by amorphous regions. In the naturally damaged samples, neo-formed phyllosilicate phases are shown to be breakdown products of highly damaged regions. A clear reduction of the Fe(III) component has been

  3. Mechanism of Rhabdophane-(La) And Lanthanite-(La) Formation during Reduction of Bioavailabe Nutrients in Water based on SEM and XRD Study

    NASA Astrophysics Data System (ADS)

    Szopa, Krzysztof; Banasik, Kamila; Krzykawski, Tomasz

    2012-01-01

    This study presents results of SEM and XRD investigation of products formed after La-rich bentonite application into water containing PO43- and CO32- ions. The main product of the investigated reaction with phosphate and carbonate anions is rabdophane-(La) and lanthanite-(La), respectively. Studied material has adaptation in many water reservoirs only for phosphorus ions reduction. Further studies might find application in case of reduction others hazardous ions. They could be precipitated in the same fast and effective way, to other stable, nontoxic mineral phases. Niniejszy artykuł traktuje o możliwości redukcji nutrientów (np. PO43-, CO32-) za pomocą bentonitu wzbogaconego w lantan. Jak dotąd jedynym zastosowaniem wspomnianego bentonitu jest redukcja jonów fosfonowych w środowiskach wodnych (np. jeziora, rzeki, zastoiska) do stabilnego i nietoksycznego związku mineralnego jakim jest rabdofan-(La). Na podstawie analiz SEM oraz XRD wykazano, że badany materiał umożliwia również redukcję jonów węglanowych do stabilnej i nietoksycznej fazy mineralnej-węglanowej (lantanit-(La)). Dalsze studia nad bentonitem lantanowym, poczynione względem innych, niepożądanych jonów (np. jonów azotanowych czy arsenianowych) mogą przynieść odpowiedzi względem ewentualnego i dalszego, środowiskowego zastosowania bentonitu lantanowego.

  4. Stability of mineral fibres in contact with human cell cultures. An in situ μXANES, μXRD and XRF iron mapping study.

    PubMed

    Pollastri, Simone; Gualtieri, Alessandro F; Vigliaturo, Ruggero; Ignatyev, Konstantin; Strafella, Elisabetta; Pugnaloni, Armanda; Croce, Alessandro

    2016-12-01

    Relevant mineral fibres of social and economic importance (chrysotile UICC, crocidolite UICC and a fibrous erionite from Jersey, Nevada, USA) were put in contact with cultured diploid human non-tumorigenic bronchial epithelial (Beas2B) and pleural transformed mesothelial (MeT5A) cells to test their cytotoxicity. Slides of each sample at different contact times up to 96 h were studied in situ using synchrotron XRF, μ-XRD and μ-XAS (I18 beamline, Diamond Light Source, UK) and TEM investigations. XRF maps of samples treated for 96 h evidenced that iron is still present within the chrysotile and crocidolite fibres and retained at the surface of the erionite fibres, indicating its null to minor mobilization in contact with cell media; this picture was confirmed by the results of XANES pre-edge analyses. μ-XRD and TEM data indicate greater morphological and crystallinity modifications occurring in chrysotile, whereas crocidolite and erionite show to be resistant in the biological environment. The contact of chrysotile with the cell cultures seems to lead to earlier amorphization, interpreted as the first dissolution step of these fibres. The formation of such silica-rich fibre skeleton may prompt the production of HO in synergy with surface iron species and could indicate that chrysotile may be much more reactive and cytotoxic in vitro in the (very) short term whereas the activity of crocidolite and erionite would be much more sluggish but persistent in the long term.

  5. 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.

  6. 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.

  7. Structural and morphological characterization of Poly(o-ethoxyaniline) Emeraldine-salt form using FTIR, XRD, LeBail Method and SEM

    NASA Astrophysics Data System (ADS)

    Silva, Adriano de S.; Soares, Juliana C.; Mafud, Ana Carolina; de Souza, Sérgio M.; Fernandes, Edson G. R.; Mascarenhas, Yvonne P.; Sanches, Edgar A.

    2014-08-01

    The introduction of polar functional and alkyl groups into the main chain of Polyaniline (PANI) is a mechanism to obtain soluble polymers in a wider variety of organic solvents. Poly(o-ethoxyaniline) (POEA) is a derivative of PANI and its structural difference is the presence of the group (-OC2H5) in the ortho position of the carbon rings. Despite the large number of studies performed with PANI and its derivatives, there are few that focus on a structural study of these materials in doped form (ES). Poly(o-ethoxyaniline) Emeraldine-salt form (POEA-ES) was synthesized in polymerization times of 3, 24 and 48 h. Through XRD measurements were observed that different polymerization times did not cause structural changes in polymer structures. It were found in XRD patterns peaks at 2θ = 8°, 12°, 16°, 24°, 26°, 38°, 44° and 52°. Crystallinity percentage was calculated using the Peak Fitting Module Program and showed that POEA-ES has around 39% of crystallinity. FTIR analysis allowed to identify characteristic absorption bands in the structure of POEA-ES. By Scanning Electron Microscopy (SEM) it was observed micrometric particles of varying sizes, with morphologies similar to interconnected vesicular microspheres. Through LeBail Method, it was observed that crystallites of POEA-ES are present in the order of 26 Å. It was found a conductivity value of 0.3 × 10-7 S/cm for POEA-ES.

  8. 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.

  9. 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.

  10. Synthesis, characterization and magnetic properties of carbon nanotubes decorated with magnetic MIIFe2O4 nanoparticles

    NASA Astrophysics Data System (ADS)

    Ali, Syed Danish; Hussain, Syed Tajammul; Gilani, Syeda Rubina

    2013-04-01

    In this study, a simple, efficient and reproducible microemulsion method was applied for the successful decoration of carbon nanotubes (CNTs) with magnetic MIIFe2O4 (M = Co, Ni, Cu, Zn) nanoparticles. The structure, composition and morphology of the prepared nanocomposite materials were characterized using X-ray diffraction (XRD), Rutherford backscattering spectroscopy (RBS), Fourier transform infrared spectroscopy (FTIR) and Scanning electron microscopy (SEM). The magnetic properties were investigated by the vibrating sample magnetometer (VSM). The SEM results illustrated that large quantity of MIIFe2O4 nanoparticles were uniformly decorated around the circumference of CNTs and the sizes of the nanoparticles ranged from 15 to 20 nm. Magnetic hysteresis loop measurements revealed that all the MIIFe2O4/CNTs nanocomposites displayed ferromagnetic behavior at 300 K and can be manipulated using an external magnetic field. The CoFe2O4/CNTs nanocomposite showed maximum value of saturation magnetization which was 37.47 emu g-1. The as prepared MIIFe2O4/CNTs nanocomposites have many potential application in magnetically guided targeted drug delivery, clinical diagnosis, electrochemical biosensing, magnetic data storage and magnetic resonance imaging.

  11. Amine-functionalized magnetic mesoporous silica nanoparticles for DNA separation

    NASA Astrophysics Data System (ADS)

    Sheng, Wei; Wei, Wei; Li, Junjian; Qi, Xiaoliang; Zuo, Gancheng; Chen, Qi; Pan, Xihao; Dong, Wei

    2016-11-01

    We report a modified approach for the functionalized magnetic mesoporous silica nanoparticles (MMSN) using polymer microspheres incorporated with magnetic nanoparticles in the presence of cetyltrimethylammonium bromide (CTAB) and the core-shell magnetic silica nanoparticles (MSN). These particles were functionalized with amino groups via the addition of aminosilane directly to the particle sol. We then evaluate their DNA separation abilities and find the capacity of DNA binding significantly increased (210.22 μg/mg) compared with normal magnetic silica spheres (138.44 μg/mg) by using an ultraviolet and visible spectrophotometer (UV). The morphologies, magnetic properties, particle size, pore size, core-shell structure and Zeta potential are characterized by Fourier transform infrared spectroscopy (FT-IR), vibrating sample magnetometer (VSM), Transmission electron microscopy (TEM), Powder X-ray diffraction (XRD), and dynamic light scattering (DLS). This work demonstrates that our MMSN own an excellent potential application in bioseparation and drug delivery.

  12. Magnetic Bearing

    NASA Technical Reports Server (NTRS)

    1996-01-01

    AVCON, Inc. produces advanced magnetic bearing systems for industrial use, offering a unique technological approach based on contract work done at Marshall Space Flight Center and Lewis Research Center. Designed for the turbopump of the Space Shuttle main engine, they are now used in applications such as electric power generation, petroleum refining, machine tool operation and natural gas pipelines. Magnetic bearings support moving machinery without physical contact; AVCON's homopolar approach is a hybrid of permanent and electromagnets which are one-third the weight, smaller and more power- efficient than previous magnetic bearings.

  13. Magnetic disk

    NASA Technical Reports Server (NTRS)

    Mallinson, John C.

    1992-01-01

    Magnetic disk recording was invented in 1953 and has undergone intensive development ever since. As a result of this 38 years of development, the cost per byte and the areal density have halved and doubled respectively every 2-2 1/2 years. Today, the cost per byte is lower than 10(exp -6) dollars per byte and area densities exceed 100 10(exp 6) bits per square inch. In this talk, the recent achievements in magnetic disk recording are first surveyed briefly. Then, the principal areas of current technical development are outlined. Finally, some comments are made about the future of magnetic disk recording.

  14. Lunar magnetism

    NASA Technical Reports Server (NTRS)

    Hood, L. L.; Sonett, C. P.; Srnka, L. J.

    1984-01-01

    Aspects of lunar paleomagnetic and electromagnetic sounding results which appear inconsistent with the hypothesis that an ancient core dynamo was the dominant source of the observed crustal magnetism are discussed. Evidence is summarized involving a correlation between observed magnetic anomalies and ejecta blankets from impact events which indicates the possible importance of local mechanisms involving meteoroid impact processes in generating strong magnetic fields at the lunar surface. A reply is given to the latter argument which also presents recent evidence of a lunar iron core.

  15. HRTEM Imaging of Atoms at Sub-Angstrom Resolution

    SciTech Connect

    O'Keefe, Michael A.; Allard, Lawrence F.; Blom, Douglas A.

    2005-04-06

    John Cowley and his group at Arizona State University pioneered the use of transmission electron microscopy (TEM) for high-resolution imaging. Images were achieved three decades ago showing the crystal unit cell content at better than 4 Angstrom resolution. This achievement enabled researchers to pinpoint the positions of heavy atom columns within the unit cell. Lighter atoms appear as resolution is improved to sub-Angstrom levels. Currently, advanced microscopes can image the columns of the light atoms (carbon, oxygen, nitrogen) that are present in many complex structures, and even the lithium atoms present in some battery materials. Sub-Angstrom imaging, initially achieved by focal-series reconstruction of the specimen exit surface wave, will become common place for next-generation electron microscopes with CS-corrected lenses and monochromated electron beams. Resolution can be quantified in terms of peak separation and inter-peak minimum, but the limits imposed on the attainable resolution by the properties of the micro-scope specimen need to be considered. At extreme resolution the ''size'' of atoms can mean that they will not be resolved even when spaced farther apart than the resolution of the microscope.

  16. HRTEM study comparing naturally and experimentally weathered pyroxenoids

    SciTech Connect

    Banfield, J.F.; Ferruzzi, G.G.; Casey, W.H.; Westrich, H.R.

    1995-01-01

    The mineralogy and chemistry of both naturally and experimentally weathered MnSiO{sub 3} chain silicate minerals (rhodonite and pyroxmangite) were compared. In natural MnSiO{sub 3}, high-resolution transmission-electron microscope observations reveal that alteration begins at grain boundaries and planar defects parallel to the silicate chains that represent junctions between regions with different chain periodicities. Dissolution along these defects results in elongate etch pits that may be partly filled by smectite. Smectite (Ca{sub 0.3}Mn{sub 2}Zn{sub 0.4}Al{sub 0.1}Si{sub 4}O{sub 10}(OH){sub 2}) also develops in larger etches at grain boundaries. The Zn apparently released by weathering of coexisting sphalerite, may facilitate crystallization of manganese-smectite; rhodochrosite is also an initial product. X-ray diffraction patterns from highly altered materials reveal only rhodochrosite and quartz. Simplified reactions are H{sub 2}CO{sub 3}(aq) + 4 MnSiO{sub 3}(s) = Mn{sub 3}Si{sub 4}O{sub 10}(OH){sub 2}(s) + MnCO{sub 3}(s) accompanied by 3H{sub 2}CO{sub 3}(aq) + Mn{sub 3}Si{sub 4}O{sub 10}(OH){sub 2}(s) = 3 MnCO{sub 3}(s) + 4SiO{sub 2}(s) + 4H{sub 2}O. Pyroxenoid dissolution is incongruent under experimental conditions. A 3-7 nm-thick layer of amorphous silica is present at the mineral surface after {approximately}2000 h of reaction in acidic and near-neutral pH solutions that were undersaturated with respect to bulk amorphous silica. This thin layer of polymeric silica, which is absent on unreacted grains, is interpreted to have formed largely by incongruent dissolution at the mineral surface as protons in solution rapidly exchange for near-surface Mn. The layer may also contain silica readsorbed back onto the surface from solution. The net result is that silica from the pyroxenoid is redistributed directly into reaction products. Upon aging in air for a year, leached layers partially recrystallize.

  17. Preparation and properties of the magnetic absorbent polymer via the chemical transformation process

    NASA Astrophysics Data System (ADS)

    Liu, Shengyu; Zhang, Suhong; Guo, Jianying; Wen, Jing; Qiao, Yan

    2017-01-01

    Magnetic polyacrylic acid sodium polymer (MPAAS) was prepared by chemical transformation method. Key parameters were investigated in the synthesis process of the magnetic polymer and an optimum preparation condition was gained. The structure of the magnetic polymer was characterized by X-ray diffraction (XRD), Fourier transform infrared spectrosocopy (FTIR) and scanning electron microscope (SEM). Magnetic property of the magnetic polymer was measured by the magnet and superconducting quantum interference device (SQUID). Both the swelling ratio and kinetics and the water retention ratio and kinetics were investigated. Based on the results, it can be gained that both swelling rate and equilibrium swelling rate were lowered after magnetization while the water retention ability of the magnetic polymer is stronger than that of the polymer.

  18. Effect of magnetic fields on melt-spun Nd2Fe14B-based ribbons

    NASA Astrophysics Data System (ADS)

    Van Nguyen, Vuong; Rong, Chuanbing; Ding, Yong; Liu, J. Ping

    2012-04-01

    The effect of a magnetic field on microstructure and magnetic properties of Nd2Fe14B-based melt-spun ribbons is investigated. The magnetic field was applied in perpendicular or parallel direction to the ribbon plane during quench with a field strength up to several kilo Oersteds. The XRD patterns and TEM graphs show a strong grain size reduction upon the magnetic field application. The magnetic field also enhances the (00l) texture of ribbons when the field is perpendicular to the ribbon plane. The refined microstructure with significantly reduced grain size leads to enhanced magnetic exchange interactions between the hard and soft phases in the Nd2Fe14B/Fe nanocomposite ribbons. This magnetic field-assisted melt-spinning technique is promising for producing nanocomposite magnets with enhanced energy density.

  19. 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

  20. Magnetic Reconnection

    NASA Video Gallery

    This science visualization shows a magnetospheric substorm, during which, magnetic reconnection causes energy to be rapidly released along the field lines in the magnetotail, that part of the magne...

  1. Magnetic monopoles

    SciTech Connect

    Fryberger, D.

    1984-12-01

    In this talk on magnetic monopoles, first the author briefly reviews some historical background; then, the author describes what several different types of monopoles might look like; and finally the author discusses the experimental situation. 81 references.

  2. CRYOGENIC MAGNETS

    DOEpatents

    Post, R.F.; Taylor, C.E.

    1963-05-21

    A cryogenic magnet coil is described for generating magnetic fields of the order of 100,000 gauss with a minimum expenditure of energy lost in resistive heating of the coil inductors and energy lost irreversibly in running the coil refrigeration plant. The cryogenic coil comprises a coil conductor for generating a magnetic field upon energization with electrical current, and refrigeration means disposed in heat conductive relation to the coil conductor for cooling to a low temperature. A substantial reduction in the power requirements for generating these magnetic fields is attained by scaling the field generating coil to large size and particular dimensions for a particular conductor, and operating the coil at a particular optimum temperature commensurate with minimum overall power requirements. (AEC)

  3. Superconducting magnets

    SciTech Connect

    Willen, E.; Dahl, P.; Herrera, J.

    1985-01-01

    This report provides a self-consistent description of a magnetic field in the aperture of a superconducting magnet and details how this field can be calculated in a magnet with cos theta current distribution in the coils. A description of an apparatus that can be used to measure the field uniformity in the aperture has been given. Finally, a detailed description of the magnet being developed for use in the Superconducting Super Collider is given. When this machine is built, it will be by far the largest application of superconductivity to date and promises to make possible the experimental discoveries needed to understand the basic laws of nature governing the world in which we live.

  4. Magnetic Bacteria.

    ERIC Educational Resources Information Center

    Nelson, Jane Bray; Nelson, Jim

    1992-01-01

    Describes the history of Richard Blakemore's discovery of magnetotaxic organisms. Discusses possible reasons why the magnetic response in bacteria developed. Proposes research experiments integrating biology and physics in which students investigate problems using cultures of magnetotaxic organisms. (MDH)

  5. 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.

  6. Length-Scale-Dependent Phase Transformation of LiFePO4 : An In situ and Operando Study Using Micro-Raman Spectroscopy and XRD.

    PubMed

    Siddique, N A; Salehi, Amir; Wei, Zi; Liu, Dong; Sajjad, Syed D; Liu, Fuqiang

    2015-08-03

    The charge and discharge of lithium ion batteries are often accompanied by electrochemically driven phase-transformation processes. In this work, two in situ and operando methods, that is, micro-Raman spectroscopy and X-ray diffraction (XRD), have been combined to study the phase-transformation process in LiFePO4 at two distinct length scales, namely, particle-level scale (∼1 μm) and macroscopic scale (∼several cm). In situ Raman studies revealed a discrete mode of phase transformation at the particle level. Besides, the preferred electrochemical transport network, particularly the carbon content, was found to govern the sequence of phase transformation among particles. In contrast, at the macroscopic level, studies conducted at four different discharge rates showed a continuous but delayed phase transformation. These findings uncovered the intricate phase transformation in LiFePO4 and potentially offer valuable insights into optimizing the length-scale-dependent properties of battery materials.

  7. Superconducting magnet

    NASA Technical Reports Server (NTRS)

    1985-01-01

    Extensive computer based engineering design effort resulted in optimization of a superconducting magnet design with an average bulk current density of approximately 12KA/cm(2). Twisted, stranded 0.0045 inch diameter NbTi superconductor in a copper matrix was selected. Winding the coil from this bundle facilitated uniform winding of the small diameter wire. Test coils were wound using a first lot of the wire. The actual packing density was measured from these. Interwinding voltage break down tests on the test coils indicated the need for adjustment of the wire insulation on the lot of wire subsequently ordered for construction of the delivered superconducting magnet. Using the actual packing densities from the test coils, a final magnet design, with the required enhancement and field profile, was generated. All mechanical and thermal design parameters were then also fixed. The superconducting magnet was then fabricated and tested. The first test was made with the magnet immersed in liquid helium at 4.2K. The second test was conducted at 2K in vacuum. In the latter test, the magnet was conduction cooled from the mounting flange end.

  8. Development of novel FePt/nanodiamond hybrid nanostructures: L10 phase size-growth suppression and magnetic properties

    NASA Astrophysics Data System (ADS)

    Douvalis, A. P.; Bourlinos, A. B.; Tucek, J.; Čépe, K.; Bakas, T.; Zboril, R.

    2016-05-01

    A new type of hybrid nanomaterial composed of magnetic FePt nanoparticles grown on the surface of nanodiamond nanotemplate assemblies is described for the first time. Post annealing in vacuum of the as-made nanomaterial bearing cubic A1 soft magnetic FePt nanoparticles leads to the development of FePt nanoparticles with tetragonal L10 hard, magnetic-phase characteristics, leaving untouched the nanodiamond nanotemplate assemblies. X-ray diffraction, high-resolution transmission electron microscopy including chemical mapping (HRTEM/HAADF), magnetization measurements, and 57Fe Mössbauer spectroscopy data show that the magnetic FePt nanoparticles, with average sizes of 3 and 8 nm in the as-made and annealed hybrids, respectively, are homogenously distributed within the nanodiamond template in both nanomaterials. As a consequence, their structural, morphological, and magnetic properties differ significantly from the corresponding properties of the nonsupported (free) as-made and annealed FePt nanoparticles with average sizes of 6 and 32 nm, respectively, developed by the same methods. This spatial isolation suppresses the size-growth of the FePt nanoparticles during the post-annealing procedure, triggering superparamagnetic relaxation phenomena, which are exposed as a combination of hard and soft magnetic-phase characteristics.

  9. Occluded cobalt species over ZSM-5 matrix: Design, preparation, characterization and magnetic behavior

    SciTech Connect

    Pierella, Liliana B. Saux, Clara; Bertorello, Hector R.; Bercoff, Paula G.; Botta, Pablo M.; Rivas, J.

    2008-08-04

    Co-containing molecular sieves with MFI structure was synthesized by the hydrothermal crystallization method and cobalt was incorporated in it by wet impregnation at different percentages. Thermal post-treatments were applied to Co-ZSM-5: calcination and reduction. X ray diffraction (XRD) and FTIR studies confirmed crystallinity, structure and orthorhombic symmetry of the obtained samples (Co-ZSM-5 calcined and Co-ZSM-5 reduced). The XRD, Raman spectroscopy, SEM and TPR techniques for the calcined samples showed the presence of Co{sub 3}O{sub 4} which diminished in the reduced samples and Co{sup 0} appeared. The magnetic behavior of the materials was evaluated by magnetization (M) variation with applied magnetic field (H) at different temperatures. Low magnetization is observed in the calcined samples while high values are attained in the reduced samples, due to the presence of metallic Co.

  10. Ion-pairing in aqueous CaCl2 and RbBr solutions. Simultaneous structural refinement of XAFS and XRD data

    SciTech Connect

    Pham, Thai V.; Fulton, John L.

    2013-01-22

    We present a new methodology involving the simultaneous refinement of both x-ray absorption and x-ray diffraction spectra (X-ray Absorption/Diffraction Structural Refinement,XADSR), to study hydration and ion pair structure of CaCl2 and RbBr salts in concentrated aqueous solutions. The XADSR analysis includes the XAFS spectra analysis of both the cation and anion as a probe of their short-range structure with an XRD spectral analysis as a probe of the global structural. Together they deliver a comprehensive picture of the cation and anion hydration, the contact ion pair (CIP) structure and the solvent-separated ion pair (SSIP) structure. XADSR analysis of 6.0 m aqueous CaCl2 reveals that there are an insignificant number of Ca2+-Cl- CIP’s, but there are approximately 3.4 SSIP’s separated by about 4.99 Å. In contrast XADSR analysis of aqueous RbBr yields about 0.7 pair CIP at a bond length 3.51 Å. The present work demonstrates a new approach for a direct co-refinement of XRD and XAFS spectra in a simple and reliable fashion, opening new opportunities for analysis in various disordered and crystalline systems. This work was supported by the U.S. Department of Energy (DOE), Office of Basic Energy Sciences, Division of Chemical Sciences, Geosciences and Biosciences. Pacific Northwest National Laboratory (PNNL) is operated for the U.S. Department of Energy by Battelle.

  11. Chemical and morphological characterization of TSP and PM2.5 by SEM-EDS, XPS and XRD collected in the metropolitan area of Monterrey, Mexico

    NASA Astrophysics Data System (ADS)

    González, Lucy T.; Rodríguez, F. E. Longoria; Sánchez-Domínguez, M.; Leyva-Porras, C.; Silva-Vidaurri, L. G.; Acuna-Askar, Karim; Kharisov, B. I.; Villarreal Chiu, J. F.; Alfaro Barbosa, J. M.

    2016-10-01

    Total suspended particles (TSP) and particles smaller than 2.5 μm (PM2.5) were collected at four sites in the metropolitan area of Monterrey (MAM) in Mexico. The samples were characterized by X-ray Diffraction (XRD), X-ray Photoelectron Spectroscopy (XPS), and Scanning Electron Microscopy (SEM). In order to determine the possible sources of emissions of atmospheric particulate matter, a principal component analysis (PCA) was performed. The XRD results showed that the major crystalline compounds found in the TPS were CaCO3 and SiO2; while in the PM2.5 CaSO4 was found. The XPS analysis showed that the main elements found on the surface of the particles were C, O, Si, Ca, S, and N. The deconvolution carried out on the high-resolution spectra for C1s, S2p and N1s, showed that the aromatics, sulfates and pyrrolic-amides were the main groups contributing to the signal of these elements, respectively. The C-rich particles presented a spherical morphology, while the Ca- and Si-based particles mostly showed a prismatic shape. The PCA analysis together with the results obtained from the characterization techniques, suggested that the main contributors to the CaCO3 particles collected in the PM were most probably produced and emitted into the atmosphere by local construction industries and exploitation of rich-deposits of calcite. Meanwhile, the SiO2 found in the MAM originated from the suspension of geological material abundant in the region, and the carbon particles were mainly produced by the combustion of fossil fuels.

  12. Ceria-based Catalysts for the Production of H2 Through the Water-gas-shift Reaction: Time-Resolved XRD and XAFS Studies

    SciTech Connect

    Wang,X.; Rodriguez, J.; Hanson, J.; Gamarra, D.; Marinez-Arias, A.; Fernandez-Garcia, M.

    2008-01-01

    Hydrogen is a potential alternate energy source for satisfying many of our energy needs. In this work, we studied H2 production from the water-gas-shift (WGS) reaction over Ce1-x Cu x O2 catalysts, prepared with a novel microemulsion method, using two synchrotron-based techniques: time-resolved X-ray diffraction (XRD) and X-ray absorption fine structure (XAFS). The results are compared with those reported for conventional CuO x /CeO2 and AuO x /CeO2 catalysts obtained through impregnation of ceria. For the fresh Ce1-x Cu x O2 catalysts, the results of XAFS measurements at the Cu K-edge indicate that Cu is in an oxidation state higher than in CuO. Nevertheless, under WGS reaction conditions the Ce1-x Cu x O2 catalysts undergo reduction and the active phase contains very small particles of metallic Cu and CeO2-x . Time-resolved XRD and XAFS results also indicate that Cud+ and Aud+ species present in fresh CuO x /CeO2 and AuO x /CeO2 catalysts do not survive above 200 C under the WGS conditions. In all these systems, the ceria lattice displayed a significant increase after exposure to CO and a decrease in H2O, indicating that CO reduced ceria while H2O oxidized it. Our data suggest that H2O dissociation occurred on the Ovacancy sites or the Cu-Ovacancy and Au-Ovacancy interfaces. The rate of H2 generation by a Ce0.95Cu0.05O2 catalyst was comparable to that of a 5 wt% CuO x /CeO2 catalyst and much bigger than those of pure ceria or CuO.

  13. MAGNETIC IMAGING OF NANOCOMPOSITE MAGNETS

    SciTech Connect

    VOLKOV,V.V.ZHU,Y.

    2003-08-03

    Understanding the structure and magnetic behavior is crucial for optimization of nanocomposite magnets with high magnetic energy products. Many contributing factors such as phase composition, grain size distribution and specific domain configurations reflect a fine balance of magnetic energies at nanometer scale. For instance, magnetocrystalline anisotropy of grains and their orientations, degree of exchange coupling of magnetically soft and hard phases and specific energy of domain walls in a material. Modern microscopy, including Lorentz microscopy, is powerful tool for visualization and microstructure studies of nanocomposite magnets. However, direct interpretation of magnetically sensitive Fresnel/Foucault images for nanomagnets is usually problematic, if not impossible, because of the complex image contrast due to small grain size and sophisticated domain structure. Recently we developed an imaging technique based on Lorentz phase microscopy [l-4], which allows bypassing many of these problems and get quantitative information through magnetic flux mapping at nanometer scale resolution with a magnetically calibrated TEM [5]. This is our first report on application of this technique to nanocomposite magnets. In the present study we examine a nanocomposite magnet of nominal composition Nd{sub 2}Fe{sub 14+{delta}}B{sub 1.45} (14+{delta}=23.3, i.e. ''hard'' Nd{sub 2}Fe{sub 14}B-phase and 47.8 wt% of ''soft'' {alpha}-Fe phase ({delta}=9.3)), produced by Magnequench International, Inc. Conventional TEM/HREM study (Fig. 1-2) suggests that material has a bimodal grain-size distribution with maximum at d{sub max}=25 nm for Nd{sub 2}Fe{sub 14}B phase and d{sub max} = 15 nm for {alpha}-Fe phase (Fig.1c, Fig.2) in agreement with synchrotron X-ray studies (d{sub max}=23.5 nm for Nd{sub 2}Fe{sub 14}B [6]). Lattice parameters for Nd{sub 2}Fe{sub 14}B phase are a=8.80 and c=12.2 {angstrom}, as derived from SAED ring patterns (Fig.1a), again in good agreement with X-ray data

  14. Synthesis, structural and magnetic characterization of soft magnetic nanocrystalline ternary FeNiCo particles

    NASA Astrophysics Data System (ADS)

    Toparli, Cigdem; Ebin, Burçak; Gürmen, Sebahattin

    2017-02-01

    The present study focuses on the synthesis, microstructural and magnetic properties of ternary FeNiCo nanoparticles. Nanocrystalline ternary FeNiCo particles were synthesized via hydrogen reduction assisted ultrasonic spray pyrolysis method in single step. The effect of precursor concentration on the morphology and the size of particles was investigated. The syntheses were performed at 800 °C. Structure, morphology and magnetic properties of the as-prepared products were characterized through X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and vibrating sample magnetometer (VSM) studies. Scherer calculation revealed that crystallite size of the ternary particles ranged between 36 and 60 nm. SEM and TEM investigations showed that the particle size was strongly influenced by the precursor concentration and Fe, Ni, Co elemental composition of individual particles was homogeneous. Finally, the soft magnetic properties of the particles were observed to be a function of their size.

  15. Covalent magnetism and magnetic impurities.

    PubMed

    Gruber, C; Bedolla, P O; Mohn, P

    2013-05-08

    We use the model of covalent magnetism and its application to magnetic insulators applied to the case of insulating carbon doped BaTiO3. Since the usual Stoner mechanism is not applicable we study the possibility of the formation of magnetic order based on a mechanism favoring singly occupied orbitals. On the basis of our model parameters we formulate a criterion similar to the Stoner criterion but also valid for insulators. We describe the model of covalent magnetism using a molecular orbital picture and determine the occupation numbers for spin-up and spin-down states. Our model allows a simulation of the results of our ab initio calculations for E(ℳ) which are found to be in very good agreement.

  16. Mechanical synthesis of nanostructured nickel-zinc ferrite and investigation of magnetic properties

    NASA Astrophysics Data System (ADS)

    Radhika, K.; Yasin, Sk. Mohammad; Kumar, N. Harish

    2012-06-01

    Nanocrystalline Ni-Zn ferrite was synthesized at room temperature by high energy ball milling. Crystallographic phases appearing during ball milling & crystallite sizes were determined from X-ray diffraction (XRD) analysis. The magnetic response of the powder samples were investigated using vibrating sample magnetometer (VSM) which showed 30hr milled un annealed sample to be superparamagnetic.

  17. Uniaxial magnetic anisotropy in Pd/Fe bilayers on Al2O3 (0001) induced by oblique deposition

    NASA Astrophysics Data System (ADS)

    Chi, Chiao-Sung; Wang, Bo-Yao; Pong, Way-Faung; Ho, Tsung-Ying; Tsai, Cheng-Jui; Lo, Fang-Yuh; Chern, Ming-Yau; Lin, Wen-Chin

    2012-06-01

    This study reports the preparation of self-organized 1-dimensional magnetic structures of Fe on Al2O3 (0001) by oblique deposition. The x-ray diffraction (XRD) results in this study show the preferred (110) texture of the Fe films. XRD and extended x-ray adsorption fine structure measurements indicate larger oblique deposition angle (65°) leads to more disorder in the Fe crystalline structure. After capping with a Pd overlayer, the Pd/Fe/Al2O3 (0001) still exhibits uniaxial magnetic anisotropy induced by the underlying 1-dimensional Fe nanostructure. This uniaxial magnetic anisotropy changes with the variation in Fe thickness and oblique deposition angle. These results clearly indicate the feasibility of manipulating uniaxial magnetic anisotropy and crystalline order through the oblique deposition of magnetic materials.

  18. Magnetic Heads

    NASA Astrophysics Data System (ADS)

    Yokoshima, Tokihiko

    Figure 6.1 shows how rapidly the areal density of hard disk drives (HDD) has been increasing over the past 20 years [1]. Several critical innovations were necessary to bring about such rapid progress in the field of magnetic recording [2]. One of the most significant innovations from the viewpoint of material improvement was the electrodeposition of permalloy (Ni80Fe20), which was introduced by IBM in 1979 as the core material of a thin-film inductive head to increase the magnetic recording density [3]. After the introduction of the magneto-resistive (MR) element as the read head and the electrodeposited permalloy as the write head by IBM in 1991 [4], the rate of increase in the recording density of HDDs jumped from 30% per year to 60% per year. Recently, a giant magneto-resistive (GMR) element has been used for the read element instead of the MR element. The rate of increase in the recording density jumped to over 100% per year in 1999, which is an incredible rate of increase. Since 2002, however, the rate of increase has decreased to 30%; thus, new innovations are required to maintain the rate of increase. In 2004, the practical use of perpendicular magnetic recording instead of longitudinal magnetic recording was announced [5]. This system is a critical innovation for developing high-performance HDD systems with high-recording density. The design of the magnetic recording head was changed because of the change of the recording system.

  19. Magnetic characteristics of CoPd and FePd antidot arrays on nanoperforated Al2O3 templates

    NASA Astrophysics Data System (ADS)

    Maximenko, A.; Fedotova, J.; Marszałek, M.; Zarzycki, A.; Zabila, Y.

    2016-02-01

    Hard magnetic antidot arrays show promising results in context of designing of percolated perpendicular media. In this work the technology of magnetic FePd and CoPd antidot arrays fabrication is presented and correlation between surface morphology, structure and magnetic properties is discussed. CoPd and FePd antidot arrays were fabricated by deposition of Co/Pd and Fe/Pd multilayers (MLs) on porous anodic aluminum oxide templates with bowl-shape cell structure with inclined intercellular regions. FePd ordered L10 structure was obtained by successive vacuum annealing at elevated temperatures (530 °C) and confirmed by XRD analysis. Systematic analysis of magnetization curves evidenced perpendicular magnetic anisotropy of CoPd antidot arrays, while FePd antidot arrays revealed isotropic magnetic anisotropy with increased out-of-plane magnetic contribution. MFM images of antidots showed more complicated contrast, with alternating magnetic dots oriented parallel and antiparallel to tip magnetization moment.

  20. Electrical and magnetic properties of nano-sized magnesium ferrite

    NASA Astrophysics Data System (ADS)

    T, Smitha; X, Sheena; J, Binu P.; Mohammed, E. M.

    2015-02-01

    Nano-sized magnesium ferrite was synthesized using sol-gel techniques. Structural characterization was done using X-ray diffractometer and Fourier Transform Infrared Spectrometer. Vibration Sample Magnetometer was used to record the magnetic measurements. XRD analysis reveals the prepared sample is single phasic without any impurity. Particle size calculation shows the average crystallite size of the sample is 19nm. FTIR analysis confirmed spinel structure of the prepared samples. Magnetic measurement study shows that the sample is ferromagnetic with high degree of isotropy. Hysterisis loop was traced at temperatures 100K and 300K. DC electrical resistivity measurements show semiconducting nature of the sample.

  1. One step synthesis of quantum dot-magnetic nanoparticle heterodimers for dual modal imaging applications.

    PubMed

    Lee, Jiyeon; Hwang, Gyoyeon; Hong, Yeon Sun; Sim, Taebo

    2015-04-21

    Dual modal nanoprobes are promising tools for accurately detecting target molecules as part of the diagnosis of diseases including cancers. We have explored a new dual modal bioimaging probe that is comprised of a quantum dot (QD)-magnetic nanoparticle (MNP) hybrid. The MNP-QD heterodimers explored are fabricated by using a platinum-guanine coordination bonding guided self-assembly process, employing the metal-DNA conjugation method. Investigations utilizing energy dispersive spectroscopy (EDS) equipped high resolution transmission electron microscopy (HRTEM) demonstrate that the heterodimer contains an iron (Fe) dominant MNP and a cadmium (Cd) dominant QD. Finally, the results of cell studies show that the MNP-QD conjugates display good HeLa cell uptake in the absence of non-specific binding to the cell membrane and, as such, they can be used to label cells in vitro and in vivo as part of a new cell imaging technique.

  2. Magnetic light

    PubMed Central

    Kuznetsov, Arseniy I.; Miroshnichenko, Andrey E.; Fu, Yuan Hsing; Zhang, JingBo; Luk’yanchuk, Boris

    2012-01-01

    Spherical silicon nanoparticles with sizes of a few hundreds of nanometers represent a unique optical system. According to theoretical predictions based on Mie theory they can exhibit strong magnetic resonances in the visible spectral range. The basic mechanism of excitation of such modes inside the nanoparticles is very similar to that of split-ring resonators, but with one important difference that silicon nanoparticles have much smaller losses and are able to shift the magnetic resonance wavelength down to visible frequencies. We experimentally demonstrate for the first time that these nanoparticles have strong magnetic dipole resonance, which can be continuously tuned throughout the whole visible spectrum varying particle size and visually observed by means of dark-field optical microscopy. These optical systems open up new perspectives for fabrication of low-loss optical metamaterials and nanophotonic devices. PMID:22768382

  3. Influence of milled α-Fe powders on structure and magnetic properties of Sm(Co,Zr)7/α-(Fe,Co) nanocomposite magnets made by mechanical alloying

    NASA Astrophysics Data System (ADS)

    Liu, Z.; Chen, R. J.; Lee, D.; Yan, A. R.

    2011-04-01

    Sm(Co,Zr)7/α-(Fe,Co) nanocomposite magnets were produced by extensive milling of the mixture of crushed as-cast SmCo6.8Zr0.2 powders and 10 wt. % iron powders followed by annealing. The iron powders were added either with 600 min premilling or without premilling. The phase structures are studied by XRD patterns and thermomagnetic curves (M-T). According to the results of XRD patterns, the structures of the Sm(Co,Zr)7/α-(Fe,Co) nanocomposite magnets made with the premilled Fe powders consist of SmCo7 phase and α-(Co,Fe) phase. However, the composite of Sm (Co,Zr)7/α-Fe nanocomposite made from Fe powders without premilling consists of SmCo7, α-(Co,Fe) and SmCo5 phases. The α-(Co,Fe) phase is further studied by XRD and thermomagnetic measurements. It indicates that different composition of α-(Co,Fe) phase was obtained in two Sm(Co,Zr)7/α-(Fe,Co) nanocomposite magnets made with the premilled α-Fe powders and without premilled α-Fe powders. The magnetic properties of the soft phase can be tailored. The intergrain exchange coupling strength of the Sm(Co,Zr)7/α-(Fe,Co) nanocomposite magnets is found to be influenced by the soft-phase grain size and properties.

  4. X-radiography, XRD and Ultrasonic Data Transfer Function Technique - Simultaneous Measurements Under Simulated Mantle Conditions in a Multi-Anvil Device

    NASA Astrophysics Data System (ADS)

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

    2004-05-01

    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 is an important tool for the determination of the elastic properties. Ultrasonic interferometry allows the highly precise travel time measurement at a sample enclosed in a high-pressure multi-anvil device. But the calculation of wave velocities requires the exact sample length under in situ conditions. There are two options - scanning the interfaces of the sample by XRD (Mueller et al., 2003) and X-radiography (Li et al., 2001). The multi-anvil apparatus MAX80 is equipped for both methods. Only the X-radiography is fast enough for transient measurements. Contrary to XRD measurements, imaging the sample by X-rays requires a beam diameter larger than the sample length. Therefore the fixed primary slits of Max80 were exchanged by 4-blade high precision slits of Advanced Design Consulting, Inc. A Ce-YAG-crystal converts the X-ray image to an optical one, redirected by a mirror and captured by a CCD-camera. To derive the sample length, the different brightness of sample, buffer rod and reflector at the electronic image is evaluated. Classical ultrasonic interferometry is very time consuming, because the ultrasonic waves of the frequency range under study are generated and detected one after another with a given step rate. A 60 MHz frequency sweep with 100 kHz steps lasts for more than 30 minutes. This is a serious limitation for all transient measurements, but also limits the data collection at elevated temperatures to prevent the pressure transmitting boron epoxy cubes and the anvils from overheating. The ultrasonic transfer function technique (UTF), first described by Li et al. (2002), generates all the frequencies simultaneously. Related to the results and experiences of Li the UTF-technique was developed independently at GFZ. This version allows to

  5. Magnetic particles

    NASA Technical Reports Server (NTRS)

    Chang, Manchium (Inventor); Colvin, Michael S. (Inventor)

    1989-01-01

    Magnetic polymer particles are formed by swelling porous, polymer particles and impregnating the particles with an aqueous solution of precursor magnetic metal salt such as an equimolar mixture of ferrous chloride and ferric chloride. On addition of a basic reagent such as dilute sodium hydroxide, the metal salts are converted to crystals of magnetite which are uniformly contained througout the pores of the polymer particle. The magnetite content can be increased and neutral buoyancy achieved by repetition of the impregnaton and neutralization steps to adjust the magnetite content to a desired level.

  6. MAGNETIC GRID

    DOEpatents

    Post, R.F.

    1960-08-01

    An electronic grid is designed employing magnetic forces for controlling the passage of charged particles. The grid is particularly applicable to use in gas-filled tubes such as ignitrons. thyratrons, etc., since the magnetic grid action is impartial to the polarity of the charged particles and, accordingly. the sheath effects encountered with electrostatic grids are not present. The grid comprises a conductor having sections spaced apart and extending in substantially opposite directions in the same plane, the ends of the conductor being adapted for connection to a current source.

  7. Magnetic and microstructural properties of Al substituted M-type Ca-Sr hexaferrites

    NASA Astrophysics Data System (ADS)

    Yang, Yujie; Wang, Fanhou; Liu, Xiansong; Shao, Juxiang; Huang, Duohui

    2017-01-01

    In the current study, Al substituted M-type Ca-Sr hexaferrites, with composition Ca0.6Sr0.1La0.3Fe12-xAlxO19 (0≤x≤1.4), have been prepared using the conventional ceramic techniques. The phase composition of the magnetic powders was characterized by X-ray diffraction (XRD). The XRD data show that the magnetic powders with Al content (x) from 0 to 0.8 show α-Fe2O3 as a second phase, while the magnetic powders with x from 1.0 to 1.4 consist of pure magnetoplumbite without any other impurity phases. A field emission scanning electron microscopy (FE-SEM) was used to observe the morphologies of the magnetic powders. FE-SEM images of the magnetic powders show the hexagonal platelet-like shape. The magnetic properties of the magnetic powders were measured by a physical property measurement system-vibrating sample magnetometer (PPMS-VSM). The saturation magnetization (Ms) linearly decreases with Al content (x) from 0 to 1.4. While the remanent magnetization (Mr) first increases with Al content (x) from 0 to 0.2 and then decreases when Al content (x)≥0.2. However, the coercivity (Hc) increases with Al content (x) from 0 to 1.4.

  8. Synthesis and characterization of cationic lipid coated magnetic nanoparticles using multiple emulsions as microreactors

    NASA Astrophysics Data System (ADS)

    Akbaba, Hasan; Karagöz, Uğur; Selamet, Yusuf; Kantarcı, A. Gülten

    2017-03-01

    The aim of this study was to develop a novel iron oxide nanoparticle synthesis method with in-situ surface coating. For this purpose multiple emulsions were used as microreactors for the first time and magnetic iron oxide particles synthesized in the core of cationic solid lipid nanoparticles. DLS, SEM, TEM, VSM, Raman Spectrometer, XRD, and XPS techniques were performed for characterization of the magnetic nanoparticles. Obtained magnetic nanoparticles are superparamagnetic and no additional process was needed for surface adjustments. They are positively charged as a result of cationic lipid coating and has appropriate particle size (<30 nm) for drug or nucleic acid delivery. Structure analysis showed that magnetic core material is in the form of magnetite. Saturation magnetization value was measured as 15-17 emu g-1 for lipid coated magnetic nanoparticles obtained by multiple emulsion method which is reasonably sufficient for magnetic targeting.

  9. Magnetic behaviour studies on nanocrystalline cobalt ferrite by employing the Arrott plot

    NASA Astrophysics Data System (ADS)

    Kumar, Rajnish; Kar, Manoranjan

    2016-05-01

    Vibrating Sample Magnetometer (VSM) has been used to analyze the magnetic behavior of ferrimagnetic material (CoFe2O4) synthesized by the citric acid modified sol-gel method. X-ray diffraction (XRD) pattern confirms the phase purity of the sample. Its magnetic measurement has been carried out at room temperature in the field range ±1.5T. The magnetocrystalline anisotropy and saturation magnetization of CoFe2O4 are two important parameters which need to be studied for exploring its technological applications like memory device, magnetic sensors etc. Law of Approach (LA) to saturation and the Arrott plot analysis have been carried out to obtain the saturation magnetization. The difference in the saturation magnetization obtained from the two methods gives the qualitative understanding of magnetocrystalline anisotropy and lattice strain present in the sample. The present study explores a new way of analyzing magnetic hysteresis loop of nanocrystalline cobalt ferrite.

  10. Surface stabilized nanosized Ce(x)Zr(1-x)O(2) solid solutions over SiO(2): characterization by XRD, Raman, and HREM techniques.

    PubMed

    Reddy, Benjaram M; Lakshmanan, Pandian; Khan, Ataullah; Loridant, Stéphane; López-Cartes, Carlos; Rojas, Teresa C; Fernandez, Asunción

    2005-07-21

    Ce(x)Zr(1)(-)(x)O(2) solid solutions deposited over silica surface were investigated by X-ray diffraction (XRD), Raman spectroscopy (RS), and high-resolution transmission electron microscopy (HREM) techniques in order to understand the role of silica support and the temperature stability of these composite oxides. For the purpose of comparison, an unsupported Ce(x)Zr(1)(-)(x)O(2) was also synthesized and subjected to characterization by various techniques. The Ce(x)Zr(1)(-)(x)O(2)/SiO(2) (CZ/S) (1:1:2 mole ratio based on oxides) was synthesized by depositing Ce(x)Zr(1)(-)(x)O(2) solid solution over a colloidal SiO(2) support by a deposition precipitation method and unsupported Ce(x)Zr(1)(-)(x)O(2) (CZ) (1:1 mole ratio based on oxides) was prepared by a coprecipitation procedure, and the obtained catalysts were subjected to thermal treatments from 773 to 1073 K. The XRD measurements disclose the presence of cubic phases with the composition Ce(0.75)Zr(0.25)O(2) and Ce(0.6)Zr(0.4)O(2) in CZ samples, while CZ/S samples possess Ce(0.75)Zr(0.25)O(2), Ce(0.6)Zr(0.4)O(2), and Ce(0.5)Zr(0.5)O(2) in different proportions. The crystallinity of these phases increased with increasing calcination temperature. The cell a parameter estimations indicate contraction of ceria lattice due to the incorporation of zirconium cations into the CeO(2) unit cell. Raman measurements indicate the presence of oxygen vacancies, lattice defects, and displacement of oxygen ions from their normal lattice positions in both the series of samples. The HREM results reveal, in the case of CZ/S samples, a well-dispersed nanosized Ce-Zr-oxides over the surface of amorphous SiO(2). The structural features of these crystals as determined by digital diffraction analysis of experimental images reveal that the Ce-Zr-oxides are mainly in the cubic geometry and exhibit high thermal stability. Oxygen storage capacity measurements by a thermogravimetric method reveal a substantial enhancement in the oxygen

  11. Part I. Synthesis and applications of molecular sieves. Part II. The effect of temperature and support in reduction of cobalt oxide: An in situ XRD study

    NASA Astrophysics Data System (ADS)

    Garces Trujillo, Luis Javier

    Part I. Alkylation of aniline (PhNH2) with methanol (MeOH) over co-crystallized zeolite RHO-Zeolite X (FAU) and over zeolite Linde Type L (Sr,K-LTL) as catalysts has been studied. Co-crystallized zeolite RHO-Zeolite X (FAU) favors the formation of N,N-dimethylaniline (NNDMA), with high selectivity >90%, having an advantage over pure zeolite X(FAU) of staying active even after 10 h of reaction. Activity of co-crystallized RHO-Zeolite X (FAU) is higher than that for Sr,K-LTL in terms of production of NNDMA. Octahedral molecular sieves (OMS-2) have been reported as catalysts for oxidation reactions. Effects of using polyvinyl alcohol (PVA) and polyvinyl pyrrolidone (PVP) in the synthesis of OMS-2 have been studied. Structure of OMS-2 was kept when PVA or PVP were used as indicated by XRD and FTIR data. PVA and PVP were useful to improve the film hardness of OMS-2 applied on glass surfaces as measured by the pencil hardness test, and Knoop microhardness test. By using PVA or PVP as non-chelating agents, an increase in surface area from 59 (m2/g) to 114 (m2/g), a decrease in particle size, from 29.8 nm to 12.1 nm, and a hardness value of 4H using the pencil hardness test, and 17.73 HK by Knoops micro hardness tests for OMS-2 prepared with PVA were observed. ZK-5 (KFI) molecular sieve was synthesized in the K2O: SrO: Al2O3: SiO2: 160 H2O: THF system using conventional hydrothermal heating. Products were characterized by XRD, TGA, FESEM, EDX and TPD-MS. Molar ratios of THF/Al2O3 from 0.4 to 1.0 gives best results in terms of crystallinity and purity for the prepared ZK-5. Part II. Reduction of cobalt oxide (Co 3O4) at different temperatures and in combination with different modifiers and supported on gamma-Al2O3 was monitored by in situ X-ray diffraction. Complete reduction of cobalt oxide to the (hcp) phase is observed at 250°C. Different reduction sequence can give different results in terms of crystalline phase obtained for cobalt even if the same maximum reduction

  12. Structural changes and thermal stability of charged LiNixMnyCozO2 cathode materials studied by combined in situ time-resolved XRD and mass spectroscopy

    DOE PAGES

    Bak, Seong -Min; Hu, Enyuan; Zhou, Yongning; ...

    2014-11-24

    Thermal stability of charged LiNixMnyCozO2 (NMC, with x + y + z = 1, x:y:z = 4:3:3 (NMC433), 5:3:2 (NMC532), 6:2:2 (NMC622), and 8:1:1 (NMC811)) cathode materials is systematically studied using combined in situ time- resolved X-ray diffraction and mass spectroscopy (TR-XRD/MS) techniques upon heating up to 600 °C. The TR-XRD/MS results indicate that the content of Ni, Co, and Mn significantly affects both the structural changes and the oxygen release features during heating: the more Ni and less Co and Mn, the lower the onset temperature of the phase transition (i.e., thermal decomposition) and the larger amount of oxygenmore » release. Interestingly, the NMC532 seems to be the optimized composition to maintain a reasonably good thermal stability, comparable to the low-nickel-content materials (e.g., NMC333 and NMC433), while having a high capacity close to the high-nickel-content materials (e.g., NMC811 and NMC622). The origin of the thermal decomposition of NMC cathode materials was elucidated by the changes in the oxidation states of each transition metal (TM) cations (i.e., Ni, Co, and Mn) and their site preferences during thermal decomposition. It is revealed that Mn ions mainly occupy the 3a octahedral sites of a layered structure (R3¯m) but Co ions prefer to migrate to the 8a tetrahedral sites of a spinel structure (Fd3¯m) during the thermal decomposition. Such element-dependent cation migration plays a very important role in the thermal stability of NMC cathode materials. The reasonably good thermal stability and high capacity characteristics of the NMC532 composition is originated from the well-balanced ratio of nickel content to manganese and cobalt contents. As a result, this systematic study provides insight into the rational design of NMC-based cathode materials with a desired balance between thermal stability and high energy density.« less

  13. Following the movement of Cu ions in a SSZ-13 zeolite during dehydration, reduction and adsorption: a combined in situ TP-XRD, XANES/DRIFTS study

    SciTech Connect

    Kwak, Ja Hun; Varga, Tamas; Peden, Charles HF; Gao, Feng; Hanson, Jonathan C.; Szanyi, Janos

    2014-05-05

    Cu-SSZ-13 has been shown to possess high activity and superior N2 formation selectivity in the selective catalytic reduction of NOx under oxygen rich conditions. Here, a combination of synchrotron-based (XRD and XANES) and vibrational (DRIFTS) spectroscopy tools have been used to follow the changes in the location and coordination environment of copper ions in a Cu-SSZ-13 zeolite during calcinations, reduction with CO, and adsorption of CO and H2O. XANES spectra collected during these procedures provides critical information not only on the variation in the oxidation state of the copper species in the zeolite structure, but also on the changes in the coordination environment around these ions as they interact with the framework, and with different adsorbates (H2O and CO). Time-resolved XRD data indicate the movement of copper ions and the consequent variation of the unit cell parameters during dehydration. DRIFT spectra provide information about the adsorbed species present in the zeolite, as well as the oxidation states of and coordination environment around the copper ions. A careful analysis of the asymmetric T-O-T vibrations of the CHA framework perturbed by copper ions in different coordination environments proved to be especially informative. The results of this study will aid the identification of the location, coordination and oxidation states of copper ions obtained during in operando catalytic studies. Financial support was provided by the US Department of Energy (DOE), Office of Energy Efficiency and Renewable Energy, Vehicle Technologies Program. Part of this work (sample preparation) was performed in the Environmental Molecular Sciences Laboratory (EMSL) at Pacific Northwest National Laboratory (PNNL). The EMSL is a national scientific user facility supported by the US DOE, Office of Biological and Environmental Research. PNNL is a multi-program national laboratory operated for the US DOE by Battelle. All of the spectroscopy work reported here was

  14. Uranium speciation as a function of depth in contaminated hanford sediments--a micro-XRF, micro-XRD, and micro- and bulk-XAFS study.

    PubMed

    Singer, David M; Zachara, John M; Brown, Gordon E

    2009-02-01

    The distribution and speciation of U and Cu in contaminated vadose zone and aquifer sediments from the U.S. DOE Hanford site (300 Area) were determined using a combination of synchrotron-based micro-X-ray fluorescence (microXRF) imaging, micro-X-ray absorption near edge structure (microXANES) spectroscopy, and micro-X-ray diffraction (microXRD) techniques combined with bulk U LIII-edge X-ray absorption fine structure (XAFS) spectroscopy. Samples were collected from within the inactive North Process Pond (NPP2) at 8 ft (2.4 m, NPP2-8) depth and 12 ft (3.7 m, NPP2-12) depth in the vadose zone, and fines were isolated from turbid groundwater just below the water Table (12-14 ft, approximately 4 m, NPP2-GW). microXRF imaging, microXRD, and microXANES spectroscopy revealed two major U occurrences within the vadose and groundwater zones: (1) low to moderate concentrations of U(VI) associated with fine-textured grain coatings that were consistently found to contain clinochlore (referred to here as chlorite) observed in all three samples, and (2) U(VI)-Cu(II) hotspots consisting of micrometer-sized particles associated with surface coatings on grains of muscovite and chlorite observed in samples NPP2-8' and NPP2-GW. In the aquifer fines (NPP2-GW), these particles were identified as cuprosklodowskite (cps: Cu[(UO2)(SiO2OH)]2 x 6H2O) and metatorbernite (mtb: Cu(UO2)2(PO4)2 x 8H2O). In contrast, the U-Cu-containing particles in the vadose zone were X-ray amorphous. Analyses of U LIII-edge XAFS spectra by linear-combination fitting indicated that U speciation consisted of (1) approximately 75% uranyl sorbed to chlorite and approximately 25% mtb-like X-ray amorphous U-Cu-phosphates (8 ft depth), (2) nearly 100% sorbed uranyl (12 ft depth), and (3) approximately 70% uranyl sorbed to chlorite and approximately 30% cps/mtb (groundwater zone). These findings suggest that dissolution of U(VI)-Cu(II)-bearing solids as well as desorption of U(VI), mainly from phyllosilicates, are

  15. Morphology evolution of single-crystalline hematite nanocrystals: magnetically recoverable nanocatalysts for enhanced facet-driven photoredox activity.

    PubMed

    Patra, Astam K; Kundu, Sudipta K; Bhaumik, Asim; Kim, Dukjoon

    2016-01-07

    We have developed a new green chemical approach for the shape-controlled synthesis of single-crystalline hematite nanocrystals in aqueous medium. FESEM, HRTEM and SAED techniques were used to determine the morphology and crystallographic orientations of each nanocrystal and its exposed facets. PXRD and HRTEM techniques revealed that the nanocrystals are single crystalline in nature; twins and stacking faults were not detected in these nanocrystals. The structural, vibrational, and electronic spectra of these nanocrystals were highly dependent on their shape. Different shaped hematite nanocrystals with distinct crystallographic planes have been synthesized under similar reaction conditions, which can be desired as a model for the purpose of properties comparison with the nanocrystals prepared under different reaction conditions. Here we investigated the photocatalytic performance of these different shaped-nanocrystals for methyl orange degradation in the presence of white light (λ > 420 nm). In this study, we found that the density of surface Fe(3+) ions in particular facets was the key factor for the photocatalytic activity and was higher on the bitruncated-dodecahedron shape nanocrystals by coexposed {104}, {100} and {001} facets, attributing to higher catalytic activity. The catalytic activity of different exposed facet nanocrystals were as follows: {104} + {100} + {001} (bitruncated-dodecahedron) > {101} + {001} (bitruncated-octahedron) > {001} + {110} (nanorods) > {012} (nanocuboid) which provided the direct evidence of exposed facet-driven photocatalytic activity. The nanocrystals were easily recoverable using an external magnet and reused at least six times without significant loss of its catalytic activity.

  16. Synthesis, structural and magnetic properties of ZnxMg1-xFe2O4 nanoferrites

    NASA Astrophysics Data System (ADS)

    Masina, Patrick; Moyo, Thomas; Abdallah, Hafiz M. I.

    2015-05-01

    Znx Mg1-x Fe2 O4 nanoparticles (0 ≤ x ≤ 1 in steps of 0.1) have been produced by centrifugation using the low temperature glycol-thermal method at 200 °C. Single-phase formation was confirmed by X-ray powder diffraction which revealed a well-defined cubic spinel structure with space group Fd3m. HRTEM and TEM were also used for the morphology studies. The crystallite size of the compounds ranged from 10.6 to 22.2 nm. A strong correlation was found between X-ray density and Zn-concentration, x. The magnetic properties as a function x were investigated by using 57Fe Mössbauer spectroscopy, magnetization measurements using a Lakeshore vibrating sample magnetometer (VSM) at room temperature. We also report VSM measurement on a cryogen free measurement system at isothermal temperatures between 4 K and 300 K in external applied magnetic fields of up to 5 T. For x < 0.8, the room-temperature Mössbauer results show that the samples were transformed from paramagnetic state to magnetic ordered state. The temperature-dependences of saturation magnetization and coercive field follow the modified Bloch's law and Kneller's law, respectively. Strong correlation between saturation magnetization MS (0) and crystallite size D is observed. Two distinct composition ranges with Zn content are identified for which MS (0) variation with x is explained by the Néel and Yafet-Kittel models.

  17. Magnetic Monopoles

    NASA Astrophysics Data System (ADS)

    't Hooft, Gerardus

    Before 1974, speculations concerning the existence of pure magnetic charges had been diverse. Many experimental searches had been carried out, and up to today, no single magnetic charge has ever been isolated, apart from some indirect evidence [1] that slowly evaporated when it appeared to be impossible to reproduce it. The theoretical situation was also somewhat confused. Dirac [2] had written a brilliant paper on the subject, showing the Dirac quantization rule. But then Julian Schwinger came with an argument that a factor 2 should be added to this quantization rule — this would be falsified by our later results; presently, we know that if the Dirac quantum is odd, there will be a violation of the spin-statistics addition theorem: fermions can be made out of bosons. Many researchers tried to devise a perturbative scheme to handle monopoles in field theory — in vain, because, if the electric charge unit e is small enough for perturbation theory to make sense, then the magnetic charge unit g = 2πn/e will be far too big. In particular, the use of a separate `dual vector potential' for magnetic charges is doomed to lead to inconsistencies if also electric charges occur. Either g or e is small, but never both…

  18. Magnetic tape

    NASA Technical Reports Server (NTRS)

    Robinson, Harriss

    1992-01-01

    The move to visualization and image processing in data systems is increasing the demand for larger and faster mass storage systems. The technology of choice is magnetic tape. This paper briefly reviews the technology past, present, and projected. A case is made for standards and the value of the standards to users.

  19. Magnetic Liquids

    NASA Technical Reports Server (NTRS)

    1987-01-01

    Ferrofluidics Corporation's recent innovation is a spindle for rotating computer discs that supports the disc's rotating shaft on a film of magnetic fluid instead of conventional ball bearings. According to its developers, the spindle offers greatly increased rotational stability, meaning substantially reduced vibration and mechanical noise, and non- repeatable runout. This allows disc drives to store two to 10 times more information.

  20. Identification of possible sources of atmospheric PM10 using particle size, SEM-EDS and XRD analysis, Jharia Coalfield Dhanbad, India.

    PubMed

    Roy, Debananda; Singh, Gurdeep; Gosai, Nitin

    2015-11-01

    Identification of responsible sources of pollution using physical parameter particulate matter (PM)10 in a critically polluted area is discussed in this paper. Database was generated by Ambient Air Quality Monitoring (AAQM) with respect to PM10 and PM2.5 in 18 monitoring stations at Jharia coalfield as per the siting criteria (IS: 5182, Part XIV) during 2011 to 2012. Identification of the probable sources of PM10 was carried out through particle size, shape, morphology analysis (scanning electron microscopy (SEM)), suitable compounds (X-ray diffraction (XRD)) and elements (energy-dispersive spectroscopy (EDS)). Monitoring stations nearby opencast mine were affected by the big-sized and irregular-shaped particles; on the other hand, monitoring stations nearby city were affected by the small-sized and regular-shaped particles. In a city area, additional sources like diesel generator (DG) set, construction activities, coal burning, etc., were identified. Blistering effects were also observed in the particles from mine fire-affected areas. Using the X-ray diffraction technique, presence of FeS2, CuO, FeSO4 and CuSO4 compounds was observed, which indicates the effects of mine fire on particulate emission due to presence of SO4(2-) and S2- ions.

  1. Composition-dependent structure of polycrystalline magnetron-sputtered V-Al-C-N hard coatings studied by XRD, XPS, XANES and EXAFS.

    PubMed

    Krause, Bärbel; Darma, Susan; Kaufholz, Marthe; Mangold, Stefan; Doyle, Stephen; Ulrich, Sven; Leiste, Harald; Stüber, Michael; Baumbach, Tilo

    2013-08-01

    V-Al-C-N hard coatings with high carbon content were deposited by reactive radio-frequency magnetron sputtering using an experimental combinatorial approach, deposition from a segmented sputter target. The composition-dependent coexisting phases within the coating were analysed using the complementary methods of X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), X-ray absorption near-edge spectroscopy (XANES) and extended X-ray absorption fine-structure spectroscopy (EXAFS). For the analysis of the X-ray absorption near-edge spectra, a new approach for evaluation of the pre-edge peak was developed, taking into account the self-absorption effects in thin films. Within the studied composition range, a mixed face-centred cubic (V,Al)(C,N) phase coexisting with a C-C-containing phase was observed. No indication of hexagonal (V,Al)(N,C) was found. The example of V-Al-C-N demonstrates how important a combination of complementary methods is for the detection of coexisting phases in complex multi-element coatings.

  2. Low-temperature synthesis of SrAl{sub 2}O{sub 4} by a modified sol-gel route: XRD and Raman characterization

    SciTech Connect

    Escribano, Purificacion; Marchal, Monica; Luisa Sanjuan, Maria; Alonso-Gutierrez, Pablo; Julian, Beatriz; Cordoncillo, Eloisa . E-mail: cordonci@qio.uji.es

    2005-06-15

    Among other alkaline-earth aluminates, the monoclinic (M) polymorph of SrAl{sub 2}O{sub 4} can be used as host material for Eu{sup 2+} luminescence based phosphors. With the aim of reducing the synthesis temperature of this polymorph, we have produced and characterized by XRD and Raman scattering solid solutions of the SrAl{sub 2-x}B{sub x}O{sub 4} system (x=<0.3) obtained by two different methods, a ceramic route and a modified sol-gel synthesis. Though the addition of boron lowers the temperature of obtention of the M polymorph in both type of samples, lower B contents are needed to stabilize the M form as single phase for samples prepared by the sol-gel method than through the ceramic route. In the sol-gel method, the M polymorph can be obtained at temperatures as low as 1200 deg. C, with a Boron content of just 1%. Rietveld profile analysis allows us to conclude that coexistence of the monoclinic and hexagonal polymorphs of SrAl{sub 2}O{sub 4} occurs for samples synthesized below an onset temperature of about 1000-1100 deg. C, that depends on the sample composition. Above those temperatures, only the monoclinic phase is formed.

  3. TF-XRD examination of surface-reactive TiO2 coatings produced by heat treatment and CO2 laser treatment.

    PubMed

    Moritz, Niko; Areva, Sami; Wolke, Joop; Peltola, Timo

    2005-07-01

    When surface-reactive (bioactive) coatings are applied to medical implants by means of CO2 laser processing, the bioactivity of the surface of the implant can be locally modified to match the properties of the surrounding tissues to provide a firm fixation of the implant. The aim of this study was to compare the heat treated TiO2 coatings with the laser-treated TiO2 coatings in terms of amorphous-crystalline-phase development. The coatings were characterized with thin-film X-ray diffraction (TF-XRD), atomic force microscopy (AFM) and scanning electron microscopy (SEM). The TiO2 coatings heat treated at 500 degrees C known to be bioactive in SBF (simulated body fluid) consisted mainly of anatase with some rutile-phase, suggesting a predominant effect of anatase on reactivity of coatings. However, the coatings preheat-treated at 500 degrees C with further laser treatment exhibited enhanced bioactivity while consisting mainly of rutile. These findings indicated a key role of both rutile and anatase for the reactivity of the coatings. Without preheat treatment, by laser treatment alone, the amorphous titania coatings developed into mixed anatase/rutile containing coatings. This structural organization and the increase in crystal size are thus considered to be the reasons for their bioactivity. The SBF results indicate the possibility to control bioactivity by altering laser power used through the anatase/rutile crystallinity enhancement.

  4. The Mineralogy of Martian Dust: Design and Analysis Considerations for an X-Ray Diffraction/X-Ray Fluorescence (XRD/XRF) Instrument for Exobiological Studies

    NASA Technical Reports Server (NTRS)

    Blake, David; Vaniman, David; Bish, David; Morrison, David (Technical Monitor)

    1994-01-01

    A principal objective of Mars exploration is the search for evidence of past life which may have existed during an earlier clement period of Mars history. We would like to investigate the history of surface water activity (which is a requirement for all known forms of life) by identifying and documenting the distribution of minerals which require water for their formation or distribution. A knowledge of the mineralogy of the present Martian surface would help to identify areas which, due to the early activity of water, might have harbored ancient life. It would be desirable to establish the presence and characterize the distribution of hydrated minerals such as clays, and of minerals which are primarily of sedimentary origin such as carbonates, silica and evaporites. Mineralogy, which is more critical to exobiological exploration than is simple chemical analysis (absent the detection of organics), will remain unknown or will at best be imprecisely constrained unless a technique sensitive to mineral structure such as powder X-ray diffraction (XRD) is employed. Additional information is contained in the original extended abstract.

  5. An XRD and Electron Diffraction Study of Cristobalite-Related Phases in the NaAlO 2-NaAlSiO 4System

    NASA Astrophysics Data System (ADS)

    Thompson, John G.; Melnitchenko, Alexandra; Palethorpe, Stephen R.; Withers, Ray L.

    1997-06-01

    A detailed study of the sodium aluminate-carnegieite system (Na2-xAl2-xSixO4, 0≤x≤1) at temperatures between 800 and 1300°C has revealed five previously unreported phases. All of the new phases can be described as modulated variants of an underlyingβ-cristobalite parent structure. Atx≈0.05 theγ-NaAlO2-type structure (P41212,a=1/2ap,c=cp) (p=parent) is stabilized to room-temperature; atx≈0.2-0.45 an orthorhombic (Pbca,a=2ap,b=2bp,c=1/2cp) KGaO2-type structure is obtained, except atx≈0.35 where a new tetragonal (P41212,a=2ap,c=cp) phase is observed; atx≈0.5-0.6 a new cubic (P213,a=2ap) phase is obtained; atx≈0.7-0.9 a new orthorhombic (Pc21b,a=2ap,b=2bp,c=2cp) phase is obtained. XRD and electron diffraction data, refined unit cell dimensions, and the phase relationships at 1300°C are presented. The proposed space group symmetries are based on observed extinction conditions and constraints provided by a modulated structure description of the new phases. The materials are prepared by gel synthesis followed by solid state reaction in air.

  6. Experimental (XRD, FT-IR and UV-Vis) and theoretical modeling studies of Schiff base (E)-N'-((5-nitrothiophen-2-yl)methylene)-2-phenoxyaniline.

    PubMed

    Tanak, Hasan; Ağar, Ayşen Alaman; Büyükgüngör, Orhan

    2014-01-24

    The Schiff base compound (E)-N'-((5-nitrothiophen-2-yl)methylene)-2-phenoxyaniline has been synthesized and characterized by IR, UV-Vis, and X-ray diffraction (XRD) methods. The molecular geometry from X-ray experiment in the ground state has been compared using the density functional theory (DFT) with the 6-311++G(d,p) basis set. The calculated results show that the optimized geometry can well reproduce the crystal structure, and the theoretical vibrational frequency values show good agreement with experimental values. By using TD-DFT method, electronic absorption spectra of the title compound have been predicted and a good agreement with the TD-DFT method and the experimental one is determined. The energetic behavior of the title compound in solvent media has been examined using B3LYP method with the 6-311++G(d,p) basis set by applying the Onsager and the integral equation formalism polarizable continuum model (IEF-PCM). The predicted nonlinear optical properties of the title compound are greater than ones of urea. In addition, DFT calculations of the title compound, molecular electrostatic potential (MEP), natural bond orbital (NBO) and thermodynamic properties were performed at B3LYP/6-311++G(d,p) level of theory.

  7. Composition-dependent structure of polycrystalline magnetron-sputtered V–Al–C–N hard coatings studied by XRD, XPS, XANES and EXAFS

    PubMed Central

    Krause, Bärbel; Darma, Susan; Kaufholz, Marthe; Mangold, Stefan; Doyle, Stephen; Ulrich, Sven; Leiste, Harald; Stüber, Michael; Baumbach, Tilo

    2013-01-01

    V–Al–C–N hard coatings with high carbon content were deposited by reactive radio-frequency magnetron sputtering using an experimental combinatorial approach, deposition from a segmented sputter target. The composition-dependent coexisting phases within the coating were analysed using the complementary methods of X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), X-ray absorption near-edge spectroscopy (XANES) and extended X-ray absorption fine-structure spectroscopy (EXAFS). For the analysis of the X-ray absorption near-edge spectra, a new approach for evaluation of the pre-edge peak was developed, taking into account the self-absorption effects in thin films. Within the studied composition range, a mixed face-centred cubic (V,Al)(C,N) phase coexisting with a C–C-containing phase was observed. No indication of hexagonal (V,Al)(N,C) was found. The example of V–Al–C–N demonstrates how important a combination of complementary methods is for the detection of coexisting phases in complex multi-element coatings. PMID:24046506

  8. Limestone calcination under calcium-looping conditions for CO2 capture and thermochemical energy storage in the presence of H2O: an in situ XRD analysis.

    PubMed

    Valverde, Jose Manuel; Medina, Santiago

    2017-03-15

    This work reports an in situ XRD analysis of whether the calcination/carbonation behavior of natural limestone (CaCO3) is affected by the addition of H2O to the calciner at a very low concentration under relevant Calcium-Looping (CaL) conditions for CO2 capture in coal fired power plants (CFPP) and Thermochemical Energy Storage (TCES) in Concentrated Solar Power plants (CSP). Previous studies have demonstrated that the presence of steam in the calciner at a high concentration yields a significant increase in the reaction rate. However, a further undesired consequence is the serious deterioration of the CaO mechanical strength, which would lead to particle attrition and mass loss in any CaL process based on the use of circulating fluidized beds. The results presented in this manuscript on the time evolution of the wt% and crystallite size of the phases involved in the calcination/carbonation reactions indicate that the calcination rate is still notably increased by the presence of H2O at very low concentrations whereas the reactivity toward carbonation and crystal structure of the formed CaO are not essentially affected, which suggests that the CaO mechanical strength is not impaired. Thus, the benefit of using steam for calcination in the CaL process could be still retained while at the same time particle attrition would not be promoted.

  9. XRD technique: a way to discriminate structural changes in iron-based amorphous materials [An Alternative Method of Synthesizing Iron-based Amorphous Alloys

    SciTech Connect

    Saw, Cheng K.; Day, Dan; Farmer, Joe C.; Bauer, William

    2008-02-06

    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.

  10. Development of an x-ray diffraction camera used in magnetic fields up to 10 T.

    PubMed

    Mitsui, Yoshifuru; Koyama, Keiichi; Takahashi, Kohki; Watanabe, Kazuo

    2011-12-01

    A high-field x-ray diffraction (HF-XRD) camera was developed to observe structural changes of magnetic materials in magnetic fields up to 10 T. The instrument mainly consists of a Debye-Scherrer-type camera with a diameter of 80.1 mm, a 10-T cryocooled superconducting magnet with a 100-mm room-temperature bore, an x-ray source, a power supply, and a chiller for the x-ray source. An x-ray detector (image plate) in the HF-XRD camera can be taken out and inserted into the magnet without changing the sample position. The performance of the instrument was tested by measuring the HF-XRD for silicon and ferromagnetic MnBi powders. A change of x-ray diffraction pattern was observed due to the magnetic orientation of MnBi, showing that the instrument is useful for studying field-induced orientation processes and structural properties of field-controlled materials.

  11. Effect of air annealing on structural and magnetic properties of Ni/NiO nanoparticles

    NASA Astrophysics Data System (ADS)

    Nadeem, K.; Ullah, Asmat; Mushtaq, M.; Kamran, M.; Hussain, S. S.; Mumtaz, M.

    2016-11-01

    We reported systematic study on structural and magnetic properties of nickel/nickel oxide (Ni/NiO) nanoparticles annealed under air atmosphere at different temperatures in the range 400-800 °C. The XRD spectra revealed two phases such as Ni and NiO. The average crystallite size increases with increasing annealing temperature. A phase diagram was developed between two phases versus annealing temperature using XRD analysis. At lower annealing temperatures, Ni phase is dominant which does not easily undergo oxidation to form NiO. The NiO phase increases with increasing annealing temperature. FTIR spectroscopy revealed an increase in the NiO phase content at higher annealing temperature, which is in agreement with the XRD analysis. SEM images showed that nanoparticles are well separated at lower annealing temperatures but get agglomerated at higher annealing temperatures. The ferromagnetic (FM) Ni phase content and saturation magnetization (Ms) showed nearly the same trend with increasing annealing temperature. The nanoparticles annealed at 500 °C and 800 °C revealed highest and lowest Ms values, respectively, which is in accordance with the XRD phase diagram. Coercivity showed an overall decreasing trend with increasing annealing temperature due to decreased concentration of FM Ni phase and increasing average crystallite size. All these measurements indicate that the structural and magnetic properties of Ni/NiO nanoparticles are strongly influenced by the annealing temperature.

  12. Analysis of "Meridiani Planum"-like evaporites using CheMin, an XRD/XRF instrument proposed for the Mars Science Laboratory (MSL)

    NASA Astrophysics Data System (ADS)

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

    2004-12-01

    The discovery of up to 30-40 wt% sulfate salts in sediments at Meridiani Planum [1-2] indicates that evaporite sediments have played an important role in the hydrogeologic history of Mars. Data available to date support the presence of the mineral jarosite (a hydrous Fe-sulfate), Mg-sulfate, and lesser amounts of salts containing Cl and Br. One of the most exciting features of the Meridiani sediments is the possibility that the salts may be hydrated. Water storage in minerals may be a significant source of the elevated hydrogen abundances seen in some equatorial regions by the Odyssey spacecraft, with abundances up to 8-9 wt% water-equivalent present in areas where water ice should not be stable [3]. Is it possible that salt hydrates in evaporite sediments can account for some of this equatorial water? The ability to quantify mixed-salt mineralogies will be important for determining brine history on Mars. Definitive mineralogy, a key requirement of MSL, can be accomplished by the CheMin X-ray Diffraction / X-ray Fluorescence (XRD/XRF) instrument [4]. The MSL approach to investigating this kind of deposit can be based on the capabilities demonstrated by MER-B (visual petrography, Mossbauer, APXS, and Mini-TES). The enhanced drilling capability of MSL can be used to collect and transfer cores to the rock crusher for pulverizing and ultimate delivery of crushed material to CheMin. If MSL is able to traverse kilometers or tens of kilometers, CheMin characterization of changes in evaporite mineralogy, zonation in evaporite facies or the mineralogical identity of detrital grains could be used to conduct an analysis of the evaporative basin - lateral extent, water depth, salinity, facies changes, etc. The ability to quantify hydrated mineral assemblages will be important for reconstructing brine evolution and for determining the nature of interactions between brine minerals and detrital mineralogy. The important contribution of CheMin to a site like Meridiani will be to

  13. Magnetic and mineralogical properties of salt rocks from the Zechstein of the Northern German Basin

    NASA Astrophysics Data System (ADS)

    Heinrich, Frances C.; Schmidt, Volkmar; Schramm, Michael; Mertineit, Michael

    2017-01-01

    Magnetic properties of rocks are often studied to characterize composition and fabric of rocks. For salt rocks, the basic relationships between their magnetic properties and composition, which are necessary to interpret rock magnetic data, are not yet established. Therefore, we studied different types of natural salt rock and pure salt minerals. We measured their magnetic properties (magnetic susceptibility, IRM acquisition curves, FORC diagrams, temperature-dependent magnetic susceptibility) and used analytical methods such as microscopy, XRD and ICP-OES to understand the relationship between magnetic properties and mineralogy. Salt rocks mainly consist of the diamagnetic minerals halite, carnallite, sylvine and anhydrite with negative magnetic susceptibilities. The magnetic susceptibilities of pure synthetic NaCl and KCl single crystals, show values of -14.5 × 10-6 SI and -13.5 × 10-6 SI, respectively. In contrast, in natural salt rocks higher magnetic susceptibility values were measured. The magnetic susceptibility of the samples investigated in this study shows a general increase from light rock salt (max. -10 × 10-6 SI) over carnallitite (max. 134 × 10-6 SI) to red sylvinite (max. 270 × 10-6 SI). Whole rock analyses suggests that increased magnetic susceptibility can be attributed to paramagnetic and ferromagnetic minerals that are contained within the insoluble residue. The magnetic susceptibility is mainly controlled by magnetite and phyllosilicates. Its measurement can therefore be used to detect subtle changes in the content of these minerals.

  14. Magnetic and structural properties of ferrofluids based on Cobalt-Zinc ferrite nanoparticles

    NASA Astrophysics Data System (ADS)

    Prieto, P.; Lopez, J.; Gomez, M. E.; Prado, J.; Caicedo, J.; Zambrano, G.; Gonzalez, L.; Esteve, J.

    2012-02-01

    Ferrofluids are colloidal systems composed of a single domain of magnetic nanoparticles with a mean diameter around 10 nm, dispersed in a liquid carrier. Magnetic Co(1-x)ZnxFe2O4 ferrite nanoparticles were prepared via co-precipitation method from aqueous salt solutions in an alkaline medium. The composition and structure of the samples were characterized through EDX and XRD, respectively. Transmission Electron Microscopy studies permitted determining nanoparticle size. Grain size of nanoparticle conglomerates was established via Atomic Force Microscopy. The magnetic behavior of ferrofluids was characterized by Vibrating Sample Magnetometer; and finally, a Magnetic Force Microscope was used to visualize the magnetic domains of nanoparticles. The mean size of the crystallite of nanoparticles determined by using the Scherrer approximation diminished when the Zn concentration increases. The size of the nanoparticles obtained by TEM is in good agreement with the crystallite size calculated from XRD measures. The magnetic properties investigated at room temperature presented super-paramagnetic behavior, determined by the shape of the hysteresis loop. Finally, our magnetic nanoparticles are considered a soft magnetic material.

  15. Magnetic performance of orthorhombic Mn35Ge35Te30 nanocrystals

    NASA Astrophysics Data System (ADS)

    Mahdy, Iman A.

    2017-01-01

    Nanocrystalline antiferromagnetic Mn35Ge35Te30 diluted magnetic semiconductors powder syntheses by the conventional direct reaction of pure metals. Nanocrystalline nature of the prepared sample confirmed using various techniques, where x-Ray diffraction (XRD) and atomic force microscope (AFM) measurements shows ~96 nm particle size, while transmission electron microscope (TEM) shows 92 nm particle size. XRD analysis show orthorhombic symmetry with lattice parameters a=7.386611±(0.0066) Å, b=8.962502±(0.0090) Å and c=7.027349±(0.0040) Å. Electron Spin resonance (ESR) show a broad asymmetric line whereas the remnant Mn2+ six-hyperfine lines are broadened within |+1/2>→|-1/2> line according to high anisotropy; calculated Landé g-factor is 2.047. Vibrating sample magnetometer (VSM) analysis, field-moment characteristics revealed a hysteresis loop with small coercive field indicating that Mn35Ge35Te30 is a soft magnetic material. Moreover, hysteresis measurements at different temperatures show increasing magnetization with increasing temperature up to 150 K followed by decreased with increasing temperature up to 300 K. This behavior indicated to the antiferromagnetic nature of the prepared nanocrystalline materials. Magnetic moment - temperature measurements show Néel temperature TN=172.6 K. Magnetic force microscope revealed magnetic domains as a result of interaction between magnetic dipole moments of magnetic cantilever and pressed powder.

  16. Magnetic switching

    SciTech Connect

    Birx, D.; Cook, E.; Hawkins, S.; Poor, S.; Reginato, L.; Schmidt, J.; Smith, M.

    1983-06-01

    The paper discusses the development program in magnetic switching which was aimed at solving the rep-rate and reliability limitations of the ATA spark gaps. The end result has been a prototype physically very similar to the present Advanced Test Accelerator (ATA) pulse power unit but vastly superior in performance. This prototype, which is easily adaptable to the existing systems, has achieved a burst rep-rate of 20 kHz and an output voltage of 500 kV. A one-on-one substitution of the existing pulse power module would result in a 100 MeV accelerator. Furthermore, the high efficiency of the magnetic pulse compression stages has allowed CW operation of the prototype at one kilohertz opening up other applications for the pulse power. Performance and design details will be described.

  17. Structural and magnetic properties of mechanically alloyed Co 20Cu 80 solid solution

    NASA Astrophysics Data System (ADS)

    Yoo, Y. G.; Yang, D. S.; Yu, S. C.; Kim, W. T.; M. Lee, J.

    1999-08-01

    Microstructural change during the mechanical alloying of Co 20Cu 80 has been studied by X-ray diffractometry (XRD) and extended X-ray absorption fine structure (EXAFS) techniques. EXAFS analysis shows clearly the formation of supersaturated Co 20Cu 80 solid solution with FCC crystal structure during mechanical alloying, which is in good agreement with XRD analysis. Magnetic properties also have been studied by SQUID magnetometer from 4 to 290 K. The supersaturated Co 20Cu 80 solid solution shows wide distribution in Co cluster size due to the continuous blocking of Co cluster as a function of temperature.

  18. Adsorption and Separation of Light Gases on an Amino-Functionalized Metal–Organic Framework: An Adsorption and In Situ XRD Study

    SciTech Connect

    Couck S.; Stavitski E.; Gobehiya, E.; Kirschhock, C.E.A.; Serra-Crespo, P.; Juan-Alcaniz, J.; Martinez Joaristi, A.; Gascon, J.; Kapteijn, F.; Baron, G. V.; Denayer J.F.M.

    2012-02-29

    The NH{sub 2}-MIL-53(Al) metal-organic framework was studied for its use in the separation of CO{sub 2} from CH{sub 4}, H{sub 2}, N{sub 2} C{sub 2}H{sub 6} and C{sub 3}H{sub 8} mixtures. Isotherms of methane, ethane, propane, hydrogen, nitrogen, and CO{sub 2} were measured. The atypical shape of these isotherms is attributed to the breathing properties of the material, in which a transition from a very narrow pore form to a narrow pore form and from a narrow pore form to a large pore form occurs, depending on the total pressure and the nature of the adsorbate, as demonstrated by in-situ XRD patterns measured during adsorption. Apart from CO{sub 2}, all tested gases interacted weakly with the adsorbent. As a result, they are excluded from adsorption in the narrow pore form of the material at low pressure. CO{sub 2} interacted much more strongly and was adsorbed in significant amounts at low pressure. This gives the material excellent properties to separate CO{sub 2} from other gases. The separation of CO{sub 2} from methane, nitrogen, hydrogen, or a combination of these gases has been demonstrated by breakthrough experiments using pellets of NH{sub 2}-MIL-53(Al). The effect of total pressure (1-30 bar), gas composition, temperature (303-403 K) and contact time has been examined. In all cases, CO{sub 2} was selectively adsorbed, whereas methane, nitrogen, and hydrogen nearly did not adsorb at all. Regeneration of the adsorbent by thermal treatment, inert purge gas stripping, and pressure swing has been demonstrated. The NH{sub 2}-MIL-53(Al) pellets retained their selectivity and capacity for more than two years.

  19. XRD line-broadening characteristics of M-oxides (M = Mg, Mg-Al, Y, Fe) nanoparticles produced by coprecipitation method

    SciTech Connect

    Pratapa, S.; Susanti, L.; Insany, Y. A. S.; Alfiati, Z.; Hartono, B.; Mashuri,; Triwikantoro; Baqiya, M. A.; Purwaningsih, S.; Yahya, E.; Darminto; Taufiq, Ahmad; Fuad, Abdullah

    2010-10-24

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

  20. Magnetic Materials

    DTIC Science & Technology

    1985-03-01

    Defense supported the development of microwave ferrites , and today 85 percent of that market is still military. Magnetostrictive sensors for sonar...or hard ferrite , Although both cobalt and samarium are expensive and the production process is difficult v4,*-°’. because of the strong tendency of...plentiful materials supply and low magnet cost. This calls for automated mass-production methods for ferrites and, perhaps, Nd-Fe-based REPMs. But for

  1. Optical Magnetism

    DTIC Science & Technology

    2014-09-15

    anisotropic and exhibit chirality , and investigated the dispersion relations of plane wave propagation in chiral (bi-isotropic) and the more general...tensor components of ǫr, µr, and in addition the chirality parameter tensor κ. II. MAGNETISM FROM CARBON NANOTUBE COIL ARRAYS Our preliminary studies...nanocoils, it is important to pay attention to the subtle issue of chirality . Most meta- materials exhibit only simple constitutive relations of the form D

  2. Effects of uniformities of deposition of respirable particles on filters on determining their quartz contents by using the direct on-filter X-ray diffraction (DOF XRD) method.

    PubMed

    Chen, Ching-Hwa; Tsaia, Perng-Jy; Lai, Chane-Yu; Peng, Ya-Lian; Soo, Jhy-Charm; Chen, Cheng-Yao; Shih, Tung-Sheng

    2010-04-15

    In this study, field samplings were conducted in three workplaces of a foundry plant, including the molding, demolding, and bead blasting, respectively. Three respirable aerosol samplers (including a 25-mm aluminum cyclone, nylon cyclone, and IOSH cyclone) were used side-by-side to collect samples from each selected workplace. For each collected sample, the uniformity of the deposition of respirable dusts on the filter was measured and its free silica content was determined by both the DOF XRD method and NIOSH 7500 XRD method (i.e., the reference method). A same trend in measured uniformities can be found in all selected workplaces: 25-mm aluminum cyclone>nylon cyclone>IOSH cyclone. Even for samples collected by the sampler with the highest uniformity (i.e., 25-mm aluminum cyclone), the use of the DOF XRD method would lead to the measured free silica concentrations 1.15-2.89 times in magnitude higher than that of the reference method. A new filter holder should be developed with the minimum uniformity comparable to that of NIOSH 7500 XRD method (=0.78) in the future. The use of conversion factors for correcting quartz concentrations obtained from the DOF XRD method based on the measured uniformities could be suitable for the foundry industry at this stage.

  3. Magnetic Reconnection

    SciTech Connect

    Masaaki Yamada, Russell Kulsrud and Hantao Ji

    2009-09-17

    We review the fundamental physics of magnetic reconnection in laboratory and space plasmas, by discussing results from theory, numerical simulations, observations from space satellites, and the recent results from laboratory plasma experiments. After a brief review of the well-known early work, we discuss representative recent experimental and theoretical work and attempt to interpret the essence of significant modern findings. In the area of local reconnection physics, many significant findings have been made with regard to two- uid physics and are related to the cause of fast reconnection. Profiles of the neutral sheet, Hall currents, and the effects of guide field, collisions, and micro-turbulence are discussed to understand the fundamental processes in a local reconnection layer both in space and laboratory plasmas. While the understanding of the global reconnection dynamics is less developed, notable findings have been made on this issue through detailed documentation of magnetic self-organization phenomena in fusion plasmas. Application of magnetic reconnection physics to astrophysical plasmas is also brie y discussed.

  4. Structural and magnetic characterization of the Y xSr 1-xMnO 3 systems

    NASA Astrophysics Data System (ADS)

    Saleta, Martín E.; Polla, Griselda; Quintero, Mariano; Vega, Daniel

    2006-10-01

    Structural, magnetic and electrical transport properties were studied in the solid solution Y xSr 1-xMnO 3 for the range of 0.4⩽ x⩽0.9. These compounds were obtained in the perovskite phase (ABO 3) and scan a wide range of mean ionic radii for the A site and the corresponding tolerance factor. The samples were synthesized using a liquid mix method, at 900 °C in O 2 atmosphere, and characterized by X-ray powder diffraction (XRD), magnetic susceptibility and electric transport measurements. XRD data for all samples were refined by the Rietveld method in the space group Pnma. Magnetic measurements indicate a paramagnetic behavior in the range between 100 and 300 K. The dependence of structural parameters, like octahedron distortion and A site coordination number as a function of Y content was obtained showing a clear correlation with the magnetic behavior.

  5. Optical and magnetic properties of zinc oxide quantum dots doped with cobalt and lanthanum.

    PubMed

    Yu, Shiyong; Zhao, Jing; Su, Hai-Quan

    2013-06-01

    Cobalt and Lanthanum-doped ZnO QDs are synthesized by a modified sol-gel method under atmospheric conditions. The as-prepared quantum dots are characterized by X-ray powder diffraction (XRD), energy dispersive X-ray (EDX) analysis and high resolution transmission electron microscopy (HRTEM). The optical properties of the products are studied by fluorescent spectroscopy. With a proper Co and La doping, these nanoparticles possess exceptionally small size and enhanced fluorescence. Hysteresis loops of un-doped ZnO QDs and Co and La-doped ZnO QDs indicate that both the samples show ferromagnetic behavior at room temperature. Finally, these nanoparticles can label the BGC 803 cells successfully in short time and present no evidence of toxicity or adverse affect on cell growth even at the concentration up to 1 mM. We expect that the as-prepared Co and La-doped ZnO QDs can provide a better reliability of the collected data and find promising applications in biological, medical and other fields.

  6. Magnetic anisotropy of ultrafine 316L stainless steel fibers

    NASA Astrophysics Data System (ADS)

    Shyr, Tien-Wei; Huang, Shih-Ju; Wur, Ching-Shuei

    2016-12-01

    An as-received 316L stainless steel fiber with a diameter of 20 μm was drawn using a bundle drawing process at room temperature to form ultrafine stainless steel fibers with diameters of 12, 8, and 6 μm. The crystalline phases of the fibers were analyzed using the X-ray diffraction (XRD) profile fitting technique. The grain sizes of γ-austenite and α‧-martensite were reduced to nanoscale sizes after the drawing process. XRD analysis and focused ion beam-scanning electron microscope observations showed that the newly formed α‧-martensitic grains were closely arrayed in the drawing direction. The magnetic property was measured using a superconducting quantum interference device vibrating sample magnetometer. The magnetic anisotropy of the fibers was observed by applying a magnetic field parallel and perpendicular to the fiber axis. The results showed that the microstructure anisotropy including the shape anisotropy, magnetocrystalline anisotropy, and the orientation of the crystalline phases strongly contributed to the magnetic anisotropy.

  7. Synthesis of high magnetization Fe and FeCo nanoparticles by high temperature chemical reduction

    SciTech Connect

    Kandapallil, B; Colborn, RE; Bonitatibus, PJ; Johnson, F

    2015-03-15

    Fe and FeCo ferromagnetic nanoparticles in the 5-10 nm size regimes featuring high magnetization were synthesized using a modified chemical reduction method. The structure and morphology of these nanoparticles were confirmed by XRD and TOM analysis. These small, monodisperse and phase pure nanoparticles exhibited magnetic saturation of 210 emu/g (Fe) and 220 emu/g (Fe+Co) for Fe and FeCo nanoparticles respectively. The magnetization was found to be dependent on the temperature at which the reducing agent was introduced. (C) 2014 Elsevier B.V. All rights reserved,

  8. Magnetic particulate matters in the ashes of few commonly used Indian cigarettes.

    PubMed

    Bhattacharjee, Ashis; Mandal, Haradhan; Roy, Madhusudan; Kusz, Joachim; Zubko, Maciej

    2014-11-01

    Physical aspects of tobacco samples, used in some commonly available Indian brands of cigarettes, with emphasis on their magnetic characterization before and after they get burnt into ashes, are described. The present work highlights the ultrafine nature of the cigarette ashes and provides a compositional insight of their constituent particulate matters as revealed by the XRD and SEM studies. Based on the EDX spectra, elemental distributions of different tobacco samples, before and after they get burnt, are presented. In this work, magnetic measurements of the un-burnt tobacco samples are reported. An attempt is made to shed light on the origin of magnetism observed in these samples.

  9. Synthesis of nanostructured iron oxides dispersed in carbon materials and in situ XRD study of the changes caused by thermal treatment

    NASA Astrophysics Data System (ADS)

    Gonçalves, Gustavo R.; Schettino, Miguel A.; Morigaki, Milton K.; Nunes, Evaristo; Cunha, Alfredo G.; Emmerich, Francisco G.; Passamani, Edson C.; Baggio-Saitovitch, Elisa; Freitas, Jair C. C.

    2015-07-01

    Carbon-based magnetic nanocomposites are of large interest for applications in catalysis, magnetic separation, water cleaning, and magnetic resonance imaging, among others. This work describes the synthesis of nanocomposites consisting of iron oxides dispersed into a char (obtained from the carbonization at 700 °C of a lignocellulosic precursor) and the study of the thermal transformations occurring in these materials as a consequence of heat treatments. The materials were prepared by impregnation of the char with iron nitrate in the presence of ammonium hydroxide in aqueous suspension. X-ray diffraction experiments performed using synchrotron radiation and Mössbauer spectroscopy showed that the as-prepared material was composed of amorphous Fe3+ oxides. Scanning electron microscopy images combined with energy-dispersive X-ray spectrometry indicated a homogeneous dispersion of iron oxides and of silica particles (naturally present in the lignocellulosic precursor) throughout the char. X-ray diffractograms recorded in situ during the heat treatment of the as-prepared material showed the presence of small hematite crystallites (average size 22 nm) starting from ca. 300 °C. Further heating caused a progressive growth of the hematite crystallites up to ca. 500 °C, when the conversion to magnetite (Fe3O4) started to take place. At higher temperatures, wüstite (Fe1-xO) was detected as an intermediate phase and austenitic iron (γ-Fe) became the dominant phase at temperatures from 900 °C. A steep weight loss was observed in the TG curve accompanying this last reduction stage; upon cooling, γ-Fe was converted into α-Fe (ferrite), which was the dominant phase at room temperature in this heat-treated sample.

  10. Synthesis of magnetic nanofibers using femtosecond laser material processing in air

    PubMed Central

    2011-01-01

    In this study, we report formation of weblike fibrous nanostructure and nanoparticles of magnetic neodymium-iron-boron (NdFeB) via femtosecond laser radiation at MHz pulse repetition frequency in air at atmospheric pressure. Scanning electron microscopy (SEM) analysis revealed that the nanostructure is formed due to aggregation of polycrystalline nanoparticles of the respective constituent materials. The nanofibers diameter varies between 30 and 70 nm and they are mixed with nanoparticles. The effect of pulse to pulse separation rate on the size of the magnetic fibrous structure and the magnetic strength was reported. X-ray diffraction (XRD) analysis revealed metallic and oxide phases in the nanostructure. The growth of magnetic nanostructure is highly recommended for the applications of magnetic devices like biosensors and the results suggest that the pulsed-laser method is a promising technique for growing nanocrystalline magnetic nanofibers and nanoparticles for biomedical applications. PMID:21711890

  11. Powder XRD, SEM, and Multinuclear MAS-NMR Investigations of the Interactions Between Glass and Crystalline Phases of Li, Na, or K Ceramic Waste Forms

    SciTech Connect

    Lambregts, Marsha J.; Frank, Steve M.

    2005-08-01

    Interactions between the glass and crystalline phases of ceramic waste forms were investigated via powder X-ray diffraction, scanning electron microscopy, and Si-29, Al-27, Na-23, Li-7, and Cl-35 magic angle spinning nuclear magnetic resonance spectroscopy. LiCl, NaCl, or KCl waste form samples were made with or without glass. The waste forms containing glass consist of sodalite and glass phases with minor amounts of nepheline. Samples without glass form varying amounts of sodalite and nepheline. The glass frit, intended to bind the zeolite particles together, changes in composition, showing marked increases in aluminum and alkali content.

  12. Noncentrosymmetric Magnets Hosting Magnetic Skyrmions.

    PubMed

    Kanazawa, Naoya; Seki, Shinichiro; Tokura, Yoshinori

    2017-03-17

    The concept of a skyrmion, which was first introduced by Tony Skyrme in the field of particle physics, has become widespread in condensed matter physics to describe various topological orders. Skyrmions in magnetic materials have recently received particular attention; they represent vortex-like spin structures with the character of nanometric particles and produce fascinating physical properties rooted in their topological nature. Here, a series of noncentrosymmetric ferromagnets hosting skyrmions is reviewed: B20 metals, Cu2 OSeO3 , Co-Zn-Mn alloys, and GaV4 S8 , where Dzyaloshinskii-Moriya interaction plays a key role in the stabilization of skyrmion spin texture. Their topological spin arrangements and consequent emergent electromagnetic fields give rise to striking features in transport and magnetoelectric properties in metals and insulators, such as the topological Hall effect, efficient electric-drive of skyrmions, and multiferroic behavior. Such electric controllability and nanometric particle natures highlight magnetic skyrmions as a potential information carrier for high-density magnetic storage devices with excellent energy efficiency.

  13. Magnetic liposomes for colorectal cancer cells therapy by high-frequency magnetic field treatment

    NASA Astrophysics Data System (ADS)

    Hardiansyah, Andri; Huang, Li-Ying; Yang, Ming-Chien; Liu, Ting-Yu; Tsai, Sung-Chen; Yang, Chih-Yung; Kuo, Chih-Yu; Chan, Tzu-Yi; Zou, Hui-Ming; Lian, Wei-Nan; Lin, Chi-Hung

    2014-09-01

    In this study, we developed the cancer treatment through the combination of chemotherapy and thermotherapy using doxorubicin-loaded magnetic liposomes. The citric acid-coated magnetic nanoparticles (CAMNP, ca. 10 nm) and doxorubicin were encapsulated into the liposome (HSPC/DSPE/cholesterol = 12.5:1:8.25) by rotary evaporation and ultrasonication process. The resultant magnetic liposomes ( ca. 90 to 130 nm) were subject to characterization including transmission electron microscopy (TEM), dynamic light scattering (DLS), X-ray diffraction (XRD), zeta potential, Fourier transform infrared (FTIR) spectrophotometer, and fluorescence microscope. In vitro cytotoxicity of the drug carrier platform was investigated through 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide (MTT) assay using L-929 cells, as the mammalian cell model. In vitro cytotoxicity and hyperthermia (inductive heating) studies were evaluated against colorectal cancer (CT-26 cells) with high-frequency magnetic field (HFMF) exposure. MTT assay revealed that these drug carriers exhibited no cytotoxicity against L-929 cells, suggesting excellent biocompatibility. When the magnetic liposomes with 1 μM doxorubicin was used to treat CT-26 cells in combination with HFMF exposure, approximately 56% cells were killed and found to be more effective than either hyperthermia or chemotherapy treatment individually. Therefore, these results show that the synergistic effects between chemotherapy (drug-controlled release) and hyperthermia increase the capability to kill cancer cells.

  14. Magnetically separable nanocomposites with photocatalytic activity under visible light for the selective transformation of biomass-derived platform molecules

    EPA Science Inventory

    Novel magnetically separable TiO2-guanidine-(Ni,Co)Fe2O4 nanomaterials were prepared and characterised by a series of techniques including XRD, SEM, TEM, N2 physisorption as well as XPS and subsequently tested for their photocatalytic activities in the selective transformation of...

  15. Magnetic Cellulose Nanocrystal Based Anisotropic Polylactic Acid Nanocomposite Films: Influence on Electrical, Magnetic, Thermal, and Mechanical Properties.

    PubMed

    Dhar, Prodyut; Kumar, Amit; Katiyar, Vimal

    2016-07-20

    This paper reports a single-step co-precipitation method for the fabrication of magnetic cellulose nanocrystals (MGCNCs) with high iron oxide nanoparticle content (∼51 wt % loading) adsorbed onto cellulose nanocrystals (CNCs). X-ray diffraction (XRD), Fourier transform infrared (FTIR), and Raman spectroscopic studies confirmed that the hydroxyl groups on the surface of CNCs (derived from the bamboo pulp) acted as anchor points for the adsorption of Fe3O4 nanoparticles. The fabricated MGCNCs have a high magnetic moment, which is utilized to orient the magnetoresponsive nanofillers in parallel or perpendicular orientations inside the polylactic acid (PLA) matrix. Magnetic-field-assisted directional alignment of MGCNCs led to the incorporation of anisotropic mechanical, thermal, and electrical properties in the fabricated PLA-MGCNC nanocomposites. Thermomechanical studies showed significant improvement in the elastic modulus and glass-transition temperature for the magnetically oriented samples. Differential scanning calorimetry (DSC) and XRD studies confirmed that the alignment of MGCNCs led to the improvement in the percentage crystallinity and, with the absence of the cold-crystallization phenomenon, finds a potential application in polymer processing in the presence of magnetic field. The tensile strength and percentage elongation for the parallel-oriented samples improved by ∼70 and 240%, respectively, and for perpendicular-oriented samples, by ∼58 and 172%, respectively, in comparison to the unoriented samples. Furthermore, its anisotropically induced electrical and magnetic properties are desirable for fabricating self-biased electronics products. We also demonstrate that the fabricated anisotropic PLA-MGCNC nanocomposites could be laminated into films with the incorporation of directionally tunable mechanical properties. Therefore, the current study provides a novel noninvasive approach of orienting nontoxic bioderived CNCs in the presence of low

  16. Investigation on by-products of bioenergy systems (anaerobic digestion and gasification) as potential crop nutrient using FTIR, XRD, SEM analysis and phyto-toxicity test.

    PubMed

    Kataki, Sampriti; Hazarika, Samarendra; Baruah, D C

    2017-03-09

    Success and acceptability of the bio energy conversion technology to a large extent depend upon management of the inevitable by-products generated during the conversion process. By-products can be considered favourable as organic fertilizer as they retain nutrients with varying composition depending upon input biomass. However, characteristics of these heterogeneous resources with respect to feedstock and processing conditions have to be assessed to state on their agricultural and environmental benefits. Therefore, 3 types of anaerobic digestion by-products (digestate) from surplus biomass viz. cow dung, Ipomoea carnea:cow dung (60:40 dry weight basis) and rice straw:green gram stover:cow dung (30:30:40 dry weight basis) and one gasification by-product (biochar) from rice husk are considered to understand the fertilizer prospects. Considering 3 potential application options, digestate from each feedstock option was further processed as separated solid, separated liquid and ash from solid digestates. Thus, a total of 10 by-products were investigated for understanding their prospects as fertilizer using Fourier Transform Infrared Spectroscopy (FTIR), X-ray diffraction (XRD), Scanning Electron Microscopy (SEM) and Energy Dispersive X ray Spectroscopy (EDX) and phyto-toxicity test to have a broad insight in terms of their organic, mineral, elemental composition, morphological feature and potential phyto-toxicity. In general, irrespective of origin of feedstock, solid digestate, ash digestate and char showed similarity in terms of composition of functional groups with some degree of variation in relative content as reflected by FTIR analysis. Dominance of organic functional groups in separated solid digestates compared to liquid fraction indicated the former as favourable organic amendments. Quartz was the prevalent mineral phase in all separated solid, ash digestate and rice husk char. Digestates in ash phase represent more concentrated plant nutrient source with

  17. [Comporison Sduty of Microstructure by Metallographicalk on the Polarized Light and Texture by XRD of CC 5083 and CC 5182 Aluminium Alloy after Cold Rolling and Recrystallization].

    PubMed

    Chen, Ming-biao; Li, Yong-wei; Tan, Yuan-biao; Ma, Min; Wang, Xue-min; Liu, Wen-chang

    2015-03-01

    At present the study of relation between microstructure, texture and performance of CC 5083 aluminium alloy after cold tolling and recrystallization processes is still finitude. So that the use of the CC 5083 aluminium alloy be influenced. Be cased into electrical furnace, hot up with unlimited speed followed the furnace hot up to different temperature and annealed 2h respectively, and be cased into salt-beth furnace, hot up quickly to different temperature and annealed 30 min respectively for CC 5083 and CC 5182 aluminum alloy after cold roling with 91.5% reduction. The microstructure be watched use metallographic microscope, the texture be inspected by XRD. The start temperature of recrystallization and grain grow up temperature within annealing in the electric furnace of CC 5083 aluminum alloy board is 343 degrees C, and the shap of grain after grow up with long strip (the innovation point ); The start temperature of recrystallization within annealling in the salt bath furnace of CC 5083 is 343 degrees C. The start temperature and end temperature of recrystallization within annealling of CC 5083 and CC 5182 aluminum alloy is 371 degrees C. The grain grow up outstanding of cold rooled CC 5152 aluminum alloy after annealed with 454 degrees C in the electric furnace and salt bath furnace. The start temperature of grain grow up of CC 5083 alluminurn alloy annealed in the electric furnace and salt bath furnace respectively is higher than the start temperature of grain grow up of CC 5182 alluminum alloy annealed in the electric furnace and salt bath furnace respectively. The strat temperature of recrystallization grain grow up is higher than which annealled with other three manner annealing process. The recrystallization temperature of CC 5182 annealed in the salt bath furnace is higher than which annealed in the electric furnace. The recrystallization temperature of the surface layer of CC 5083 and CC 5182 aluminum alloy is higher than the inner layer (the innovation

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

    NASA Astrophysics Data System (ADS)

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

    2006-12-01

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

  19. The CheMin XRD on the Mars Science Laboratory Rover Curiosity: Construction, Operation, and Quantitative Mineralogical Results from the Surface of Mars

    NASA Technical Reports Server (NTRS)

    Blake, David F.

    2015-01-01

    The Mars Science Laboratory mission was launched from Cape Canaveral, Florida on Nov. 26, 2011 and landed in Gale crater, Mars on Aug. 6, 2012. MSL's mission is to identify and characterize ancient "habitable" environments on Mars. MSL's precision landing system placed the Curiosity rover within 2 km of the center of its 20 X 6 km landing ellipse, next to Gale's central mound, a 5,000 meter high pile of laminated sediment which may contain 1 billion years of Mars history. Curiosity carries with it a full suite of analytical instruments, including the CheMin X-ray diffractometer, the first XRD flown in space. CheMin is essentially a transmission X-ray pinhole camera. A fine-focus Co source and collimator transmits a 50µm beam through a powdered sample held between X-ray transparent plastic windows. The sample holder is shaken by a piezoelectric actuator such that the powder flows like a liquid, each grain passing in random orientation through the beam over time. Forward-diffracted and fluoresced X-ray photons from the sample are detected by an X-ray sensitive Charge Coupled Device (CCD) operated in single photon counting mode. When operated in this way, both the x,y position and the energy of each photon are detected. The resulting energy-selected Co Kalpha Debye-Scherrer pattern is used to determine the identities and amounts of minerals present via Rietveld refinement, and a histogram of all X-ray events constitutes an X-ray fluorescence analysis of the sample.The key role that definitive mineralogy plays in understanding the Martian surface is a consequence of the fact that minerals are thermodynamic phases, having known and specific ranges of temperature, pressure and composition within which they are stable. More than simple compositional analysis, definitive mineralogical analysis can provide information about pressure/temperature conditions of formation, past climate, water activity and the like. Definitive mineralogical analyses are necessary to establish

  20. Phase alignment and crystal orientation of Al 3Ni in Al-Ni alloy by imposition of a uniform high magnetic field

    NASA Astrophysics Data System (ADS)

    Wang, Chunjiang; Wang, Qiang; Wang, Zhongying; Li, Hutian; Nakajima, Keiji; He, Jicheng

    2008-03-01

    Solidification experiments of aluminum-nickel binary alloys under uniform high magnetic fields have been conducted. The effects of high magnetic fields on the crystal orientation of Al 3Ni were investigated by XRD and the alignment of primary phases Al 3Ni were also analyzed. Experimental results showed that the easy magnetization axis of Al 3Ni crystal oriented parallel to the imposed magnetic fields and the primary phase Al 3Ni aligned perpendicular to the magnetic fields. Magnetic orientation of crystal was determined by magnetic anisotropy energy. Whereas the phase alignment should be contributed to the combined effects of magnetic orientation, crystal growth and the effects of magnetic fields on mass transport during solidification.

  1. Magnetic Nanoparticle Sensors

    PubMed Central

    Koh, Isaac; Josephson, Lee

    2009-01-01

    Many types of biosensors employ magnetic nanoparticles (diameter = 5–300 nm) or magnetic particles (diameter = 300–5,000 nm) which have been surface functionalized to recognize specific molecular targets. Here we cover three types of biosensors that employ different biosensing principles, magnetic materials, and instrumentation. The first type consists of magnetic relaxation switch assay-sensors, which are based on the effects magnetic particles exert on water proton relaxation rates. The second type consists of magnetic particle relaxation sensors, which determine the relaxation of the magnetic moment within the magnetic particle. The third type is magnetoresistive sensors, which detect the presence of magnetic particles on the surface of electronic devices that are sensitive to changes in magnetic fields on their surface. Recent improvements in the design of magnetic nanoparticles (and magnetic particles), together with improvements in instrumentation, suggest that magnetic material-based biosensors may become widely used in the future. PMID:22408498

  2. Biomimetic magnetic silk scaffolds.

    PubMed

    Samal, Sangram K; Dash, Mamoni; Shelyakova, Tatiana; Declercq, Heidi A; Uhlarz, Marc; Bañobre-López, Manuel; Dubruel, Peter; Cornelissen, Maria; Herrmannsdörfer, Thomas; Rivas, Jose; Padeletti, Giuseppina; De Smedt, Stefaan; Braeckmans, Kevin; Kaplan, David L; Dediu, V Alek

    2015-03-25

    Magnetic silk fibroin protein (SFP) scaffolds integrating magnetic materials and featuring magnetic gradients were prepared for potential utility in magnetic-field assisted tissue engineering. Magnetic nanoparticles (MNPs) were introduced into SFP scaffolds via dip-coating methods, resulting in magnetic SFP scaffolds with different strengths of magnetization. Magnetic SFP scaffolds showed excellent hyperthermia properties achieving temperature increases up to 8 °C in about 100 s. The scaffolds were not toxic to osteogenic cells and improved cell adhesion and proliferation. These findings suggest that tailored magnetized silk-based biomaterials can be engineered with interesting features for biomaterials and tissue-engineering applications.

  3. Thin Magnetically Soft Wires for Magnetic Microsensors

    PubMed Central

    Zhukova, Valentina; Ipatov, Mihail; Zhukov, Arcady

    2009-01-01

    Recent advances in technology involving magnetic materials require development of novel advanced magnetic materials with improved magnetic and magneto-transport properties and with reduced dimensionality. Therefore magnetic materials with outstanding magnetic characteristics and reduced dimensionality have recently gained much attention. Among these magnetic materials a family of thin wires with reduced geometrical dimensions (of order of 1–30 μm in diameter) have gained importance within the last few years. These thin wires combine excellent soft magnetic properties (with coercivities up to 4 A/m) with attractive magneto-transport properties (Giant Magneto-impedance effect, GMI, Giant Magneto-resistance effect, GMR) and an unusual re-magnetization process in positive magnetostriction compositions exhibiting quite fast domain wall propagation. In this paper we overview the magnetic and magneto-transport properties of these microwires that make them suitable for microsensor applications. PMID:22291562

  4. Superconducting magnet

    DOEpatents

    Satti, John A.

    1980-01-01

    A superconducting magnet designed to produce magnetic flux densities of the order of 4 to 5 Webers per square meter is constructed by first forming a cable of a plurality of matrixed superconductor wires with each wire of the plurality insulated from each other one. The cable is shaped into a rectangular cross-section and is wound with tape in an open spiral to create cooling channels. Coils are wound in a calculated pattern in saddle shapes to produce desired fields, such as dipoles, quadrupoles, and the like. Wedges are inserted between adjacent cables as needed to maintain substantially radial placement of the long dimensions of cross sections of the cables. After winding, individual strands in each of the cables are brought out to terminals and are interconnected to place all of the strands in series and to maximize the propagation of a quench by alternating conduction from an inner layer to an outer layer and from top half to bottom half as often as possible. Individual layers are separated from others by spiraled aluminum spacers to facilitate cooling. The wound coil is wrapped with an epoxy tape that is cured by heat and then machined to an interference fit with an outer aluminum pipe which is then affixed securely to the assembled coil by heating it to make a shrink fit. In an alternate embodiment, one wire of the cable is made of copper or the like to be heated externally to propagate a quench.

  5. Magnetic Storms

    NASA Technical Reports Server (NTRS)

    Tsurutani, Bruce T.; Gonzalez, Walter D.

    1998-01-01

    One of the oldest mysteries in geomagnetism is the linkage between solar and geomagnetic activity. The 11-year cycles of both the numbers of sunspots and Earth geomagnetic storms were first noted by Sabine. A few years later, speculation on a causal relationship between flares and storms arose when Carrington reported that a large magnetic storm followed the great September 1859 solar flare. However, it was not until this century that a well-accepted statistical survey on large solar flares and geomagnetic storms was performed, and a significant correlation between flares and geomagnetic storms was noted. Although the two phenomena, one on the Sun and the other on the Earth, were statistically correlated, the exact physical linkage was still an unknown at this time. Various hypotheses were proposed, but it was not until interplanetary spacecraft measurements were available that a high-speed plasma stream rich in helium was associated with an intense solar flare. The velocity of the solar wind increased just prior to and during the helium passage, identifying the solar ejecta for the first time. Space plasma measurements and Skylab's coronagraph images of coronal mass elections (CMES) from the Sun firmly established the plasma link between the Sun and the Earth. One phenomenon associated with magnetic storms is brilliant "blood" red auroras, as shown.

  6. The magnetization process: Hysteresis

    NASA Technical Reports Server (NTRS)

    Balsamel, Richard

    1990-01-01

    The magnetization process, hysteresis (the difference in the path of magnetization for an increasing and decreasing magnetic field), hysteresis loops, and hard magnetic materials are discussed. The fabrication of classroom projects for demonstrating hysteresis and the hysteresis of common magnetic materials is described in detail.

  7. Magnet innovations for linacs

    SciTech Connect

    Halbach, K.

    1986-06-01

    It is possible to produce large magnetic fields at the aperture of permanent magnet quadrupoles, even when the magnetic aperture is very small. That, combined with their compactness, makes permanent magnet quadrupoles very powerful components of small aperture linacs. Results will be presented about past and present work on both fixed and variable strength permanent magnets suitable for use in and around linacs.

  8. Permanent magnet assembly

    DOEpatents

    Chell, Jeremy; Zimm, Carl B.

    2006-12-12

    A permanent magnet assembly is disclosed that is adapted to provide a magnetic field across an arc-shaped gap. Such a permanent magnet assembly can be used, for example, to provide a time-varying magnetic field to an annular region for use in a magnetic refrigerator.

  9. Vertical Si nanowire arrays fabricated by magnetically guided metal-assisted chemical etching

    NASA Astrophysics Data System (ADS)

    Chun, Dong Won; Kim, Tae Kyoung; Choi, Duyoung; Caldwell, Elizabeth; Kim, Young Jin; Paik, Jae Cheol; Jin, Sungho; Chen, Renkun

    2016-11-01

    In this work, vertically aligned Si nanowire arrays were fabricated by magnetically guided metal-assisted directional chemical etching. Using an anodized aluminum oxide template as a shadow mask, nanoscale Ni dot arrays were fabricated on an Si wafer to serve as a mask to protect the Si during the etching. For the magnetically guided chemical etching, we deposited a tri-layer metal catalyst (Au/Fe/Au) in a Swiss-cheese configuration and etched the sample under the magnetic field to improve the directionality of the Si nanowire etching and increase the etching rate along the vertical direction. After the etching, the nanowires were dried with minimal surface-tension-induced aggregation by utilizing a supercritical CO2 drying procedure. High-resolution transmission electron microscopy (HR-TEM) analysis confirmed the formation of single-crystal Si nanowires. The method developed here for producing vertically aligned Si nanowire arrays could find a wide range of applications in electrochemical and electronic devices.

  10. Vertical Si nanowire arrays fabricated by magnetically guided metal-assisted chemical etching.

    PubMed

    Chun, Dong Won; Kim, Tae Kyoung; Choi, Duyoung; Caldwell, Elizabeth; Kim, Young Jin; Paik, Jae Cheol; Jin, Sungho; Chen, Renkun

    2016-11-11

    In this work, vertically aligned Si nanowire arrays were fabricated by magnetically guided metal-assisted directional chemical etching. Using an anodized aluminum oxide template as a shadow mask, nanoscale Ni dot arrays were fabricated on an Si wafer to serve as a mask to protect the Si during the etching. For the magnetically guided chemical etching, we deposited a tri-layer metal catalyst (Au/Fe/Au) in a Swiss-cheese configuration and etched the sample under the magnetic field to improve the directionality of the Si nanowire etching and increase the etching rate along the vertical direction. After the etching, the nanowires were dried with minimal surface-tension-induced aggregation by utilizing a supercritical CO2 drying procedure. High-resolution transmission electron microscopy (HR-TEM) analysis confirmed the formation of single-crystal Si nanowires. The method developed here for producing vertically aligned Si nanowire arrays could find a wide range of applications in electrochemical and electronic devices.

  11. A silicon dioxide modified magnetic nanoparticles-labeled lateral flow strips for HBs antigen.

    PubMed

    Zhang, Xueqing; Jiang, Lin; Zhang, Chunlei; Li, Ding; Wang, Can; Gao, Feng; Cui, Daxiang

    2011-12-01

    Herein we reported a new type of silicon dioxide wrapped magnetic nanoparticles-labeled lateral flow strip for detection of HBs antigen in sera. The SiO2 wrapped Fe3O4 nanocomposites were prepared and characterized by HR-TEM, FTIR and magnetometer. As-prepared nanocomposites were used to label anti-HBV surface monoclonal antibody, the lateral flow strips were constructed, and 100 specimens of sera were collected and tested. Results showed that the prepared SiO2 wrapped Fe3O4 nanocomposites were shell/core structure, well dispersed, with the size of 25 nm in diameter, the thickness of the shell was about 3 nm, their magnetic saturation intensity was 44.3 meu g(-1). Clinical sera specimens test results showed that the prepared lateral flow strips were with the detection limitation of 5 pg/mL by naked eye observation, and 0.1 pg/mL by CCD reader or MAR Analyzer, specificity was 100%. In conclusion, one kind of silicon dioxide wrapped magnetic nanoparticles-labeled lateral flow strip for ultrasensitive detection of HBs antigen was successfully developed, its ease of use, sensitiveness and low-cost make it well-suited for population-based on-the-site hepatitis B screening.

  12. Radiolabeled D-Penicillamine Magnetic Nanocarriers for Targeted Purposes.

    PubMed

    Özyüncü, Seniha Yolcular; Teksöz, Serap; Içhedef, Çiğdem; Medinel, E Ilker; Avci, Çiğir Biray; Gündüz, Cumhur; Ünak, Perihan

    2016-04-01

    The aim of this study is to synthesize D-Penicillamine (D-PA) conjugated magnetic nanocarriers for targeted purposes. Magnetic nanoparticles were prepared by partial reduction method and surface modification was done with an amino silane coupling agent's (structural properties), AEAPS, the particles were characterized by Scanning Electron Microscope (SEM), X-ray Diffraction (XRD). After that D-PA was linked with the magnetic nanoparticles (MNPs) and has been radiolabeled with [99mTc(CO)3]+ core. Quality controls of [99mTc(CO)3-MNP-D-PA] were established by Cd(Te) detector. The radiolabeling efficiency of magnetic nanoparticles ([99mTc(CO)3-MNP-D-PA]) was about 97.05% with good in vitro stability during the 24 hour period. As a parallel study, radiolabeled D-PA complex ([99mTc(CO)3-D-PA]) was prepared with a radiolabeling yield of 97.93%. At the end, biologic activities of binding complexes were investigated on MCF7 human breast cancer cells. Our results show that, radiolabeled magnetic nanoparticles with core [99mTc(CO)3]+ ([99mTc(CO)3-MNP-D-PA]) showed the highest uptake on MCF7 cells which were applied magnetic field in the wells. In that case, result of this study emphasizes that radiolabeled magnetic nanoparticles with core [99mTc(CO)3]+ would support new occurrences of new agents.

  13. Magnetoresponsive conductive colloidal suspensions with magnetized carbon nanotubes

    NASA Astrophysics Data System (ADS)

    Abdalla, Ahmed M.; Abdel Fattah, Abdel Rahman; Ghosh, Suvojit; Puri, Ishwar K.

    2017-01-01

    We synthesize a novel and hitherto unreported class of colloidal suspensions for which the dispersed phase, which consists of multiwall carbon nanotubes (MWNTs) decorated with magnetic nanoparticles (MNPs), is both magnetoresponsive and electrically conductive. Synthesis of the dispersed phase merges processes for producing ferrofluids and magnetic MWNTs (mMWNTs). We explore means to tune the properties of these magnetic conductive colloids (MCCs) by varying the (1) MNP material composition, and (2) MNP:MWNT (w/w) magnetization weight ratio (γ). The mMWNTs are examined using XRD, TEM, EDX and SQUID and MCCs are by measuring their zeta potential and electric conductivity. Magnetite (Fe3O4) MNPs, which possess a high Curie temperature, produce mMWNTs with high saturation magnetization that respond relatively weakly to temperature variations. Mn0.2Cu0.2Zn0.6Fe2O4 and Cu0.4Zn0.6Fe2O4 MNPs with lower Curie temperatures are more sensitive to changing temperature. Increasing the MNP Cu content improves the electric conductivity of the corresponding MCC while increasing γ enhances its magnetic response. After γ is raised above a threshold value, mMWNT decoration on the CNT surface becomes nonuniform since the MNPs now agglomerate perpendicular to the nanotube surface. These colloidal suspensions are a promising new class of material that can be manipulated with a magnetic field to tune their electrical conductivity.

  14. Structural reinvestigation of Li3FeN2: Evidence of cationic disorder through XRD, solid-state NMR and Mössbauer spectroscopy

    NASA Astrophysics Data System (ADS)

    Panabière, E.; Emery, N.; Lorthioir, C.; Sougrati, M. T.; Jumas, J.-C.; Bach, S.; Pereira-Ramos, J.-P.; Smith, R. I.; Willmann, P.

    2016-08-01

    A significant cationic disorder is evidenced on Li3FeN2 prepared through solid-state reaction under controlled atmosphere. This derivative anti fluorite type structure (orthorhombic, space group Ibam, a=4.870(1) Å, b=9.652(1) Å and c=4.789(1) Å), solved first through single crystal X-ray diffraction [7], is usually described by Li+ and Fe+3 ordered distribution in tetrahedral sites formed by the nitrogen network, leading to [FeN4/2]3- edge-sharing tetrahedral chains. From 7Li/6Li Nuclear Magnetic Resonance spectroscopy, 57Fe Mössbauer spectroscopy and powder X-ray and neutron diffraction, we demonstrate that about 4% of lithium sites are filled by iron and about 11% of iron sites are occupied by Li, which can explain the discrepancy within the Gudat's model observed on larger scale solid-state synthesis samples.

  15. Infrared spectroscopy as a tool to characterise starch ordered structure--a joint FTIR-ATR, NMR, XRD and DSC study.

    PubMed

    Warren, Frederick J; Gidley, Michael J; Flanagan, Bernadine M

    2016-03-30

    Starch has a heterogeneous, semi-crystalline granular structure and the degree of ordered structure can affect its behaviour in foods and bioplastics. A range of methodologies are employed to study starch structure; differential scanning calorimetry, (13)C nuclear magnetic resonance, X-ray diffraction and Fourier transform infrared spectroscopy (FTIR). Despite the appeal of FTIR as a rapid, non-destructive methodology, there is currently no systematically defined quantitative relationship between FTIR spectral features and other starch structural measures. Here, we subject 61 starch samples to structural analysis, and systematically correlate FTIR spectra with other measures of starch structure. A hydration dependent peak position shift in the FTIR spectra of starch is observed, resulting from increased molecular order, but with complex, non-linear behaviour. We demonstrate that FTIR is a tool that can quantitatively probe short range interactions in starch structure. However, the assumptions of linear relationships between starch ordered structure and peak ratios are overly simplistic.

  16. Gas-phase synthesis of magnetic metal/polymer nanocomposites.

    PubMed

    Starsich, Fabian H L; Hirt, Ann M; Stark, Wendelin J; Grass, Robert N

    2014-12-19

    Highly magnetic metal Co nanoparticles were produced via reducing flame spray pyrolysis, and directly coated with an epoxy polymer in flight. The polymer content in the samples varied between 14 and 56 wt% of nominal content. A homogenous dispersion of Co nanoparticles in the resulting nanocomposites was visualized by electron microscopy. The size and crystallinity of the metallic fillers was not affected by the polymer, as shown by XRD and magnetic hysteresis measurements. The good control of the polymer content in the product nanocomposite was shown by elemental analysis. Further, the successful polymerization in the gas phase was demonstrated by electron microscopy and size measurements. The presented effective, dry and scalable one-step synthesis method for highly magnetic metal nanoparticle/polymer composites presented here may drastically decrease production costs and increase industrial yields.

  17. Gas-phase synthesis of magnetic metal/polymer nanocomposites

    NASA Astrophysics Data System (ADS)

    Starsich, Fabian H. L.; Hirt, Ann M.; Stark, Wendelin J.; Grass, Robert N.

    2014-12-01

    Highly magnetic metal Co nanoparticles were produced via reducing flame spray pyrolysis, and directly coated with an epoxy polymer in flight. The polymer content in the samples varied between 14 and 56 wt% of nominal content. A homogenous dispersion of Co nanoparticles in the resulting nanocomposites was visualized by electron microscopy. The size and crystallinity of the metallic fillers was not affected by the polymer, as shown by XRD and magnetic hysteresis measurements. The good control of the polymer content in the product nanocomposite was shown by elemental analysis. Further, the successful polymerization in the gas phase was demonstrated by electron microscopy and size measurements. The presented effective, dry and scalable one-step synthesis method for highly magnetic metal nanoparticle/polymer composites presented here may drastically decrease production costs and increase industrial yields.

  18. CONDENSED MATTER: ELECTRONIC STRUCTURE, ELECTRICAL, MAGNETIC, AND OPTICAL PROPERTIES: Effect of Temperature on Structural and Magnetic Properties of Laser Ablated Iron Oxide Deposited on Si(100)

    NASA Astrophysics Data System (ADS)

    Shahid, Ramay M.; Saadat, Siddiqi A.; M. Sabieh, Anwar; Shin C., S.

    2009-11-01

    We fabricate Fe3O4 thin films on Si(100) substrates at different temperatures using pulsed laser deposition, and study the effect of annealing and deposition temperature on the structural and magnetic properties of Fe3O4 thin films. Subsequently, the films are characterized by x-ray diffraction (XRD), scanning electron microscopy (SEM) and vibrating sample magnetometery (VSM). The XRD results of these films confirm the presence of the Fe3O4 phase and show room-temperature ferromagnetism, as observed with VSM. We demonstrate the optimized deposition and annealing conditions for an enhanced magnetization of 854 emu/cm3 that is very high when compared to the bulk sample.

  19. Effect of magnetic anisotropy and particle size distribution on temperature dependent magnetic hyperthermia in Fe3O4 ferrofluids

    NASA Astrophysics Data System (ADS)

    Palihawadana Arachchige, Maheshika; Nemala, Humeshkar; Naik, Vaman; Naik, Ratna

    Magnetic hyperthermia (MHT) has a great potential as a non-invasive cancer therapy technique. Specific absorption rate (SAR) which measures the efficiency of heat generation, mainly depends on magnetic properties of nanoparticles such as saturation magnetization (Ms) and magnetic anisotropy (K) which depend on the size and shape. Therefore, MHT applications of magnetic nanoparticles often require a controllable synthesis to achieve desirable magnetic properties. We have synthesized Fe3O4 nanoparticles using two different methods, co-precipitation (CP) and hydrothermal (HT) techniques to produce similar XRD crystallite size of 12 nm, and subsequently coated with dextran to prepare ferrofluids for MHT. However, TEM measurements show average particle sizes of 13.8 +/-3.6 nm and 14.6 +/-3.6 nm for HT and CP samples, implying the existence of an amorphous surface layer for both. The MHT data show the two samples have very different SAR values of 110 W/g (CP) and 40W/g (HT) at room temperature, although they have similar Ms of 70 +/-4 emu/g regardless of their different TEM sizes. We fitted the temperature dependent SAR using linear response theory to explain the observed results. CP sample shows a larger magnetic core with a narrow size distribution and a higher K value compared to that of HT sample.

  20. Structural and magnetic properties of turmeric functionalized CoFe2O4 nanocomposite powder

    NASA Astrophysics Data System (ADS)

    Mehran, E.; Farjami Shayesteh, S.; Sheykhan, M.

    2016-10-01

    The structural and magnetic properties of the synthesized pure and functionalized CoFe2O4 magnetic nanoparticles (NPs) are studied by analyzing the results from the x-ray diffraction (XRD), transmission electron microscopy (TEM), FT-IR spectroscopy, thermogravimetry (TG), and vibrating sample magnetometer (VSM). To extract the structure and lattice parameters from the XRD analysis results, we first apply the pseudo-Voigt model function to the experimental data obtained from XRD analysis and then the Rietveld algorithm is used in order to optimize the model function to estimate the true intensity values. Our simulated intensities are in good agreement with the experimental peaks, therefore, all structural parameters such as crystallite size and lattice constant are achieved through this simulation. Magnetic analysis reveals that the synthesized functionalized NPs have a saturation magnetization almost equal to that of pure nanoparticles (PNPs). It is also found that the presence of the turmeric causes a small reduction in coercivity of the functionalized NPs in comparison with PNP. Our TGA and FTIR results show that the turmeric is bonded very well to the surface of the NPs. So it can be inferred that a nancomposite (NC) powder of turmeric and nanoparticles is produced. As an application, the anti-arsenic characteristic of turmeric makes the synthesized functionalized NPs or NC powder a good candidate for arsenic removal from polluted industrial waste water. Project supported by the University of Guilan and the Iran Nanotechnology Initiative Council.

  1. γ-Fe2O3 magnetic nanoparticle functionalized with carboxylated multi walled carbon nanotube: Synthesis, characterization, analytical and biomedical application

    NASA Astrophysics Data System (ADS)

    Kılınç, Ersin

    2016-03-01

    In recent years, magnetic nanoparticles attained special interest in nanobiotechnology and nanomedicine due to their uniqe properties and biocompatibilities. From this perspective, hybride nanostructure composed from γ-Fe2O3 magnetic nanoparticle and carboxylated multi walled carbon nanotube was synthesized and characterized by FT-IR, VSM, SEM, HR-TEM and ICP-OES. Microscopy images showed that magnetic nanoparticles were nearly spherical structure that arranged on the axis of carboxylated MWCNT. Particle size was found lower than 10 nm. VSM results showed that the obtained magnetic nanoparticles presented superparamagnetic properties at room temperature. The magnetic saturation value was determined as 35.2 emu/g. It was used for the adsorption and controlled release of harmane, a potent tremor-producing neurotoxin. Maximum adsorption capacity was calculated as 151.5 mg/g from Langmuir isotherm. Concentration of harmane was determined by HPLC with fluorescence detection. The antimicrobial activity of synthesized magnetic nanoparticle was investigated against gram-negative and gram-positive bacteria. However, no activity was observed.

  2. Samarium/Cobalt Magnets

    NASA Technical Reports Server (NTRS)

    Das, D.; Kumar, K.; Frost, R.; Chang, C.

    1985-01-01

    Intrinsic magnetic coercivities of samarium cobalt magnets made to approach theoretical limit of 350 kA/m by carefully eliminating oxygen from finished magnet by hot isostatic pressing (HIP). HIP process viable alternative to currently used sintering process.

  3. Intraocular magnet of Parel.

    PubMed Central

    Crock, G. W.; Janakiraman, P.; Reddy, P.

    1986-01-01

    The intraocular magnet (IOM) is a new device based on permanent magnetism providing controlled energy for removal of magnetic intraocular foreign bodies. Its use is reported in 11 cases. Images PMID:3801364

  4. Magnetism of Carbonados

    NASA Technical Reports Server (NTRS)

    Kletetschka, G.; Taylor, P. T.; Wasilewski, P. J.

    2000-01-01

    Origin of Carbonado is not clear. Magnetism of Carbonado comes from the surface, indicating contemporary formation of both the surface and magnetic carriers. The interior of carbonado is relatively free of magnetic phases.

  5. MRI (Magnetic Resonance Imaging)

    MedlinePlus

    ... and Procedures Medical Imaging MRI (Magnetic Resonance Imaging) MRI (Magnetic Resonance Imaging) Share Tweet Linkedin Pin it More sharing options ... usually given through an IV in the arm. MRI Research Programs at FDA Magnetic Resonance Imaging (MRI) ...

  6. Smashing magnets

    NASA Astrophysics Data System (ADS)

    Ferrier-Barbut, Igor

    2016-11-01

    Understanding or designing phases of matter relies in the first place on the knowledge at the microscopic level of the interactions taking place between the constituents. In quantum gases, a renewed interest is rising about the interaction between two dipoles, owing to its anisotropic and long-range character. In a new paper, Burdick et al (2016 New J. Phys. 18 113004) demonstrate experimentally the angular-dependence of collisions between two dysprosium atoms, an atomic species that carries a magnetic dipole moment among the largest in the periodic table. This is realized by colliding two 164Dy Bose-Einstein condensates, and the experiments are backed by a theoretical analysis to connect these results with the two-body scattering cross-section. This represents a further step on the way to the full control of dipole-interacting many-body systems.

  7. Magnetized accretion

    NASA Astrophysics Data System (ADS)

    Heyvaerts, J.

    This lecture reviews in simple terms the general subject of large scale magnetic field coupling to plasma flows in the vicinity of accreting compact stars. The relevant astrophysical phenomenology is summarized. Disk interaction with the magnetosphere of accreting stars is first discussed, in particular the structure of the magnetopause, its stability and plasma ejection in so-called propeller systems. The physics of accretion/ejection is then considered. Acceleration and focusing mechanisms of jets from accretion disks around compact stars or black holes and the question of the self-consistency of accretion and ejection are described. By contrast, small scale MHD turbulence in disks is not discussed, neither are accretion columns near the polar caps of neutron stars or white dwarfs. The reader is only assumed to have some basic knowledge of astrophysics and of fluid mechanics and electromagnetism.

  8. Magnetic particles

    NASA Technical Reports Server (NTRS)

    Chang, Manchium (Inventor); Colvin, Michael S. (Inventor); Rembaum, Alan (Inventor); Richards, Gil F. (Inventor)

    1987-01-01

    Metal oxide containing polymers and particularly styrene, acrylic or protein polymers containing fine, magnetic iron oxide particles are formed by combining a NO.sub.2 -substituted polymer with an acid such as hydrochloric acid in the presence of metal, particularly iron particles. The iron is oxidized to fine, black Fe.sub.3 O.sub.4 particles which deposit selectively on the polymer particles. Nitrated polymers are formed by reacting functionally substituted, nitrated organic compounds such as trinitrobenzene sulfonate or dinitrofluoro benzene with a functionally coreactive polymer such as an amine modified acrylic polymer or a protein. Other transition metals such as cobalt can also be incorporated into polymers using this method.

  9. Magnetization of ferromagnetic clusters

    SciTech Connect

    Onishi, Naoki; Bertsch, G.; Yabana, Kazuhiro

    1995-02-01

    The magnetization and deflection profiles of magnetic clusters in a Stern-Gerlach magnet are calculated for conditions under which the magnetic moment is fixed in the intrinsic frame of the cluster, and the clusters enter the magnetic field adiabatically. The predicted magnetization is monotonic in the Langevin parameter, the ratio of magnetic energy {mu}{sub 0}B to thermal energy k{sub B}T. In low field the average magnetization is 2/3 of the Langevin function. The high-field moment approaches saturation asymptotically as B{sup {minus}1/2} instead of the B{sup {minus}1} dependence in the Langevin function.

  10. The Third Flight Magnet

    NASA Technical Reports Server (NTRS)

    McGhee, R. Wayne

    1998-01-01

    A self-shielded superconducting magnet was designed for the NASA Goddard Space Flight Center Adiabatic Demagnetization Refrigerator Program. This is the third magnet built from this design. The magnets utilize Cryomagnetics' patented ultra-low current technology. The magnetic system is capable of reaching a central field of two tesla at slightly under two amperes and has a total inductance of 1068 henries. This final report details the requirements of the magnet, the specifications of the resulting magnet, the test procedures and test result data for the third magnet (Serial # C-654-M), and recommended precautions for use of the magnet.

  11. Magnetic interactions in cubic iron oxide magnetic nanoparticle bound to zeolite

    NASA Astrophysics Data System (ADS)

    Singh, L. Herojit; Pati, Sudhanshu S.; Coaquira, J. A. H.; Matilla, John; Guimarães, Edi M.; Oliveira, A. C.; Kuzmann, E.; Garg, Vijayendra K.

    2016-10-01

    Magnetic interaction of the magnetite (Fe3O4) nanoparticles grown on zeolite has been studied. XRD patterns show that in the presence of 25-75 mg of zeolite the average particle size of Fe3O4 decreases to ≈6 nm, but with the increase of zeolite content (75 mgmagnetization decreases from 63 to 53 emu/g. Mössbauer studies show the presence of different Fe3O4 microenvironments, possibly in pores and on the surface of zeolite. Transformation of the superparamagnetic doublet to sextet at 80 K can indicate a variation in the magnetic interaction. At low temperature the interaction between Fe3O4 at the pore and at the surface enhances the magnetic ordering. The nanoparticles in the pores of zeolite are connected with the surface particles in low zeolite content and get isolated as the amount of zeolite increases.

  12. The effects of synthesis conditions on the magnetic properties of zinc ferrite spinel nanoparticles

    NASA Astrophysics Data System (ADS)

    El Maalam, K.; Fkhar, L.; Mahhouti, Z.; Mounkachi, O.; AitAli, M.; Hamedoun, M.; Benyoussef, A.

    2016-10-01

    Zinc ferrite nanocrystals were synthesized from metal chloride precursors via chemical co-precipitation method, using different synthesis conditions. Characterization measurements including X-ray diffraction (XRD), transmission electron microscopy (TEM) and super conductiong quantum device (SQUID) were used to study the influence of precursor's concentration and reaction time on the crystalline structure, average sizes and magnetic properties of zinc ferrite nanoparticles. The transmission images show spherical, homogenous shape and particle size ranging from 16 to 22 nm. DC magnetization (2-300 K) measurements reveal a superparamagnetic behavior for the ZnFe2O4 samples with a blocking temperature in the range of 18-24 K. Our results demonstrate that magnetic properties of magnetic particles can be largely modified by just changing the reaction condition such as concentration and reaction time, which might be a useful way to design novel magnetic materials.

  13. Innovative methodology for recovering titanium and chromium from a raw ilmenite concentrate by magnetic separation after modifying magnetic properties.

    PubMed

    Lv, Jin-Fang; Zhang, Han-Ping; Tong, Xiong; Fan, Chun-Lin; Yang, Wen-Tao; Zheng, Yong-Xing

    2017-03-05

    Raw ilmenite concentrate containing Cr can be either as a resource or as one kind of the most hazardous solid waste. In order to recover titanium and chromium from the raw concentrate which was separated from the Promenade deposit, Gaza province, Mozambique, an innovative technology using modification of magnetic property followed by magnetic separation was proposed. Magnetic property, phase and surface morphology of the sample before and after oxidizing roasting were firstly characterized by magnetism, chemistry, XRD and MLA analyses to interpret the mechanism of oxidizing roasting of the ilmenite. Then, these factors such as oxidizing roasting temperature, residence time and magnetic induction affecting on magnetic separation performance were examined and the optimum process parameters were determined. A commercial concentrate containing 47.94% TiO2 and 0.23% Cr2O3 was obtained and the recovery of TiO2 and Cr2O3 was 78.52% and 5.42%, respectively. The tailing obtained was preliminarily concentrated by a high-intensity magnetic separator and a rough chromite concentrate was gained. In order to further purify the rough one, reducing roasting was carried out to transform the minerals containing hematite into the minerals containing magnetite, followed by a low-intensity magnetic separation. The effects of these parameters such as temperature, carbon powder dosage, holding time and magnetic induction on magnetic separation performance were investigated and the optimal conditions were determined. A concentrate containing 28.65% Cr2O3 was obtained and the total recovery of Cr2O3 was 84.18%.

  14. Magnetic hyperthermia in solid magnetic colloids

    NASA Astrophysics Data System (ADS)

    Zubarev, A. Yu.; Iskakova, L. Yu.; Abu-Bakr, A. F.

    2017-02-01

    We present results of theoretical study of magnetic hyperthermia in systems of single-domain ferromagnetic particles homogeneously distributed in a solid matrix. The heat effect is induced by linearly polarized alternating magnetic field. The effect of magnetic interaction between the particles as well as influence of orientation of the particles magnetic axes are in a focus of our consideration. Analysis shows that the interparticle interaction increases intensity of the heat production. The thermal effect in the systems with parallel orientation of the particles axes of easy magnetization is significantly higher than that in the case of random orientation of these axes.

  15. Iron Nanoparticles Fabricated by High-Energy Ball Milling for Magnetic Hyperthermia

    NASA Astrophysics Data System (ADS)

    Tung, D. K.; Manh, D. H.; Phong, L. T. H.; Nam, P. H.; Nam, D. N. H.; Anh, N. T. N.; Nong, H. T. T.; Phan, M. H.; Phuc, N. X.

    2016-05-01

    Iron nanoparticles (FeNPs) have been successfully prepared by high-energy ball milling in air for various milling times from 1 h to 32 h. Their structure, particle size, elemental composition, magnetic, and inductive heating properties were investigated by means of x-ray diffraction (XRD) analysis, field-emission scanning electron microscopy, energy-dispersive x-ray (EDX) spectroscopy, vibrating-sample magnetometry, and magnetic induction heating, respectively. XRD analysis showed that the average crystallite size decreased to 11 nm after 10 h of milling, then remained almost unchanged for longer milling times. Coexistence of iron (Fe) and iron oxide (FeO) phases was detected after 12 h of milling. EDX analysis also confirmed the occurrence of oxidation, which can be reconciled with the corresponding decrease and increase in saturation magnetization ( M s) with milling time when exposed to oxygen and when annealed under H2 ambient due to oxygen reduction. The time-dependent magnetic and inductive heating responses of the FeNPs were investigated for prospective application in magnetic hyperthermia. The effect of varying the alternating-current (AC) magnetic field strength on the saturation heating temperature and specific loss power of FeNP-containing ferrofluid with concentration of 4 mg/mL was also studied and is discussed.

  16. The structural and magnetic properties of Sr-doped multiferroic CaMn7O12

    NASA Astrophysics Data System (ADS)

    Zhang, Hong-Guang; Ma, Xiao-Chen; Xie, Liang

    2015-10-01

    The structural and magnetic properties of Sr-doped multiferroic CaMn7O12 were investigated by X-ray diffraction (XRD), Raman spectra, X-ray absorption spectroscopy and temperature dependence of magnetization. The XRD indicates that the samples are rhombohedral lattice (space group R3¯) with small additional phase Mn3O4. The refined lattice parameters of the main phase increases by the Sr doping. The Raman spectra demonstrate the phonon vibration direction is affected, which is probably due to the rotation of MnO6 octahedral. However, as the valence state of Sr and Ca is same at +2, the samples with doping show nonvariation of peak position at Mn 2p X-ray absorption spectra, indicating that the ratio of Mn3+ and Mn4+ ions is unchanged. And the magnetic transition temperature both at T1 = 90K and T2 = 42K is also not tunable because the amount of magnetic interaction between Mn3+ and Mn4+ is not influenced by doping Sr ion. Only the enhancement of the magnetization at low temperature is observed, which is the same as the effect caused by external magnetic fields. An unsaturated wasp-waist type hysteresis loop is observed, indicating the competition between ferromagnetic-like and antiferromagnetic order.

  17. Comparative investigation of CuFe2O4 nano and microstructures for structural, morphological, optical and magnetic properties

    NASA Astrophysics Data System (ADS)

    Raja, G.; Gopinath, S.; Raj, R. Azhagu; Shukla, Arun K.; Alhoshan, Mansour S.; Sivakumar, K.

    2016-09-01

    CuFe2O4 nanocrystals were synthesized by the sol-gel method (SGM) and microwave method (MM) by using sucrose as a fuel. The structural, morphological, optical and magnetic properties of the products were determined and characterized in detail by X-ray diffraction (XRD), high resolution scanning electron microscopy (HR-SEM), photoluminescence (PL) spectroscopy and vibrating sample magnetometer (VSM). The XRD results confirmed the formation of cubic phase CuFe2O4. The formation of CuFe2O4 nano and microstructures were confirmed by HR-SEM. Photoluminescence emissions were determined by PL spectra, respectively. The relatively high saturation magnetization (78.22 emu/g) of CuFe2O4-MM shows that it is ferromagnetic and low saturation magnetization (35.98 emu/g) of CuFe2O4O-SGM confirms the super paramagnetic behavior.

  18. Hoosier Magnetics

    SciTech Connect

    None, None

    2015-09-30

    Hoosier Magnetics proposes to replace the indirect clinker water cooling system with a cooling system that recycles heat from the hot ferrite to preheat the combustion air. This innovative process would significantly reduce the amount of natural gas required to heat the combustion air while eliminating Hoosier’s largest source of downtime. According to the Department of Energy’s Industrial Technologies Program for Energy Efficiency and Renewable Energy, process temperature is customarily used as a rough indication of where preheating air will be cost effective. Previous studies have concluded that processes operating above 1,600° F are ideal candidates for the utilization of pre-heated combustion air. Hoosier Magnetics’ operating temperatures run between 1800-2200° F making Hoosier the perfect candidate. Using preheated air at 1200° F will result in 35% fuel savings, or $298,935 annually. Additionally, the new system would have improved process reliability and result in both production efficiency increases and cost savings. This technology is NOT practiced or utilized on a wide-spread basis but could have a significant energy reduction impact in many different high heat utilizing industries in the country. While the energy savings is apparent with this theory the application and design of such a process has not been studied.

  19. MAGNETIC DENSITOMETER

    DOEpatents

    McCann, J.A.; Jones, R.H.

    1961-08-15

    A magnetic densitometer for locating defects and metallic inclusions in materials is described. The apparatus consists of two primary coils connected in series opposition and adapted te be placed in inductive relation to the material under test, a source of constant frequency alternating current coupled across the primary coil combination, a pick-up coil disposed in symmetrical inductive relationship with said primary coils, a phase-shifter coupled to the output of the energizing source. The output of the phase-shifter is coupled in series with the pick-up coil. An amplifier is provided selective to the third harmonic of the energizing source frequency. The series combination of the pick-up coil and the phase-shifter output are connected across the input of the amplifier, and an amplitude comparitor is coupled to the output of the amplifier and the energizing source for comparing the instantaneous amplitude of the amplifier output and the instantaneous output of the energizing source and producing an output proportional to the difference in amplitude. A recorder is coupled to the output of the amplitude comparison means to give an indication of the amplitude difference, thereby providing a permanent presentation of the character of the changes in characteristics exhibited by the material under test. (AEC)

  20. One-step synthesis of magnetic chitosan polymer composite films

    NASA Astrophysics Data System (ADS)

    Cesano, Federico; Fenoglio, Gaia; Carlos, Luciano; Nisticò, Roberto

    2015-08-01

    In this study, a magnetic iron oxide-chitosan composite film is synthesized by one-step method and thoroughly investigated in order to better understand its inorganic/organic properties. A deep physico-chemical characterization of the magnetic films has been performed. In particular, the material composition was evaluated by means of XRD and ATR-FTIR spectroscopy, whereas the thermal stability and the subsequent inorganic phase transitions involving iron oxide species were followed by TGA analyses carried out at different experimental conditions (i.e. inert and oxidative atmosphere). The magnetic properties of the films were tested at the bulk and at the surface level, performing respectively magnetization hysteresis curve and magnetic force microscopy (MFM) surface mapping. Results indicate that the synthesized material can be prepared through a very simple synthetic procedure and suggests that it can be successfully applied for instance to environmental applications, such as the adsorption of contaminants from solid and liquid media thanks to its pronounced magnetic properties, which favour its recover.

  1. Induced magnetic anisotropy in Si-free nanocrystalline soft magnetic materials: A transmission x-ray diffraction study

    SciTech Connect

    Parsons, R. Suzuki, K.; Yanai, T.; Kishimoto, H.; Kato, A.; Ohnuma, M.

    2015-05-07

    In order to better understand the origin of field-induced anisotropy (K{sub u}) in Si-free nanocrystalline soft magnetic alloys, the lattice spacing of the bcc-Fe phase in nanocrystalline Fe{sub 94−x}Nb{sub 6}B{sub x} (x = 10, 12, 14) alloys annealed under an applied magnetic field has been investigated by X-ray diffraction in transmission geometry (t-XRD) with the diffraction vector parallel and perpendicular to the field direction. The saturation magnetostriction (λ{sub s}) of nanocrystalline Fe{sub 94−x}Nb{sub 6}B{sub x} was found to increase linearly with the volume fraction of the residual amorphous phase and is well described by taking into account the volume-weighted average of two local λ{sub s} values for the bcc-Fe nanocrystallites (−5 ± 2 ppm) and the residual amorphous matrix (+8 ± 2 ppm). The lattice distortion required to produce the measured K{sub u} values (∼100 J/m{sup 3}) was estimated via the inverse magnetostrictive effect using the measured λ{sub s} values and was compared to the lattice spacing estimations made by t-XRD. The lattice strain required to produce K{sub u} under the magnetoelastic model was not observed by the t-XRD experiments and so the findings of this study suggest that the origin of magnetic field induced K{sub u} cannot be explained through the magnetoelastic effect.

  2. Effect of zinc doping on magnetic and magnetoelastic properties of cobalt ferrite synthesized by autocombustion process

    NASA Astrophysics Data System (ADS)

    Reddy, M. Vinitha; Paul, J. Praveen; Das, Dibakar

    2013-06-01

    Zn-doped cobalt-ferrite, with nominal compositions Co1-xZnxFe2O4(0≤x≤0.3), were synthesized by a novel auto combustion technique. The structural properties of the Zn substituted ferrites have been characterized using x-ray diffraction (XRD). The as-synthesized powders were calcined at 800°C for 3 hrs and the powders were pressed into cylindrical pellets. Solid-state sintering at 1300°C for 12 hrs of the green pellets resulted in a single phase cubic-spinel structure, as observed and analyzed from the XRD spectra. Room temperature magnetic properties were studied using vibrating sample magnetometer (VSM) with field strengths up to ± 15 kOe. Magnetoelastic properties were measured using strain gauge method in a pulsed field magnetometer. Effect of zinc doping on its magnetic and magnetoelastic properties of cobalt ferrite is discussed in this paper.

  3. Contactless Magnetic Slip Ring

    NASA Technical Reports Server (NTRS)

    Kumagai, Hiroyuki (Inventor); Deardon, Joe D. (Inventor)

    1997-01-01

    A contactless magnetic slip ring is disclosed having a primary coil and a secondary coil. The primary and secondary coils are preferably magnetically coupled together, in a highly reliable efficient manner, by a magnetic layered core. One of the secondary and primary coils is rotatable and the contactless magnetic slip ring provides a substantially constant output.

  4. Magnetic Membrane System

    DOEpatents

    McElfresh, Michael W.; ; Lucas, Matthew S.

    2004-12-30

    The present invention provides a membrane with magnetic particles. In one embodiment the membrane is created by mixing particles in a non-magnetic base. The membrane may act as an actuator, a sensor, a pump, a valve, or other device. A magnet is operatively connected to the membrane. The magnet acts on and changes the shape of the membrane.

  5. Magnetic-flux pump

    NASA Technical Reports Server (NTRS)

    Hildebrandt, A. F.; Elleman, D. D.; Whitmore, F. C. (Inventor)

    1966-01-01

    A magnetic flux pump is described for increasing the intensity of a magnetic field by transferring flux from one location to the magnetic field. The device includes a pair of communicating cavities formed in a block of superconducting material, and a piston for displacing the trapped magnetic flux into the secondary cavity producing a field having an intense flux density.

  6. A Magnetic Paradox

    ERIC Educational Resources Information Center

    Arndt, Ebe

    2006-01-01

    Two recent articles in this journal described how an air core solenoid connected to an ac power source may restore the magnetization of a bar magnet with an alternating magnetic field (see Figs. 1 and 2). Although we are quite accustomed to using a constant magnetic field in an air core solenoid to remagnetize a ferromagnet, it is puzzling that we…

  7. Magnetic multilayer structure

    DOEpatents

    Herget, Philipp; O'Sullivan, Eugene J.; Romankiw, Lubomyr T.; Wang, Naigang; Webb, Bucknell C.

    2017-03-21

    A mechanism is provided for an integrated laminated magnetic device. A substrate and a multilayer stack structure form the device. The multilayer stack structure includes alternating magnetic layers and diode structures formed on the substrate. Each magnetic layer in the multilayer stack structure is separated from another magnetic layer in the multilayer stack structure by a diode structure.

  8. Magnetic multilayer structure

    SciTech Connect

    Herget, Philipp; O'Sullivan, Eugene J.; Romankiw, Lubomyr T.; Wang, Naigang; Webb, Bucknell C.

    2016-07-05

    A mechanism is provided for an integrated laminated magnetic device. A substrate and a multilayer stack structure form the device. The multilayer stack structure includes alternating magnetic layers and diode structures formed on the substrate. Each magnetic layer in the multilayer stack structure is separated from another magnetic layer in the multilayer stack structure by a diode structure.

  9. Structural, vibrational and magnetic properties of Ni{sub 1−x}Co{sub x}Fe{sub 2}O{sub 4} ferrites

    SciTech Connect

    Nandan, Brajesh Bhatnagar, M. C.

    2015-08-28

    The ferrite with chemical formula Ni{sub 1−x}Co{sub x}Fe{sub 2}O{sub 4} (x= 0.00, 0.50, 1.00) were prepared using sol-gel method. X-ray diffraction (XRD), Raman spectroscopy and physical property measurement system (PPMS) were used to characterize the structural, vibrational and magnetic properties. XRD pattern confirmed single crystalline spinel structure of Nickel ferrite with Co substitution. Lattice parameter variation confirms the substitution of Co{sup 2+} ions at the place of Ni{sup 2+} into the nickel ferrite. Raman scattering at room temperature is used to study the redistribution of Ni and Co cations between tetrahedral (A) and octahedral (B) sites. A shift is observed in Co substitute nickel ferrite in both XRD and Raman studies. M-H hysteresis is carried out at room temperature. Saturation magnetization of the samples is increased with the Co{sup 2+} ions substitution.

  10. Structure and magnetism in fcc magnetic transition metals on (001) diamond (abstract)

    NASA Astrophysics Data System (ADS)

    Wolf, J. A.; Krebs, J. J.; Idzerda, Y. U.; Prinz, G. A.; Kemner, K. M.

    1996-04-01

    We have prepared single crystal face centered cubic (fcc) magnetic transition metal films (Co,Ni,Fe) on (001) diamonds, the thickness of the films varying between a few tenths of a nanometer to over 100 nm. The crystalline quality and fourfold symmetry of these layers was monitored in situ during the film growth with RHEED and a chemical analysis was performed using Auger spectroscopy. In addition, the structure of the samples was investigated ex situ using X-ray diffraction and EXAFS, demonstrating the single crystal, fcc (001) structure throughout each entire film. The magnetic characterization was performed with Ferromagnetic Resonance (FMR) and Superconducting Quantum Interference Device (SQUID) hysteresis loops. The saturation magnetization of the Co films is only slightly lower than the literature values. The coercive fields are very small (˜25 Oe) and the magnetization reversal very sharp. The FMR yielded a fourfold anisotropy comparable to literature values. The observation of the first standing spinwaves underlines the good quality. The Ni films are tetragonally distorted due to the 1.2% mismatch. The FMR data indicate a significant perpendicular anisotropy slightly smaller than 4πM, the fourfold in-plane anisotropy being comparable to the bulk value. The saturation magnetization is reduced by 30% compared to bulk values, probably due to nickel-carbide which was observed in the XRD data from some samples. Neither the in-plane <110> nor the in-plane <100> axis show an easy axis behavior and both require fields in excess of 6000 Oe to saturate, the coercive fields being about 200 Oe. The RHEED patterns of the Fe films show single crystal growth with a lattice constant comparable to diamond, indicating an fcc structure. A similar structural and magnetic characterization of these films will also be presented.

  11. Illustrating the processability of magnetic layered double hydroxides: layer-by-layer assembly of magnetic ultrathin films.

    PubMed

    Coronado, E; Martí-Gastaldo, C; Navarro-Moratalla, E; Ribera, A; Tatay, S

    2013-05-20

    We report the preparation of single-layer layered double hydroxide (LDH) two-dimensional (2D) nanosheets by exfoliation of highly crystalline NiAl-NO3 LDH. Next, these unilamellar moieties have been incorporated layer-by-layer (LbL) into a poly(sodium 4-styrenesulfonate)/LDH nanosheet multilayer ultrathin film (UTF). Fourier transform infrared spectroscopy (FT-IR), ultraviolet-visible light (UV-vis), and X-ray diffraction (XRD) profiles have been used to follow the uniform growth of the UTF. The use of a magnetic LDH as the cationic component of the multilayered architecture enables study of the resulting magnetic properties of the UTFs. Our magnetic data show the appearance of spontaneous magnetization at ∼5 K, thus confirming the effective transfer of the magnetic properties of the bulk LDH to the self-assembled film that displays glassy-like ferromagnetic behavior. The high number of bilayers accessible-more than 80-opens the door for the preparation of more-complex hybrid multifunctional materials that combine magnetism with the physical properties provided by other exfoliable layered inorganic hosts.

  12. Evaluation the Impact of Annealing on Phase Evolution, Microstructure, and Magnetic Properties of Nanocrystalline Ball-Milled LiSm Ferrite

    NASA Astrophysics Data System (ADS)

    Mahmoudi, M.; Kavanlouei, M.; Maleki-Ghaleh, H.

    2014-09-01

    The impact of milling and subsequent annealing on the phase evolution, microstructure and magnetic properties of Li0.5Sm x Fe2.5- x O4 ( x = 0, 0.05, 0.1, 0.2) ferrite prepared by mechanical alloying was investigated. X-ray diffraction (XRD), scanning electron microscope, Fourier transform infrared spectroscopy, laser particle size analysis, and vibrating sample magnetometry were employed to characterize the prepared LiSm compound. The structure was evaluated by XRD, confirmed the formation of its single-phase spinel structure. The magnetic properties of the milled nanostructured powder were extensively affected by the annealing temperature. The substitution of samarium significantly influences the magnetic characteristics, proved by magnetization measurements at room temperature.

  13. Crystal structure and magnetic properties of new Fe3Co3 X 2 (X  =  Ti, Nb) intermetallic compounds

    NASA Astrophysics Data System (ADS)

    Zhang, Jie; Nguyen, Manh Cuong; Balasubramanian, Balamurugan; Das, Bhaskar; Sellmyer, David J.; Zeng, Zhi; Ho, Kai-Ming; Wang, Cai-Zhuang

    2016-05-01

    The structure and magnetic properties of new magnetic Fe3Co3 X 2 (X  =  Ti, Nb) compounds are studied by genetic algorithm, first-principles density functional theory (DFT) calculations, and experiments. The atomic structure of a hexagonal structure with P-6m2 symmetry is determined. The simulated x-ray diffraction (XRD) spectra of the P-6m2 structures agree well with experimental XRD data for both Fe3Co3Ti2 and Fe3Co3Nb2. The magnetic properties of these structures as well as the effect of the disorder of Fe and Co on their magnetic properties are also investigated. The magnetocrystalline anisotropy energy is found to be very sensitive to the occupancy disorder between Fe and Co.

  14. Linear magnetic bearing

    NASA Technical Reports Server (NTRS)

    Studer, P. A. (Inventor)

    1983-01-01

    A linear magnetic bearing system having electromagnetic vernier flux paths in shunt relation with permanent magnets, so that the vernier flux does not traverse the permanent magnet, is described. Novelty is believed to reside in providing a linear magnetic bearing having electromagnetic flux paths that bypass high reluctance permanent magnets. Particular novelty is believed to reside in providing a linear magnetic bearing with a pair of axially spaced elements having electromagnets for establishing vernier x and y axis control. The magnetic bearing system has possible use in connection with a long life reciprocating cryogenic refrigerator that may be used on the space shuttle.

  15. Hybrid superconducting magnetic suspensions

    SciTech Connect

    Tixador, P.; Hiebel, P.; Brunet, Y.

    1996-07-01

    Superconductors, especially high T{sub c} ones, are the most attractive materials to design stable and fully passive magnetic suspensions which have to control five degrees of freedom. The hybrid superconducting magnetic suspensions present high performances and a simple cooling mode. They consist of a permanent magnet bearing, stabilized by a suitable magnet-superconductor structure. Several designs are given and compared in terms of forces and stiffnesses. The design of the magnet bearing plays an important part. The superconducting magnetic bearing participates less in levitation but must provide a high stabilizing stiffness. This is achieved by the magnet configuration, a good material in term of critical current density and field cooling. A hybrid superconducting suspension for a flywheel is presented. This system consists of a magnet thrust bearing stabilized by superconductors interacting with an alternating polarity magnet structure. First tests and results are reported. Superconducting materials are magnetically melt-textured YBaCuO.

  16. Poly-l-lysine-coated magnetic nanoparticles as intracellular actuators for neural guidance

    PubMed Central

    Riggio, Cristina; Calatayud, Maria Pilar; Hoskins, Clare; Pinkernelle, Josephine; Sanz, Beatriz; Torres, Teobaldo Enrique; Ibarra, Manuel Ricardo; Wang, Lijun; Keilhoff, Gerburg; Goya, Gerardo Fabian; Raffa, Vittoria; Cuschieri, Alfred

    2012-01-01

    Purpose It has been proposed in the literature that Fe3O4 magnetic nanoparticles (MNPs) could be exploited to enhance or accelerate nerve regeneration and to provide guidance for regenerating axons. MNPs could create mechanical tension that stimulates the growth and elongation of axons. Particles suitable for this purpose should possess (1) high saturation magnetization, (2) a negligible cytotoxic profile, and (3) a high capacity to magnetize mammalian cells. Unfortunately, the materials currently available on the market do not satisfy these criteria; therefore, this work attempts to overcome these deficiencies. Methods Magnetite particles were synthesized by an oxidative hydrolysis method and characterized based on their external morphology and size distribution (high-resolution transmission electron microscopy [HR-TEM]) as well as their colloidal (Z potential) and magnetic properties (Superconducting QUantum Interference Devices [SQUID]). Cell viability was assessed via Trypan blue dye exclusion assay, cell doubling time, and MTT cell proliferation assay and reactive oxygen species production. Particle uptake was monitored via Prussian blue staining, intracellular iron content quantification via a ferrozine-based assay, and direct visualization by dual-beam (focused ion beam/scanning electron microscopy [FIB/SEM]) analysis. Experiments were performed on human neuroblastoma SH-SY5Y cell line and primary Schwann cell cultures of the peripheral nervous system. Results This paper reports on the synthesis and characterization of polymer-coated magnetic Fe3O4 nanoparticles with an average diameter of 73 ± 6 nm that are designed as magnetic actuators for neural guidance. The cells were able to incorporate quantities of iron up to 2 pg/cell. The intracellular distribution of MNPs obtained by optical and electronic microscopy showed large structures of MNPs crossing the cell membrane into the cytoplasm, thus rendering them suitable for magnetic manipulation by external

  17. Synthesis of magnetic multicomponent nanoparticles CuxNi1-xFe2O4

    NASA Astrophysics Data System (ADS)

    Bingölbali, A.; Doğan, N.; Yeşil, Z.; Asiltürk, M.

    2015-01-01

    Magnetic nanoparticles (MNPs) are of great importance in many biomedical applications, such as drug delivery, hyperthermia, and magnetic resonance imaging (MRI) contrast enhancement. To build the most effective magnetic nanoparticle systems for various biomedical applications, characteristics of particle, including size, surface chemistry, magnetic properties, and toxicity have to be fully investigated. In this work, the effects of some production methods of the magnetic nanoparticles for the bio-medical applications are discussed. In this study, multicomponents of CuxNi1-xFe2O4 nanoparticles (where x=0, 0.6, and 1) were prepared by the hydrothermal synthesis method. In addition, X-ray powder diffractometry (XRD), scanning electron microscopy (SEM), and a vibrating scanning magnetometer (VSM) were used to characterize the structural, morphological and magnetic properties of the nanoparticles. The particle sizes of the samples were measured by Malvern Instruments Zeta Sizer Nano-ZS instrument. The data were recorded under magnetic fields for different ratios of CuxNi1-xFe2O4 nanoparticles. The temperature dependence of field cooled (FC) magnetization of the CuxNi1-xFe2O4 samples has been shown in this work. Magnetizations change with decreasing the dopant value of Cu. The magnetic phase transition was observed for CuxNi1-xFe2O4 nanoparticles.

  18. Scanning electron microscopy and magnetic characterization of iron oxides in solid waste landfill leachate.

    PubMed

    Huliselan, Estevanus Kristian; Bijaksana, Satria; Srigutomo, Wahyu; Kardena, Edwan

    2010-07-15

    Leachate sludge samples were taken from two municipal solid waste sites of Jelekong and Sarimukti in Bandung, Indonesia. Their magnetic mineralogy and granulometry were analyzed to discriminate the sources of magnetic minerals using X-ray diffraction (XRD), scanning electron microscopy equipped with energy-dispersive X-ray spectroscopy (SEM-EDX) and rock magnetism. SEM-EDX analyses infer that the main magnetic minerals in the leachate sludge are iron oxides. In terms of their morphology, the grains from Jelekong are mostly octahedral and angular, which are similar to the general shapes of magnetic grains from the local soils. The grains from Sarimukti, on the other hand, are dominated by imperfect spherule shapes suggesting the product of combustion processes. Hysteresis parameters verify that the predominant magnetic mineral in leachate sludge is low coercivity ferrimagnetic mineral such as magnetite (Fe(3)O(4)). Furthermore, comparisons of rock magnetic parameters show that the magnetic minerals of soil samples from Jelekong have higher degree of magnetic pedogenesis indicating higher proportion of superparamagnetic/ultrafine particles than those of soil samples from Sarimukti. The plot of susceptibilities ratio versus coercive force has a great potential to be used as a discriminating tool for determining the source of magnetic minerals.

  19. Magnetic materials based on iron dispersed in graphitic matrices II. High temperatures and mesophase pitch

    NASA Astrophysics Data System (ADS)

    Dyakonov, Alexander J.; Jack McCormick, B.; Kahol, Pawan K.; Hamdeh, Hussein H.

    1997-03-01

    Ferromagnetic materials based on iron incorporated into pitch were synthesized, and characterized by magnetic methods (Faraday), Mössbauer spectroscopy, SEM, and XRD. A graphitic-type structure was observed to form at 350-1650°C. The important role of a mesophase structure of a pitch-precursor in the iron carbonyl absorption and anisotropic structure of the resulting iron containing material was found.

  20. Effect of Co doping on structural, optical, magnetic and dielectric properties of Bi2Fe4O9

    NASA Astrophysics Data System (ADS)

    Mohapatra, S. R.; Sahu, B.; Kaushik, S. D.; Singh, A. K.

    2015-06-01

    Polycrystalline Bi2Fe4O9 and 2% Co doped Bi2Fe4O9 were prepared by solid state reaction route. X-ray diffraction (XRD) result reveals that there is no change in the crystal structure due to Co doping and the compound has orthorhombic structure. UV-visible spectroscopy confirms the decrease in band gap due Co doping. Zero field cooled magnetization measurement at 100 Oe magnetic field shows substantial decrease in the magnetic transition temperature. Room temperature frequency dependent dielectric permittivity at 1V DC bias shows ˜10% increase in Co doped sample with respect to pure Bi2Fe4O9.

  1. The effect of varying the capping agent of magnetic/luminescent Fe3O4-InP/ZnSe core-shell nanocomposite

    NASA Astrophysics Data System (ADS)

    Paulsen, Zuraan; Onani, Martin O.; Allard, Garvin R. J.; Kiplagat, Ayabei; Okil, Joseph O.; Dejene, Francis B.; Mahanga, Geoffrey M.

    2016-01-01

    Magnetic-luminescent nanoparticles have shown great promise in various biomedical applications namely: contrast agents for magnetic resonance imaging, multifunctional drug carrier system, magnetic separation of cells, cell tracking, immunoassay, and magnetic bioseparation. This experiment describes the synthesis of a nanocomposite material, which is composed of an iron oxide (Fe3O4) superparamagnetic core and an indium phosphide/zinc selenide (InP/ZnSe) quantum dot shell. The magnetic nanoparticles (MNP's) and quantum dots (QD's) were synthesized separately before allowing them to conjugate. The MNP's were functionalized with a thiol-group allowing the QD shell to bind to the surface of the MNP by the formation of a thiol-metal bond. The nanocomposite was capped with 3-mercaptopropionic acid, oleylamine, β-cyclodextrin and their influence on the photoluminescence investigated. The synthesized nanocomposite was characterized with high- resolution transmission electron microscopy (HR-TEM), energy-dispersive spectroscopy (EDS), selective electron area diffraction (SAED), scanning electron microscopy (SEM), superconducting quantum interference device (SQUID), and photoluminescence. These techniques yielded particle size, morphology, dispersion, and chemical composition including luminescence and florescence.

  2. Microstructural evolution and magnetic properties of ultrafine solute-atom particles formed in a Cu75-Ni20-Fe5 alloy on isothermal annealing

    NASA Astrophysics Data System (ADS)

    Kim, Jun-Seop; Takeda, Mahoto; Bae, Dong-Sik

    2016-12-01

    Microstructural features strongly affect magnetism in nano-granular magnetic materials. In the present work we have investigated the relationship between the magnetic properties and the self-organized microstructure formed in a Cu75-Ni20-Fe5 alloy comprising ferromagnetic elements and copper atoms. High resolution transmission electron microscopy (HRTEM) observations showed that on isothermal annealing at 873 K, nano-scale solute (Fe,Ni)-rich clusters initially formed with a random distribution in the Cu-rich matrix. Superconducting quantum interference device (SQUID) measurements revealed that these ultrafine solute clusters exhibited super-spinglass and superparamagnetic states. On further isothermal annealing the precipitates evolved to cubic or rectangular ferromagnetic particles and aligned along the <100> directions of the copper-rich matrix. Electron energy-band calculations based on the first-principle Korringa-Kohn-Rostocker (KKR) method were also implemented to investigate both the electronic structure and the magnetic properties of the alloy. Inputting compositions obtained experimentally by scanning transmission electron microscopy-electron dispersive X-ray spectroscopy (STEM-EDS) analysis, the KKR calculation confirmed that ferromagnetic precipitates (of moment 1.07μB per atom) formed after annealing for 2 × 104 min. Magneto-thermogravimetric (MTG) analysis determined with high sensitivity the Curie temperatures and magnetic susceptibility above room temperature of samples containing nano-scale ferromagnetic particles.

  3. The effects of high magnetic field on the morphology and microwave electromagnetic properties of MnO{sub 2} powder

    SciTech Connect

    Jia Zhang; Duan Yuping; Li Shuqing; Li Xiaogang; Liu Shunhua

    2010-07-15

    MnO{sub 2} with a sea urchin-like ball chain shape was first synthesized in a high magnetic field via a simple chemical process, and a mechanism for the formation of this grain shape was discussed. The as-synthesized samples were characterized by XRD, SEM, TEM, and vector network analysis. The dielectric constant and the loss tangent clearly decreased under a magnetic field. The magnetic loss tangent and the imaginary part of the magnetic permeability increased substantially. Furthermore, the theoretically calculated values of reflection loss showed that the absorption peaks shifted to a higher frequency with increases in the magnetic field strength. - Graphical abstract: MnO{sub 2} with a sea urchin-like ball chain shape is first synthesized in a high magnetic field via a simple hydrothermal route.

  4. Magnetic Damping For Maglev

    DOE PAGES

    Zhu, S.; Cai, Y.; Rote, D. M.; ...

    1998-01-01

    Magnetic damping is one of the important parameters that control the response and stability of maglev systems. An experimental study to measure magnetic damping directly is presented. A plate attached to a permanent magnet levitated on a rotating drum was tested to investigate the effect of various parameters, such as conductivity, gap, excitation frequency, and oscillation amplitude, on magnetic damping. The experimental technique is capable of measuring all of the magnetic damping coefficients, some of which cannot be measured indirectly.

  5. Magnetically operated check valve

    NASA Astrophysics Data System (ADS)

    Morris, Brian G.; Bozeman, Richard J., Jr.

    1993-03-01

    A magnetically operated check valve is disclosed having, in one aspect, a valve body and a movable poppet disposed therein. A magnet attracts the poppet to hold the valve shut until the force of fluid flow through the valve overcomes the magnetic attraction and moves the poppet to an unseated, open position. The poppet and magnet are configured and disposed to trap a magnetically attracted particulate and prevent it from flowing to a valve seating region.

  6. Magnetically operated check valve

    NASA Technical Reports Server (NTRS)

    Morris, Brian G. (Inventor); Bozeman, Richard J., Jr. (Inventor)

    1994-01-01

    A magnetically operated check valve is disclosed. The valve is comprised of a valve body and a movable poppet disposed therein. A magnet attracts the poppet to hold the valve shut until the force of fluid flow through the valve overcomes the magnetic attraction and moves the poppet to an unseated, open position. The poppet and magnet are configured and disposed to trap a magnetically attracted particulate and prevent it from flowing to a valve seating region.

  7. Magnetically operated check valve

    NASA Astrophysics Data System (ADS)

    Morris, Brian G.; Bozeman, Richard J., Jr.

    1994-06-01

    A magnetically operated check valve is disclosed. The valve is comprised of a valve body and a movable poppet disposed therein. A magnet attracts the poppet to hold the valve shut until the force of fluid flow through the valve overcomes the magnetic attraction and moves the poppet to an unseated, open position. The poppet and magnet are configured and disposed to trap a magnetically attracted particulate and prevent it from flowing to a valve seating region.

  8. PyXRD v0.6.7: a free and open-source program to quantify disordered phyllosilicates using multi-specimen X-ray diffraction profile fitting

    NASA Astrophysics Data System (ADS)

    Dumon, M.; Van Ranst, E.

    2016-01-01

    This paper presents a free and open-source program called PyXRD (short for Python X-ray diffraction) to improve the quantification of complex, poly-phasic mixed-layer phyllosilicate assemblages. The validity of the program was checked by comparing its output with Sybilla v2.2.2, which shares the same mathematical formalism. The novelty of this program is the ab initio incorporation of the multi-specimen method, making it possible to share phases and (a selection of) their parameters across multiple specimens. PyXRD thus allows for modelling multiple specimens side by side, and this approach speeds up the manual refinement process significantly. To check the hypothesis that this multi-specimen set-up - as it effectively reduces the number of parameters and increases the number of observations - can also improve automatic parameter refinements, we calculated X-ray diffraction patterns for four theoretical mineral assemblages. These patterns were then used as input for one refinement employing the multi-specimen set-up and one employing the single-pattern set-ups. For all of the assemblages, PyXRD was able to reproduce or approximate the input parameters with the multi-specimen approach. Diverging solutions only occurred in single-pattern set-ups, which do not contain enough information to discern all minerals present (e.g. patterns of heated samples). Assuming a correct qualitative interpretation was made and a single pattern exists in which all phases are sufficiently discernible, the obtained results indicate a good quantification can often be obtained with just that pattern. However, these results from theoretical experiments cannot automatically be extrapolated to all real-life experiments. In any case, PyXRD has proven to be useful when X-ray diffraction patterns are modelled for complex mineral assemblages containing mixed-layer phyllosilicates with a multi-specimen approach.

  9. Structural and magnetic characterization of as-prepared and annealed FeCoCu nanowire arrays in ordered anodic aluminum oxide templates

    SciTech Connect

    Rodríguez-González, B.; Bran, C.; Warnatz, T.; Vazquez, M.; Rivas, J.

    2014-04-07

    Herein, we report on the preparation, structure, and magnetic characterization of FeCoCu nanowire arrays grown by DC electrodeposition inside self-assembled ordered nanopores of anodic aluminum oxide templates. A systematic study of their structure has been performed both in as-prepared samples and after annealing in the temperature range up to 800 °C, although particular attention has been paid to annealing at 700 °C after which maximum magnetic hardening is achieved. The obtained nanowires have a diameter of 40 nm and their Fe{sub 0.28}Co{sub 0.67}Cu{sub 0.05} composition was confirmed by energy dispersive X-ray spectroscopy (EDS). Focused ion-beam lamellas of two samples (as-prepared and annealed at 700 °C) were prepared for their imaging in the high-resolution transmission electron microscopy (HRTEM) perpendicularly to the electron beam, where the obtained EDS compositional mappings show a homogeneous distribution of the elements. X-ray diffraction analysis, and selected area electron diffraction (SAED) patterns confirm that nanowires exhibit a bcc cubic structure (space group Im-3m). In addition, bright-dark field images show that the nanowires have a polycrystalline structure that remains essentially the same after annealing, but some modifications were observed: (i) an overall increase and sharpening of recrystallized grains, and (ii) an apparent shrinkage of the nanowires diameter. Obtained SAED patterns also show strong textured components with determined <111> and <112> crystalline directions parallel to the wires growth direction. The presence of both directions was also confirmed in the HRTEM images doing Fourier transform analyses. Magnetic measurements show strong magnetic anisotropy with magnetization easy axis parallel to the nanowires in as-prepared and annealed samples. The magnetic properties are tuned by suitable thermal treatments so that, maximum enhanced coercivity (∼2.7 kOe) and normalized remanence (∼0.91 Ms) values are

  10. Electrodeposition of iron and iron-aluminium alloys in an ionic liquid and their magnetic properties.

    PubMed

    Giridhar, P; Weidenfeller, B; El Abedin, S Zein; Endres, F

    2014-05-28

    In this work we show that nanocrystalline iron and iron-aluminium alloys can be electrodeposited from the ionic liquid 1-butyl-1-methylpyrrolidinium trifluoromethylsulfonate, [Py1,4]TfO, at 100 °C. The study comprises CV, SEM, XRD, and magnetic measurements. Two different sources of iron(ii) species, Fe(TfO)2 and FeCl2, were used for the electrodeposition of iron in [Py1,4]TfO. Cyclic voltammetry was employed to evaluate the electrochemical behavior of FeCl2, Fe(TfO)2, and (FeCl2 + AlCl3) in the employed ionic liquid. Thick iron deposits were obtained from FeCl2/[Py1,4]TfO at 100 °C. Electrodeposition of iron-aluminium alloys was successful in the same ionic liquid at 100 °C. The morphology and crystallinity of the obtained deposits were investigated using SEM and XRD, respectively. XRD measurements reveal the formation of iron-aluminium alloys. First magnetic measurements of some deposits gave relatively high coercive forces and power losses in comparison to commercial iron-silicon samples due to the small grain size in the nanometer regime. The present study shows the feasibility of preparing magnetic alloys from ionic liquids.

  11. On the mineral core of ferritin-like proteins: structural and magnetic characterization.

    PubMed

    García-Prieto, A; Alonso, J; Muñoz, D; Marcano, L; Abad Díaz de Cerio, A; Fernández de Luis, R; Orue, I; Mathon, O; Muela, A; Fdez-Gubieda, M L

    2016-01-14

    It is generally accepted that the mineral core synthesized by ferritin-like proteins consists of a ferric oxy-hydroxide mineral similar to ferrihydrite in the case of horse spleen ferritin (HoSF) and an oxy-hydroxide-phosphate phase in plant and prokaryotic ferritins. The structure reflects a dynamic process of deposition and dissolution, influenced by different biological, chemical and physical variables. In this work we shed light on this matter by combining a structural (High Resolution Transmission Electron Microscopy (HRTEM) and Fe K-edge X-ray Absorption Spectroscopy (XAS)) and a magnetic study of the mineral core biomineralized by horse spleen ferritin (HoSF) and three prokaryotic ferritin-like proteins: bacterial ferritin (FtnA) and bacterioferritin (Bfr) from Escherichia coli and archaeal ferritin (PfFtn) from Pyrococcus furiosus. The prokaryotic ferritin-like proteins have been studied under native conditions and inside the cells for the sake of preserving their natural attributes. They share with HoSF a nanocrystalline structure rather than an amorphous one as has been frequently reported. However, the presence of phosphorus changes drastically the short-range order and magnetic response of the prokaryotic cores with respect to HoSF. The superparamagnetism observed in HoSF is absent in the prokaryotic proteins, which show a pure atomic-like paramagnetic behaviour attributed to phosphorus breaking the Fe-Fe exchange interaction.

  12. Magnetic novae

    NASA Astrophysics Data System (ADS)

    Zemko, Polina; Orio, Marina

    2016-07-01

    We present the results of optical and X-ray observations of two quiescent novae, V2491 Cyg and V4743 Sgr. Our observations suggest the intriguing possibility of localization of hydrogen burning in magnetic novae, in which accretion is streamed to the polar caps. V2491 Cyg was observed with Suzaku more than 2 years after the outburst and V4743 Sgr was observed with XMM Newton 2 and 3.5 years after maximum. In the framework of a monitoring program of novae previously observed as super soft X-ray sources we also obtained optical spectra of V4743 Sgr with the SALT telescope 11.5 years after the eruption and of V2491 Cyg with the 6m Big Azimutal Telescope 4 and 7 years post-outburst. In order to confirm the possible white dwarf spin period of V2491 Cyg measured in the Suzaku observations we obtained photometric data using the 90cm WIYN telescope at Kitt Peak and the 1.2 m telescope in Crimea. We found that V4743 Sgr is an intermediate polar (IP) and V2491 Cyg is a strong IP candidate. Both novae show modulation of their X-ray light curves and have X-ray spectra typical of IPs. The Suzaku and XMM Newton exposures revealed that the spectra of both novae have a very soft blackbody-like component with a temperature close to that of the hydrogen burning white dwarfs in their SSS phases, but with flux by at least two orders of magnitude lower, implying a possible shrinking of emitting regions in the thin atmosphere that is heated by nuclear burning underneath it. In quiescent IPs, independently of the burning, an ultrasoft X-ray flux component originates at times in the polar regions irradiated by the accretion column, but the soft component of V4743 Sgr disappeared in 2006, indicating that the origin may be different from accretion. We suggest it may have been due to an atmospheric temperature gradient on the white dwarf surface, or to continuing localized thermonuclear burning at the bottom of the envelope, before complete turn-off. The optical spectra of V2491 Cyg and V

  13. Nanocomposite Magnets: Transformational Nanostructured Permanent Magnets

    SciTech Connect

    2010-10-01

    Broad Funding Opportunity Announcement Project: GE is using nanomaterials technology to develop advanced magnets that contain fewer rare earth materials than their predecessors. Nanomaterials technology involves manipulating matter at the atomic or molecular scale, which can represent a stumbling block for magnets because it is difficult to create a finely grained magnet at that scale. GE is developing bulk magnets with finely tuned structures using iron-based mixtures that contain 80% less rare earth materials than traditional magnets, which will reduce their overall cost. These magnets will enable further commercialization of HEVs, EVs, and wind turbine generators while enhancing U.S. competitiveness in industries that heavily utilize these alternatives to rare earth minerals.

  14. Magnetically Damped Furnace Bitter Magnet Coil 1

    NASA Technical Reports Server (NTRS)

    Bird, M. D.

    1997-01-01

    A magnet has been built by the National High Magnetic Field Laboratory for NASA on a cost reimbursement contract. The magnet is intended to demonstrate the technology and feasibility of building a magnet for space based crystal growth. A Bitter magnet (named after Francis Bitter, its inventor) was built consisting of four split coils electrically in series and hydraulically in parallel. The coils are housed in a steel vessel to reduce the fringe field and provide some on-axis field enhancement. The steel was nickel plated and Teflon coated to minimize interaction with the water cooling system. The magnet provides 0.14 T in a 184 mm bore with 3 kW of power.

  15. Electrically Tunable Magnetism in Magnetic Topological Insulators

    NASA Astrophysics Data System (ADS)

    Zhang, Shou-Cheng; Wang, Jing; Lian, Biao

    2015-03-01

    The external controllability of the magnetic properties in topological insulators would be important both for fundamental and practical interests. Here we predict the electric-field control of ferromagnetism in a thin film of insulating magnetic topological insulators. The decrease of band inversion by the application of electric fields results in a reduction of magnetic susceptibility, and hence in the modication of magnetism. Remarkably, the electric field could even induce the magnetic quantum phase transition from ferromagnetism to paramagnetism. We further propose a topological transistor device in which the dissipationless charge transport of chiral edge states is controlled by an electric field. The simultaneous electrical control of magnetic order and chiral edge transport in such a device may lead to electronic and spintronic applications for topological insulators. This work is supported by the U.S. Department of Energy, Office of Basic Energy Sciences, Division of Materials Sciences and Engineering, under Contract No. DE-AC02-76SF00515.

  16. Morphology evolution of single-crystalline hematite nanocrystals: magnetically recoverable nanocatalysts for enhanced facet-driven photoredox activity

    NASA Astrophysics Data System (ADS)

    Patra, Astam K.; Kundu, Sudipta K.; Bhaumik, Asim; Kim, Dukjoon

    2015-12-01

    We have developed a new green chemical approach for the shape-controlled synthesis of single-crystalline hematite nanocrystals in aqueous medium. FESEM, HRTEM and SAED techniques were used to determine the morphology and crystallographic orientations of each nanocrystal and its exposed facets. PXRD and HRTEM techniques revealed that the nanocrystals are single crystalline in nature; twins and stacking faults were not detected in these nanocrystals. The structural, vibrational, and electronic spectra of these nanocrystals were highly dependent on their shape. Different shaped hematite nanocrystals with distinct crystallographic planes have been synthesized under similar reaction conditions, which can be desired as a model for the purpose of properties comparison with the nanocrystals prepared under different reaction conditions. Here we investigated the photocatalytic performance of these different shaped-nanocrystals for methyl orange degradation in the presence of white light (λ > 420 nm). In this study, we found that the density of surface Fe3+ ions in particular facets was the key factor for the photocatalytic activity and was higher on the bitruncated-dodecahedron shape nanocrystals by coexposed {104}, {100} and {001} facets, attributing to higher catalytic activity. The catalytic activity of different exposed facet nanocrystals were as follows: {104} + {100} + {001} (bitruncated-dodecahedron) > {101} + {001} (bitruncated-octahedron) > {001} + {110} (nanorods) > {012} (nanocuboid) which provided the direct evidence of exposed facet-driven photocatalytic activity. The nanocrystals were easily recoverable using an external magnet and reused at least six times without significant loss of its catalytic activity.We have developed a new green chemical approach for the shape-controlled synthesis of single-crystalline hematite nanocrystals in aqueous medium. FESEM, HRTEM and SAED techniques were used to determine the morphology and crystallographic orientations of

  17. Magnetic and Magnetocaloric Properties of Zn1-x Co x Fe2O4 Nanoparticles

    NASA Astrophysics Data System (ADS)

    Phan, T. L.; Tran, N.; Kim, D. H.; Dang, N. T.; Manh, D. H.; Bach, T. N.; Liu, C. L.; Lee, B. W.

    2017-02-01

    We have prepared Zn1-x Co x Fe2O4 nanoparticles (NPs) by using a hydrothermal method, and then studied their structural and magnetic properties. The analyses of x-ray diffraction (XRD) patterns and Raman scattering spectra reveal that the samples crystallized mainly in a cubic-spinel structure with the lattice parameter a ≈ 8.4 Å. Averaged crystallite sizes determined from the XRD linewidth are about 16-22 nm, close to the particle sizes of 19-28 nm determined from scanning electron microscopy images. Magnetization measurements versus temperature, M(T), in the field H = 100 Oe indicate that the ferromagnetic-paramagnetic (FM-PM) phase transition temperature (T C) of Zn1-x Co x Fe2O4 NPs increases from 606 K for x = 0 to 823 K for x = 1. The features of the M(T) curves also indicate magnetic inhomogeneity in the samples, and their magnetic property is unstable versus temperature. This is ascribed to the changes in the structural characterization and/or concentration of magnetic ions situated at the A and B sites in the spinel lattice. At room temperature, we found that both the saturation magnetization (M s) and coercivity (H c) increase with increasing Co content, with M s = 59-70 emu/g and H c = 100-1100 Oe. These results reflect that the Co doping into ZnFe2O4 NPs greatly improves their magnetic property, making them more useful for practical applications. Additionally, we also assess magnetic interactions and the magnetocaloric effect in the samples based on analyzing initial magnetization data, M(H), recorded at temperatures around T C.

  18. Large gap magnetic suspension system

    NASA Technical Reports Server (NTRS)

    Abdelsalam, Moustafa K.; Eyssa, Y. M.

    1991-01-01

    The design of a large gap magnetic suspension system is discussed. Some of the topics covered include: the system configuration, permanent magnet material, levitation magnet system, superconducting magnets, resistive magnets, superconducting levitation coils, resistive levitation coils, levitation magnet system, and the nitrogen cooled magnet system.

  19. Cosmological magnetic fields

    NASA Astrophysics Data System (ADS)

    Kunze, Kerstin E.

    2013-12-01

    Magnetic fields are observed on nearly all scales in the Universe, from stars and galaxies up to galaxy clusters and even beyond. The origin of cosmic magnetic fields is still an open question, however a large class of models puts its origin in the very early Universe. A magnetic dynamo amplifying an initial seed magnetic field could explain the present day strength of the galactic magnetic field. However, it is still an open problem how and when this initial magnetic field was created. Observations of the cosmic microwave background (CMB) provide a window to the early Universe and might therefore be able to tell us whether cosmic magnetic fields are of a primordial cosmological origin and at the same time constrain its parameters. We will give an overview of the observational evidence of large-scale magnetic fields, describe generation mechanisms of primordial magnetic fields and possible imprints in the CMB.

  20. Multifunctionality in molecular magnetism.

    PubMed

    Pinkowicz, Dawid; Czarnecki, Bernard; Reczyński, Mateusz; Arczyński, Mirosław

    2015-01-01

    Molecular magnetism draws from the fundamental ideas of structural chemistry and combines them with experimental physics resulting in one of the highest profile current topics, namely molecular materials that exhibit multifunctionality. Recent advances in the design of new generations of multifunctional molecular magnets that retain the functions of the building blocks and exhibit non-trivial magnetic properties at higher temperatures provide promising evidence that they may be useful for the future construction of nanoscale devices. This article is not a complete review but is rather an introduction into thefascinating world of multifunctional solids with magnetism as the leitmotif. We provide a subjective selection and discussion of the most inspiring examples of multifunctional molecular magnets: magnetic sponges, guest-responsive magnets, molecular magnets with ionic conductivity, photomagnets and non-centrosymmetric and chiral magnets.