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Sample records for xrd hrtem magnetic

  1. 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.

  2. 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).

  3. 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.

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

    SciTech Connect

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

    2013-05-15

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

  5. Retrieving modulation parameters from HRTEM images of modulated structures.

    PubMed

    Höche, Thomas; Neumann, Wolfgang

    2003-08-01

    Quantitative high-resolution transmission electron microscopy (qHRTEM) is methodologically extended towards the assessment of occupationally and positionally modulated structures. For this purpose, iterative digital image matching has been combined with data processing within the Rietveld refinement code JANA2000. In this approach, the number of free parameters is kept low and rather complicated modulated structures become assessable by qHRTEM. The feasibility of the improved methodology is demonstrated for the 1D modulated structure of Ba(2)TiGe(2)O(8). PMID:12672569

  6. Magnetic properties of NiFe2O4/carbon nanofibers from Venezuelan petcoke

    NASA Astrophysics Data System (ADS)

    Briceño, Sarah; Silva, Pedro; Molina, Wilmer; Brämer-Escamilla, Werner; Alcalá, Olgi; Cañizales, Edgard

    2015-05-01

    NiFe2O4/carbon nanofibers (NiFe2O4/CNFs) have been successfully synthesized by hydrotermal method using Venezuelan petroleum coke (petcoke) as carbon source and NiFe2O4 as catalyst. The morphology, structural and magnetic properties of nanocomposite products were characterized by X-ray diffraction (XRD), high-resolution transmission electron microscopy (HR-TEM), vibrating sample magnetometry (VSM) and electron paramagnetic resonance (EPR). XRD analysis revealed a cubic spinel structure and ferrite phase with high crystallinity. HR-TEM reveals the presence of CNFs with diameters of 4±2 nm. At room temperature, NiFe2O4/CNFs show superparamagnetic behavior with a maximum magnetization of 15.35 emu/g. Our findings indicate that Venezuelan petroleum coke is suitable industrial carbon source for the growth of magnetic CNFs.

  7. XRD and Mössbauer studies of crystallographic and magnetic transformations in synthesized Zn-substituted Cu-Ga-Fe compound

    NASA Astrophysics Data System (ADS)

    Ata-Allah, S. S.

    2004-12-01

    System of samples in the form of Cu 1-xZn xFe 2-yGa yO 4 with ( 0.0⩽x⩽1.0, y=0.0 and 1.0) is synthesized. X-ray diffraction study confirms the presence of a single-phase structure, where tetragonal unit cell is obtained for samples CuFe 2O 4 and CuGaFeO 4 with c/a>1. At compositional parameter x⩾0.25, tetragonal-to-cubic transformation occurs. The determined lattice parameter a for the cubic samples is found to decrease with increasing Zn content x. 57Fe Mössbauer measurements at 293, 77 and 12 K show characteristic spectra of paramagnetic, magnetic, and electronic types for the different compositions. Cation distribution obtained from the spectral analysis at 12 K revealed transformation from the ferrimagnetic inverse spinel of CuFe 2O 4 to the antiferromagnetic normal spinel of ZnFe 2O 4. Hyperfine parameters are found to be strongly dependent on temperature and concentration parameter x. Low-temperature measurements are carried out using installed and well-calibrated closed-cycle variable temperature cryostat Model REF-399-D22. Low vibration is obtained through bellows, spacer, and exchange gas isolation and a difference of 0.018 mm s -1 between the FWHM of a pure iron foil at room temperature and 12 K is achieved.

  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. HR-TEM study of atomic defects in carbon nanostructures

    SciTech Connect

    Urita, K.; Sato, Y.; Suenaga, K.; Iijima, S.

    2005-09-27

    Direct observation of the defect formation in carbon nanostructures during electron irradiation is carried out by high-resolution transmission electron microscopy (HR-TEM) on the double-wall carbon nanotubes (DWNT) and carbon nanopeapods. The irradiation damage due to the knock-on collision with high energy electron beam are found to be dependent on the curvature of the constituent graphen layers. The formation of knock-on defects is more abundant at an inner tube than an outer tube in DWNT, and at a fullerene than a carbon nanotube in carbon nanopeapods. These results definitely indicate that the effects of electron irradiation in nanocarbon materials are quite more prominent on higher surface curvature, such as fullerene.

  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. 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.

  12. 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.

  13. 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.

  14. Synthesis and characterization of luminescence magnetic nanocomposite

    NASA Astrophysics Data System (ADS)

    Kiplagat, Ayabei; Onani, Martin O.; Meyer, Mervin; Akenga, Teresa A.; Dejene, Francis B.

    2016-01-01

    We report a new type of indium based quantum dots which were conjugated to the magnetic Fe2O3 nanoparticles. They were characterized by photoluminescence (PL), high resolution transmission electron microscopy (HRTEM), superconducting quantum interference device (SQUID) and fourier transform infra-red (FTIR). The photoluminescence characteristics of the coupled and uncoupled indium based quantum dots were investigated to determine whether the fluorescing property could be retained in the bifunctional system. Generally, the PL intensity of the quantum dots was observed to reduce significantly and with huge red shift most probably due to quenching effects for the MNPs. The average size of the coupled nanoparticles were found to range between 4 and 5 nm for the quantum dots and range of 6-13 nm for the Fe2O3 magnetic nanoparticles as revealed by both HRTEM and XRD. The highest magnetic saturation reached for both bare and functionalized magnetic nanoparticles was 68.58 emu/g. The FTIR data revealed that the postulated functional groups were actually present in both the bare and functionalized nanoparticles. For instance, Fe-O was observed at around 580 cm-1, O-H at 3432 cm-1 and thiol group at 2929 cm-1 for meso-2,3-dimercaptosuccinic acid capped Fe2O3 magnetic nanoparticles. The energy dispersive spectroscopy (EDS) also confirmed that all the elements of the nanocomposite were actually present in the designed material.

  15. 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. PMID:22166763

  16. 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).

  17. 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.

  18. 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.

  19. Atom by atom: HRTEM insights into inorganic nanotubes and fullerene-like structures

    PubMed Central

    Sadan, Maya Bar; Houben, Lothar; Enyashin, Andrey N.; Seifert, Gotthard; Tenne, Reshef

    2008-01-01

    The characterization of nanostructures down to the atomic scale is essential to understand some physical properties. Such a characterization is possible today using direct imaging methods such as aberration-corrected high-resolution transmission electron microscopy (HRTEM), when iteratively backed by advanced modeling produced by theoretical structure calculations and image calculations. Aberration-corrected HRTEM is therefore extremely useful for investigating low-dimensional structures, such as inorganic fullerene-like particles and inorganic nanotubes. The atomic arrangement in these nanostructures can lead to new insights into the growth mechanism or physical properties, where imminent commercial applications are unfolding. This article will focus on two structures that are symmetric and reproducible. The first structure that will be dealt with is the smallest stable symmetric closed-cage structure in the inorganic system, a MoS2 nanooctahedron. It is investigated by means of aberration-corrected microscopy which allowed validating the suggested DFTB-MD model. It will be shown that structures diverging from the energetically most stable structures are present in the laser ablated soot and that the alignment of the different shells is parallel, unlike the bulk material where the alignment is antiparallel. These findings correspond well with the high-energy synthetic route and they provide more insight into the growth mechanism. The second structure studied is WS2 nanotubes, which have already been shown to have a unique structure with very desirable mechanical properties. The joint HRTEM study combined with modeling reveals new information regarding the chirality of the different shells and provides a better understanding of their growth mechanism. PMID:18838681

  20. Fullerene C60 functionalized γ-Fe2O3 magnetic nanoparticle: Synthesis, characterization, and biomedical applications.

    PubMed

    Kılınç, Ersin

    2016-02-01

    Hybrid magnetic nanoparticles composed from C60 fullerene and γ-Fe2O3 were synthesized by hydrothermal method. XRD, FT-IR, VSM, SEM, and HR-TEM were employed for characterizations. The magnetic saturation value of C60-γ-Fe2O3 magnetic nanoparticles was 66.5 emu g(- 1). Concentration of Fe in nanoparticles asdetermined by ICP-OES was 40.7% Fe. Particle size of C60-γ-Fe2O3 magnetic nanoparticles was smaller than 10 nm. Maximum adsorption capacity of C60-γ-Fe2O3 for flurbiprofen, a non-steroidal anti-inflammatory drug, was calculated from Langmuir isotherm as 142.9 mg g(- 1). PMID:25118710

  1. HRTEM observations of modulated structures in Ti-Pd-Cr [beta][sub 2] alloys

    SciTech Connect

    Schwartz, A.J.; Tanner, L.E.

    1992-08-01

    Conventional and high-resolution transmission electron microscopy (HRTEM) and electron diffraction (ED) have been used to examine a series of Ti[sub 50]Pd[sub 50-x]Cr[sub x][beta][sub 2] (B2, CsCl-type crystal structure) alloys with x between 6 and 10 at.% in order to determine the nature of the modulated structures that develop on cooling. The ED and HRTEM results reveal that the modulation periodicity (inverse of the satellite spacing) varies from three (110)[sub B2] planes in the 6 at.% Cr alloy to four (110)[sub B2] planes for the 10 at.% alloy. Over the same composition range, the monoclinic angle'' (defined between (200)[sub B2]and (020)[sub B2] reflections) is found to increase linearly from 88 to 90[degrees]. It is suggested that these effects are associated with the substitution of Cr for Pd that gives rise to an electronically driven (110)[sub q]<110>[sub [var epsilon

  2. Simulation of bonding effects in HRTEM images of light element materials

    PubMed Central

    Meyer, Jannik C; Künzel, Daniela; Groß, Axel; Kaiser, Ute

    2011-01-01

    Summary The accuracy of multislice high-resolution transmission electron microscopy (HRTEM) simulation can be improved by calculating the scattering potential using density functional theory (DFT) [1–2]. This approach accounts for the fact that electrons in the specimen are redistributed according to their local chemical environment. This influences the scattering process and alters the absolute and relative contrast in the final image. For light element materials with well defined geometry, such as graphene and hexagonal boron nitride monolayers, the DFT based simulation scheme turned out to be necessary to prevent misinterpretation of weak signals, such as the identification of nitrogen substitutions in a graphene network. Furthermore, this implies that the HRTEM image does not only contain structural information (atom positions and atomic numbers). Instead, information on the electron charge distribution can be gained in addition. In order to produce meaningful results, the new input parameters need to be chosen carefully. Here we present details of the simulation process and discuss the influence of the main parameters on the final result. Furthermore we apply the simulation scheme to three model systems: A single atom boron and a single atom oxygen substitution in graphene and an oxygen adatom on graphene. PMID:22003447

  3. Fabrication and temperature dependent magnetic properties of Ni-Cu-Co composite nanowires

    NASA Astrophysics Data System (ADS)

    Hussain, Muhammad; Khan, Maaz; Sun, Hongyu; Nairan, Adeela; Karim, Shafqat; Nisar, Amjad; Maqbool, M.; Ahmad, Mashkoor

    2015-10-01

    Ni-Cu-Co composite magnetic nanowires have been successfully synthesized by electrochemical deposition. Microstructural and compositional analyses were carried out using FESEM, TEM, HRTEM and XRD. Magnetic measurements were performed from in the temperature range 5-300 K. A strong diamagnetic contribution, which results from the polycarbonate template, was found to show s-shape behavior of the hysteresis loops of the nanowires. The coercivity of the samples was found to increase with the decreasing temperature following simple model of thermal activation of particle's moment over the anisotropy barrier in the temperature range 50-300 K. Saturation magnetization was found to increase with decreasing temperature following the modified Bloch's law at low temperatures.

  4. A HRTEM study on serpentinized peridotite from the Southwest Indian Ridge and implications for the deep ocean hydrothermal system

    NASA Astrophysics Data System (ADS)

    Chen, T.; Jin, Z.; Li, W.; Li, H.

    2013-12-01

    Abyssal peridotites generate at mid-ocean ridges. Along the Earth's mid-ocean ridges, abyssal peridotites undergo hydration reactions to become serpentinite minerals, especially in slow to ultraslow spreading mid-ocean ridges. The Southwest Indian Ridge (SWIR) is one of the two ultraslow spreading ridges in the world. The studied serpentinized peridotite sample was collected by the 21st Voyage of the Chinese oceanic research ship Dayang Yihao (aka Ocean No. 1) from a hydrothermal field (63.5°E, 28.0°S, and 3660 m deep) in SWIR. Serpentinized reaction has attracted increasing attention as they are an expression of mantle hydration and water cycles in the deep Earth. There are three main types of serpentinite, antigorite (forms at T > 300°c ), lizadite (forms at T < 200°c ), and chrysotile (forms at intermediate temperatures) [1]. The mineral assemblages of the SWIR serpentinized peridotite was determined by petrography and XRD techniques, which comprises lizardite, chrysotile, olivine, orthopyroxene, clinopyroxene, spinel, magnetite, and chlorite. From SEM and TEM study, serpentinized olivine and orthopyroxene were found changed to chrysotile. However, seldom lizadite was found coexisting with chrysotile in clinopyroxene. From nanobeam SAED and HRTEM analysis, it was observed that the topological structure between lizadite and clinopyroxene is [100]cpx//[001]liz, while there is no topological relationship between chrysotile and clinopyroxene. A little chlorite was observed in serpentine vein, and some nanometer-sized amphibole was observed existing at the side of serpentine vein with [100]cpx//[001]amp. Chrysotile is the dominant serpentine mineral composition in this sample, which is different from most seafloor serpentinized peridotite [2]. The coexistence of chrysotile and lizadite indicates hydration temperature below 300°c , while the existence of chlorite and amphibole suggest hydration temperature reaching greenschist facies conditions, i.e. above 300°c, in the east part of SWIR [1, 2]. Acknowledgments: This work was supported by NSFC (41172050) and CSC. The electron microscopy was accomplished at the Electron Microscopy Center at Argonne National Laboratory, a U.S. Department of Energy Office of Science Laboratory operated under Contract No. DE-AC02-06CH11357 by UChicago Argonne, LLC. References [1] O'Hanley, D.S. Serpentinites. 1984. [2] Mével, C., Geoscience, 335:825, 2003.

  5. Study on immobilization of yeast alcohol dehydrogenase on nanocrystalline Ni-Co ferrites as magnetic support.

    PubMed

    Shakir, Mohammad; Nasir, Zeba; Khan, Mohd Shoeb; Lutfullah; Alam, Md Fazle; Younus, Hina; Al-Resayes, Saud Ibrahim

    2015-01-01

    The covalent binding of yeast alcohol dehydrogenase (YADH) enzyme complex in a series of magnetic crystalline Ni-Co nanoferrites, synthesized via sol-gel auto combustion technique was investigated. The structural analysis, morphology and magnetic properties of Ni-Co nanoferrites were determined by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), vibrating-sample magnetometer (VSM), high resolution transmission electron microscopy (HRTEM) and Fourier transform infrared spectroscopy (FTIR). The comparative analysis of the HRTEM micrographs of bare magnetic nanoferrite particles and particles immobilized with enzyme revealed an uniform distribution of the particles in both the cases without undergoing change in the size which was found to be in the range 20-30 nm. The binding of YADH to Ni-Co nanoferrites and the possible binding mechanism have been suggested by comparing the FTIR results. The binding properties of the immobilized YADH enzyme were also studied by kinetic parameters, optimum operational pH, temperature, thermal stability and reusability. The immobilized YADH exhibits enhanced thermal stability as compared to the free enzyme over a wide range of temperature and pH, and showed good durability after recovery by magnetic separation for repeated use. PMID:25450541

  6. Highly efficient removal of pathogenic bacteria with magnetic graphene composite.

    PubMed

    Zhan, Sihui; Zhu, Dandan; Ma, Shuanglong; Yu, Wenchao; Jia, Yanan; Li, Yi; Yu, Hongbing; Shen, Zhiqiang

    2015-02-25

    Magnetic Fe3O4/graphene composite (abbreviated as G-Fe3O4) was synthesized successfully by solvothermal method to effectively remove both bacteriophage and bacteria in water, which was tested by HRTEM, XRD, BET, XPS, FTIR, CV, magnetic property and zeta-potential measurements. Based on the result of HRTEM, the single-sheet structure of graphene oxide and the monodisperse Fe3O4 nanoparticles on the surface of graphene can be observed obviously. The G-Fe3O4 composite were attractive for removing a wide range of pathogens including not only bacteriophage ms2, but also various bacteria such as S. aureus, E. coli, Salmonella, E. Faecium, E. faecalis, and Shigella. The removal efficiency of E. coli for G-Fe3O4 composite can achieve 93.09%, whereas it is only 54.97% with pure Fe3O4 nanoparticles. Moreover, a detailed verification test of real water samples was conducted and the removal efficiency of bacteria in real water samples with G-Fe3O4 composite can also reach 94.8%. PMID:25634911

  7. 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.

  8. Transport and magnetic properties of cobalt disulfide prepared by solid state hybrid microwave heating and hot pressing

    NASA Astrophysics Data System (ADS)

    Ouyang, Ting; Xie, Mianyu; Shi, Yunfeng; Chen, Bing; Lan, Yu; Yue, Song

    2015-07-01

    In this study, single phase cobalt disulfide (CoS2) was synthesized by temperature-controlled solid state hybrid microwave heating. The structure, composition and morphology of the obtained samples were studied using X-ray diffraction (XRD), scanning electron spectroscopy (SEM), energy dispersive X-ray spectroscopy (EDX) and high resolution transmission electron microscopy (HRTEM), respectively. The loose CoS2 polycrystalline precursor was then hot pressed to dense bulk sample. The subsequent transport and magnetic properties measurements reveal the ferromagnetic Curie temperature at the magnetic transition near 128 K. These results suggest that the magnetic transition in CoS2 is susceptible to the preparation conditions and the microstructure of the samples.

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

    NASA Astrophysics Data System (ADS)

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

    2014-12-01

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

  10. Synthesis, characterization and magnetic properties of hematite (α-Fe2O3) nanoparticles on polysaccharide templates and their antibacterial activity

    NASA Astrophysics Data System (ADS)

    Rafi, M. Mohamed; Ahmed, K. Syed Zameer; Nazeer, K. Prem; Siva Kumar, D.; Thamilselvan, M.

    2015-04-01

    The present study is to synthesize iron oxide nanoparticles on different polysaccharide templates calcined at controlled temperature, characterizing them for spectroscopic and magnetic studies leading to evaluate their antibacterial property. The synthesized iron oxide nanoparticles were characterized by X-ray diffractometer (XRD), Fourier transform infrared spectroscopy, high resolution scanning electron microscopy (HRSEM), high resolution transmission electron microscopy (HRTEM) and vibrating sample magnetometer. The iron oxide nanoparticles were tested for antibacterial activity against gram-positive and gram-negative bacterial species. The XRD confirms the crystalline nature of iron oxide nanoparticles with the mean crystallite size of 10 nm. The functional groups of the synthesized iron oxide nanoparticles were 547, 543 and 544 cm-1 characterizing the Fe-O and the broad bands at 3,398, 3,439 and 3,427 cm-1 were attributed to the stretching vibrations of hydroxyl group absorbed by iron oxide nanoparticles. HRTEM analyses revealed that the average particle size of the hematite nanoparticles are about 85, 92 and 77 nm for AF, DF and GF, respectively, which was a coincident with the results obtained from the HRSEM analysis. Magnetic measurement exhibited ferromagnetic behavior of the α-Fe2O3 at the room temperature with higher coercivity of H C = 2,303, 2,333 and 1,019 Oe for AF, DF and GF, respectively. Antibacterial test showed the inhibition against Aeromonas hydrophila and Escherichia coli with significant antagonistic activity.

  11. 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.

  12. 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.

  13. HRTEM study of oxide nanoparticles in K3-ODS ferritic steel developed for radiation tolerance

    NASA Astrophysics Data System (ADS)

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

    2011-02-01

    Crystal and interfacial structures of oxide nanoparticles and radiation damage in 16Cr-4.5Al-0.3Ti-2W-0.37 Y 2O 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 4Al 2O 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 8+ + He +) dual-beam irradiation are briefly addressed.

  14. 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.

  15. 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.

    2014-09-01

    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.

  16. Lipase immobilized on magnetic multi-walled carbon nanotubes.

    PubMed

    Tan, Huishan; Feng, Wei; Ji, Peijun

    2012-07-01

    Magnetic iron oxide nanoparticles were loaded onto the surfaces of multiwalled carbon nanotubes (MWNTs) by the impregnation method. The obtained magnetic nanotubes were characterized with high-resolution transmission electron microscopy (HRTEM), X-ray photoelectron spectroscopy (XPS), and X-ray diffraction (XRD). Yarrowia lipolytica lipase was covalently immobilized on the magnetic MWNTs (M-MWNTs). M-MWNT-lipase was characterized with XPS spectra and XRD patterns. The structural change of the immobilized lipase was analyzed through circular dichroism spectroscopy. M-MWNT-lipase was utilized for the resolution of (R, S)-1-phenyl ethanol in the organic solvent of heptane. Compared to the native lipase, the lipase immobilized on M-MWNTs has significantly improved its enzymatic activity for the resolution of (R, S)-1-phenyl ethanol in heptane. M-MWNT-lipase can be easily recovered after catalysis. In addition, the effect of sonication time on the catalytic activity was also investigated. It is found that, up to 30min sonication, the catalysis by M-MWNT-lipase is almost not affected. While, the catalytic activity of the native lipase is decreased with sonication time. PMID:22115533

  17. 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.

  18. Magnetic photocatalysts with a p-n junction: Fe3O4 nanoparticle and FeWO4 nanowire heterostructures

    NASA Astrophysics Data System (ADS)

    Cao, Xuan; Chen, Yan; Jiao, Shihui; Fang, Zhenxing; Xu, Man; Liu, Xu; Li, Lu; Pang, Guangsheng; Feng, Shouhua

    2014-10-01

    Magnetic n-type semiconductor Fe3O4 nanoparticle and p-type semiconductor FeWO4 nanowire heterostructures were successfully synthesized without any surfactants or templates via a facile one-step hydrothermal process at 160 °C. The heterojunction structure and morphology were characterized by X-ray powder diffraction (XRD), transmission electron microscopy (TEM) and high-resolution transmission electron microscopy (HRTEM). Magnetic measurements indicated the coexistence of ferrimagnetic behavior of Fe3O4 and weak antiferromagnetic behavior of FeWO4. The degradation of methylene blue (MB) under UV-Visible light irradiation was studied as a model experiment to evaluate the catalytic activity of the Fe3O4/FeWO4 heterostructure p-n junctions. The decomposition efficiency was 97.1% after one hour UV-Visible irradiation. This magnetic photocatalyst can be easily recovered from the solution using a permanent magnet and redispersed by removing the magnet.Magnetic n-type semiconductor Fe3O4 nanoparticle and p-type semiconductor FeWO4 nanowire heterostructures were successfully synthesized without any surfactants or templates via a facile one-step hydrothermal process at 160 °C. The heterojunction structure and morphology were characterized by X-ray powder diffraction (XRD), transmission electron microscopy (TEM) and high-resolution transmission electron microscopy (HRTEM). Magnetic measurements indicated the coexistence of ferrimagnetic behavior of Fe3O4 and weak antiferromagnetic behavior of FeWO4. The degradation of methylene blue (MB) under UV-Visible light irradiation was studied as a model experiment to evaluate the catalytic activity of the Fe3O4/FeWO4 heterostructure p-n junctions. The decomposition efficiency was 97.1% after one hour UV-Visible irradiation. This magnetic photocatalyst can be easily recovered from the solution using a permanent magnet and redispersed by removing the magnet. Electronic supplementary information (ESI) available: The equation used to calculate the energy band gap, XRD data of the products with various pH values, the SEM image of Fe3O4/FeWO4, and the TEM image of FeWO4 nanowires. See DOI: 10.1039/c4nr03729d

  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. Ceramic Nano-particle/Substrate Interface Bonding Formation Derived from Dynamic Mechanical Force at Room Temperature: HRTEM Examination

    NASA Astrophysics Data System (ADS)

    Yao, Hai-Long; Yang, Guan-Jun; Fan, Sheng-Qiang; Li, Cheng-Xin; Li, Chang-Jiu

    2015-04-01

    The bonding of TiO2 nano-particle/substrate is a critical factor influencing the performance of dye-sensitized solar cells. In order to reveal the bonding properties at TiO2 nano-particle/substrate interface, high-resolution transmission electron microscopy (HRTEM) analysis was adopted to TiO2 coatings prepared by three different approaches. In the HRTEM analysis, the effective bonding mode is allowed to distinguish from the false image overlapping. Results show that large areas of effective bonding between nano-TiO2 particles and the substrate surface formed in the room temperature cold sprayed coating and mechanically pressed coating, while only limited interface areas with the effective bonding were observed in the coating deposited by non-pressed method. These results confirm that both high impact pressure during the room temperature cold spraying and mechanical pressure contribute to the bonding formation at the particle/substrate interface.

  1. 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. PMID:19144257

  2. 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.

  3. Room temperature optical and magnetic properties of polyvinylpyrrolidone capped ZnO nanoparticles

    SciTech Connect

    Chakrabarti, Mahuya; Chakrabarti, Keka R.; Sanyal, D.; Chakrabarti, A.

    2009-09-15

    Defect induced room temperature ferromagnetic properties of polyvinylpyrrolidone (PVP) capped nanocrystalline ZnO samples have been studied. Crystal phase and the lattice parameter of the synthesized nanocrystalline samples have been determined from X-ray diffraction spectra (XRD) and high-resolution transmission electron micrographs (HR-TEM). Room temperature photoluminescence (PL) spectrum for the bare ZnO sample shows a strong band at {approx} 379 nm and another band at {approx} 525 nm. The PL spectra also revealed that the number of oxygen vacancies in the uncapped sample is more than the PVP capped sample. Both sample exhibit ferromagnetic property at room temperature when annealed at 500 deg. C for 3 h, due to the formation of adequate oxygen vacancy related defects. The saturation magnetization for the annealed PVP capped sample is found to be larger compared to that for the uncapped sample.

  4. Dealumination of hexagonal (EMT)/cubic (FAU) zeolite intergrowth materials: A SEM and HRTEM study

    SciTech Connect

    Ohsuna, Tetsu; Watanabe, Denjiro; Terasaki, Osamu; Anderson, M.W.; Carr, S.W.

    1994-12-01

    The aim of this paper is to describe the effects of mild dealumination of the end members (FAU, EMT) and intergrowths produced using crown ethers on the nature of the resultant zeolite. The end members and intergrowths were prepared as described previously and dealuminated according to the following procedure. The intergrowth was prepared from a mixture of crown ethers; 66% 18-crown-6 and 33% 15-crown-5 to give an ordered intergrowth. The zeolites were first calcined to remove the crown ether template (600{degree}C, flowing air, 16 h) and then exchanged with ammonium ions. The zeolite (6 g) was slurried in ammonium acetate solution (450 cm{sup 3}, 0.8 M), and to this was added slowly 15.6 cm{sup 3} of ammonium hexafluorosilicate solution (0.5 M). The mixture was stirred at 75{degree}C for 3 h. The zeolite was collected and carefully washed with water (3 x 100 cm{sup 3}). The dealuminated samples were characterized by {sup 29}Si and {sup 27}Al MAS NMR, X-ray powder diffraction and adsorption measurements. These data indicate that the resultant materials are highly crystalline and showed no signs of structural degradation both in short-range order ({sup 27}Al, {sup 29}Si MAS NMR) and long-range order (XRD). However, the SEM and high-resolution images were particularly informative.

  5. 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).

  6. Chemical characterization of soot particles emitted by Wood-Burning Cook Stoves: A XPS and HRTEM study

    NASA Astrophysics Data System (ADS)

    Carabali, Giovanni; Peralta, Oscar; Castro, Telma; Torres, Ricardo; Ruiz, Gerardo; Molina, Luisa; Saavedra, Isabel

    2014-05-01

    The morphology, microstructure, chemical composition, and electronic structure of soot particles emitted directly from biofuel cook stoves have been studied by high resolution transmission electron microscopy (HRTEM) and X-ray photoelectron spectroscopy (XPS). In order to obtain freshly emitted soot particles, 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 chain. Additionally, the morphology of soot particles was analyzed calculating the border-based fractal dimension (Df). Particles sampled on the first heating stage exhibit complex shapes with high values of Df, which are present as aggregates formed by carbon ceno-spheres. The XPS survey spectrum for soot particles shows that the main particle composition is carbon. We also observed differences in the carbon/oxygen (C/O) ratio of the particles, which probably depends on the combustion process efficiency of each cook-stove analyzed. The XPS C-1s spectra show carbon with two peaks that correspond to sp2 and sp3 hybridization. Also, real-time absorption (?a) and scattering (?s) coefficients of the particles emitted by cook stoves were measured. The trend in ?a and ?s 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.

  7. Rapid microwave-assisted synthesis of PVP-coated ultrasmall gadolinium oxide nanoparticles for magnetic resonance imaging

    NASA Astrophysics Data System (ADS)

    Vahdatkhah, Parisa; Madaah Hosseini, Hamid Reza; Khodaei, Azin; Montazerabadi, Ali Reza; Irajirad, Rasoul; Oghabian, Mohamad Ali; Delavari H., Hamid

    2015-05-01

    Synthesis of polyvinyl pyrrolidone (PVP) coated ultrasmall Gd2O3 nanoparticles (NPs) with enhanced T1-weighted signal intensity and r2/r1 ratio close to unity is performed by a microwave-assisted polyol process. PVP coated Gd2O3NPs with spherical shape and uniform size of 2.5 ± 0.5 nm have been synthesized below 5 min and structure and morphology confirmed by HRTEM, XRD and FTIR. The longitudinal (r1) and transversal relaxation (r2) of Gd2O3NPs is measured by a 3 T MRI scanner. The results showed considerable increasing of relaxivity for Gd2O3NPs in comparison to gadolinium chelates which are commonly used for clinical magnetic resonance imaging. In addition, a mechanism for Gd2O3NPs formation and in situ surface modification of PVP-grafted Gd2O3NPs is proposed.

  8. 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.

  9. Nanostructure investigation of magnetic nanomaterial Ni0.5Zn0.3Cu0.2Fe2O4 synthesized by sol-gel method

    NASA Astrophysics Data System (ADS)

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

    2015-07-01

    Magnetic nanomaterial Ni0.5Zn0.3Cu0.2Fe2O4 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 Ni0.5Zn0.3Cu0.2Fe2O4. 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 Ni0.5Zn0.3Cu0.2Fe2O4 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.

  10. 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.

  11. 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 lamellar domains within relict opal-CT fibers. These findings indicate that the type of transformation mechanism depends upon the primary structural characteristics of the authigenic opaline. varieties that are in turn influenced by the sediment lithology.

  12. RBS/C, HRTEM and HRXRD study of damage accumulation in irradiated SrTiO3

    SciTech Connect

    Jagielski, Jacek; Jozwik, Przemyslaw A.; Jozwik Biala, Iwona; Kovarik, Libor; Arey, Bruce W.; Gaca, J.; Jiang, Weilin

    2013-05-14

    Damage accumulation in argon-irradiated SrTiO3 single crystals has been studied by using combination of Rutherford Backscattering/Channeling (RBS/C), High Resolution Transmission Electron Microscopy (HRTEM) and High Resolution X-Ray Diffraction (HRXRD) techniques. The RBS/C spectra were fitted using McChasy, a Monte Carlo simulation code allowing the quantitative analysis of amorphous-like and dislocation-like types of defects. The results were interpreted by using a Multi-Step Damage Accumulation model which assumes, that the damage accumulation occurs in a series of structural transformations, the defect transformations are triggered by a stress caused by formation of a free volume in the irradiated crystal. This assumption has been confirmed by High Resolution Transmission Electron Microscopy and High Resolution X-Ray Diffraction analysis.

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

    NASA Astrophysics Data System (ADS)

    Singh, Virendra; Agrawal, H. M.

    2012-12-01

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

  14. Relationship Between Structural, Morphological, Optical and Magnetic Properties of Transition Metal (TM)-Doped ZnO Nanostructures Prepared by Microwave-Hydrothermal.

    PubMed

    Ahmed, Faheem; Arshi, Nishat; Anwar, M S; Danish, Rehan; Koo, Bon Heun

    2015-02-01

    In this work, pure and 3% TM (Co, Ni, and Cu)-doped ZnO nanostructures were prepared by microwave-hydrothermal method. The striking similarities between changes in the lattice volume, bandgap energy, morphology and saturation magnetization indicated a strong correlation between these properties. XRD, SAED and HRTEM analyses revealed that all the TM-doped ZnO nano-structures have wurtzite structure and no secondary phase was detected. FESEM and TEM results confirmed a higher aspect ratio and highly crystalline nature of nanostructures. Raman spectra revealed that no defect related mode was observed which indicated that the nanostructures have high quality and negligible defects. The value of bandgap was found to decrease with the increase in atomic number of TM dopants. RTFM was observed in all the TM-doped ZnO nanostructures and the value of Ms and Mr were decreased with TM dopants. PMID:26353673

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

    SciTech Connect

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

    2006-12-31

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

  16. 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.

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

    NASA Technical Reports Server (NTRS)

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

    1992-01-01

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

  18. 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 promising candidate for use in several potential applications including neutron capture therapy (NCT), magnetic hyperthermia, ferrofluids and magnetic resonance imaging (MRI).

  19. Optimization of the MARS-XRD collimator using converging blades

    NASA Astrophysics Data System (ADS)

    Pelliciari, Carlo; Marinangeli, Lucia; Critani, Fabio; Baliva, Antonio; Hutchinson, Ian

    2011-05-01

    Mars-XRD is an X-ray diffractometer developed for the in situ mineralogical analysis of the Martian soil. The main components of the Mars-XRD experiment are: a Fe55 radioactive source, a collimator and a CCD-based detector system. For spectroscopic requirements and quality of the machined micrograin of the sample, the beam section should not be larger then 1 × 10 mm2 at sample distance. The current collimator baseline is based on a two-windows system that uses about 20% of the total source emitting surface. To improve the X-ray flux, we are studying a collimator with converging blades which permits to use the entire source emission and tune the beam section. In order to better estimate the efficiency of this collimator and because of the high number of variables, a C++ program has been written that look for the best blades configuration among billion of combinations. In addition to the collimator configuration, this software simulator gives the sample photons distribution for different angles of the tilt of the source and for each couple of blades. The optimized collimator transmits a flux 30% higher than a system with blades with the same angular aperture and 5 times higher than a two windows collimator. Moreover the target photon distribution is a triangle function well focused on the sample surface instead of an irregular function obtained with the previous system. Higher performances arise with the source perpendicular to the source-sample direction. Thanks to this optimization we expect to strongly improve the resolution of the diffraction pattern which is the main goal of the current activities of the instrument development. This software simulator could be used also for the optimization of collimator system for the other wavelength and applications (e.g. radiotherapy).

  20. Synthesis and optical properties of TiO2-based magnetic nanocomposites

    NASA Astrophysics Data System (ADS)

    Scarisoreanu, M.; Morjan, I.; Fleaca, C.-T.; Morjan, I. P.; Niculescu, A.-M.; Dutu, E.; Badoi, A.; Birjega, R.; Luculescu, C.; Vasile, E.; Danciu, V.; Filoti, G.

    2015-05-01

    Magnetic titania nanoparticles covered/embedded in SiO2 shell/matrix were simultaneously manufactured by the single-step laser pyrolysis. The present study is a continuation of our previous investigations on the TiO2/Fe and TiO2/HMDSO (hexamethyldisiloxane) derived-systems. The aim of this work is to study the synthesis by IR (Infrared) laser pyrolysis of magnetic TiO2 based nanocomposites which implies many concurrent processes induced in the gas phase by the laser radiation. The dependence between characteristic properties and the synthesis parameters was determined by many analytical and complementary methods: XRD (X-ray diffraction) structural analysis, UV-vis (ultraviolet-visible) and EDAX (energy-dispersive X-ray) spectroscopy, TEM and HRTEM (transmission electron microscopy at low and high resolution) analysis and magnetic measurements. The results of analysis indicate the presence of disordered silica, Fe, α-Fe2O3 and mixtures of anatase and rutile phases with mean crystallite dimensions (in the 14-34 nm range) with typical character of diluted magnetic oxide systems and a lower bandgap energy (Eg = 1.85 eV) as compared with TiO2 P25 Degussa sample.

  1. Effect of morphology on the magnetic properties of Gd2O3 nanotubes

    NASA Astrophysics Data System (ADS)

    Paul, Rima; Sen, Pintu; Das, I.

    2016-06-01

    Gadolinium oxide (Gd2O3) nanotubes of micron length and average diameter 100 nm have been synthesized by a controlled template-assisted electrochemical deposition technique. Structure and morphology of the synthesized nanotubes have been well characterized by using microscopy and spectroscopy analyses. HRTEM and XRD analysis revealed the crystalline planes of Gd2O3 nanotubes. Magnetic measurements of the aligned Gd2O3 nanotubes have been performed for both parallel and perpendicular orientations of the magnetic field with respect to the axis of the Gd2O3 nanotube array. Large bifurcation in ZFC-FC over the regime of 2-320 K without any signature of long range magnetic ordering confirms the presence of SPM clusters in Gd2O3 nanotubes. Also, large magnetocaloric effect is observed in the cryogenic temperature regime. No anisotropy is seen at the low temperature region but is found to evolve with temperature and becomes significant ~300 K. These nanotubes can be considered as promising candidates for magnetic refrigeration at cryogenic temperature.

  2. 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.

  3. Mechanism of uranium(VI) uptake by Saccharomyces cerevisiae under environmentally relevant conditions: batch, HRTEM, and FTIR studies.

    PubMed

    Lu, Xia; Zhou, Xiao-jiao; Wang, Tie-shan

    2013-11-15

    Biosorption is of significance for the safety evaluation of high-level nuclear wastes repositories and remediation of radioactive contamination places. Quantitive study and structural characterization of uranium uptake by both live and heat-killed Saccharomyces cerevisiae at environmentally relevant uranium concentration and with different ionic strengths were carried out. Kinetic investigation showed the equilibrium reached within 15 min. In equilibrium studies, pH shift towards neutral indicated release of hydroxyl ions. pH was the most important factor, which partly affected electrostatic interaction between uranyl ions and S. cerevisiae surface. The high ionic strength inhibited biosorption capacity, which can be explained by a competitive reaction between sodium ions and uranyl ions. Heat killing process significantly enhanced biosorption capacity, showing an order of magnitude higher than that of live cells. High resolution transmission electron microscopy (HRTEM) coupled with energy dispersive X-ray (EDX) showed needle-like uranium-phosphate precipitation formed on the cell walls for both live and heat-killed cells. Besides, dark-field micrographs displayed considerable similar uranium-phosphate precipitation presented outside the heat-killed cells. The phosphate released during heat-killing process. FTIR illustrated function groups hydroxyl, carboxyl, phosphate, and amino groups played important role in complexation with uranium. PMID:24041822

  4. Combined HRTEM and Auger spectroscopy evidence for the existence of grain boundary premelting in nickel-doped tungsten

    NASA Astrophysics Data System (ADS)

    Luo, Jian; Gupta, Vivek K.; Yoon, Danghyok; Meyer, Harry M., III

    2006-03-01

    A combined high resolution transmission electron microscopy (HRTEM) and Auger spectroscopy study has revealed the formation of 0.6 nanometer thick, nickel-enriched, "liquid-like" grain boundary (GB) films in Ni-doped W specimens at 95C below the bulk eutectic temperature where the bulk liquid phase is no longer stable [Appl. Phys. Lett. 87, 231902 (2005)]. The stabilization of subeutectic liquid-like grain boundary cores in this model two-component metallic alloy is phenomenologically analogous to the long-sought phenomenon of grain boundary premelting. Despite various macroscopic indications of GB structural transitions, this result, to our knowledge, is the first direct evidence for the existence of such disordered nanostructures at metallic GBs. This observation offers a new explanation to the long-standing mysterious solid-state activated sintering mechanism, where accelerated sintering is attributed to the enhanced diffusion in liquid-like GB layers. This discovery also provides insights to resolve several long-standing controversies, e.g., the mechanisms of Ni-induced abnormal grain growth and GB embrittlement.

  5. HRTEM in protein crystallography

    NASA Astrophysics Data System (ADS)

    Dyson, P. W.; Spargo, A. E. C.; Tulloch, P. A.; Johnson, A. W. S.

    Electron microscopy/diffraction (ED/D) using spot-scan and low-dose imaging has been successfully applied to investigate microcrystals of an alpha-helical coiled-coil protein extracted from ootheca of the praying mantis. Fourier transforms of the images show resolution out to 4 A and can be used to phase the corresponding ED data which shows reflections out to 2 A.

  6. XRD studies of chitin-based polyurethane elastomers.

    PubMed

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

    2008-08-15

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

  7. Au doping effect on the electrical and magnetic properties of Fe3O4 nanoparticles

    NASA Astrophysics Data System (ADS)

    Mahmood, Asif; Ramay, Shahid Mahmood; Al-Zaghayer, Yousef S.; Alhazaa, A. N.; Al Masary, Waheed A.; Atiq, Shahid

    2015-12-01

    Impurities free ferromagnetic Fe3O4 was prepared via sol-gel auto-combustion method and then gold was doped with various concentrations 1, 3 and 5 wt.% using conventional deposition-precipitation method. All samples of Fe3O4 with/without Au doping were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), transmission electron microscopy (TEM) and high-resolution transmission electron microscopy (HRTEM). The room temperature magnetic hysteresis loops of all the samples were measured using a physical property measuring system (PPMS), and the results showed a ferromagnetic behavior at room temperature. The results obtained confirmed the fabrication of magnetite-gold composite nanoparticles. The results showed that the resistance and the magnetic behavior of the samples decrease sharply with the increase of Au concentration indicating semiconducting behavior. The saturation magnetization (Ms) of the bare Fe3O4 sample (94.72 emu/g) is much higher than that (66.78 emu/g) of the 5 wt.% Au-doped Fe3O4 sample.

  8. Structural and magnetic properties of CoFe2O4/NiFe2O4 core/shell nanocomposite prepared by the hydrothermal method

    NASA Astrophysics Data System (ADS)

    Sattar, A. A.; EL-Sayed, H. M.; ALsuqia, Ibrahim

    2015-12-01

    CoFe2O4/NiFe2O4 core/shell magnetic nanocomposite was synthesized by using hydrothermal method.The analysis of XRD indicated the coexistence of CoFe2O4, NiFe2O4as core/shell composite. The core/shell structure of the composite sample has been confirmed by HR-TEM images, EDX and FT-IR measurements. The size of obtained core/shell nanoparticles was 17 nm in core diameter and about 3 nm in shell thickness. The magnetization measurements showed that both the coercive field and the saturation magnetization of the resulting core/shell nanocomposite were slightly decreased compared to those of the CoFe2O4 core but the thermal stability is of the magnetization parameter was enhanced. Furthermore, superparamagnetic phase is established at temperatures higher than the room temperature. The results were discussed in terms of the surface pinning and the magnetic interaction at the interface between the core and shell.

  9. Structural and magnetic properties of magnesium ferrite nanoparticles prepared via EDTA-based sol-gel reaction

    NASA Astrophysics Data System (ADS)

    Hussein, Shaban I.; Elkady, Ashraf S.; Rashad, M. M.; Mostafa, A. G.; Megahid, R. M.

    2015-04-01

    Magnesium ferrite (MgFe2O4) nanoparticles have been prepared, for the first time, by ethylene diamine tetraacetic acid (EDTA)-based sol-gel combustion method. The prepared ferrite system is calcined at 400, 500 and 600 °C. Thermo-gravimetric and differential thermal analysis (TGA-DTA), X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, high resolution transmission electron microscopy (HRTEM) and vibrating sample magnetometry (VSM) were applied for elucidating the structural and magnetic properties of the prepared system. XRD patterns revealed that the prepared system have two spinel MgFe2O4 structures, namely cubic and tetragonal phases that are dependent on calcination temperature (Tc). The crystallite sizes varied from 8.933 to 41.583 nm, and from 1.379 to 292.565 nm for the cubic and tetragonal phases respectively depending on Tc. The deduced lattice parameters for the cubic and (tetragonal) systems are a=8.368, 8.365 and 8.377 and (a=7.011, 5.922, 5.908 and c=6.622, 8.456, 8.364) Å at Tc=400, 500 and 600 °C respectively. While the cation distribution of the cubic phase is found to be mixed spinel and Tc-dependent, it is an inverse spinel in the tetragonal phase where the Fe3+ ions occupy both the tetrahedral A- and octahedral B-sites in almost equal amount; the Mg2+ ions are found to occupy only the B-sites. The HRTEM and selected-area electron diffraction (SAED) revealed the detailed morphology of the nanoparticles, and confirmed their crystalline spinel structure. VSM indicated the existence of an appreciable fraction of superparamagnetic particles at room temperature, with pure superparamagnetic behavior observed for samples calcined at 400 °C. Besides, the magnetic properties are found to change by thermal treatment as a result of the varied phase concentration, cation distribution and lattice parameters. Thus, the new synthesis route used in this study by applying EDTA as an organic precursor for preparing MgFe2O4 nanoparticles at rather low temperatures proved to be efficient in obtaining nanoparticles with favorable structural and magnetic properties. Such properties would qualify them for several potential applications including e.g. in hyperthermia treatment, as contrast agents in magnetic resonance imaging (MRI), and in ferroelastomers technology.

  10. 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.

  11. 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.

  12. Magnetic and morphological properties of CoCu nanowires.

    PubMed

    Thongmee, S; Tang, I Ming

    2014-05-01

    Heterogeneous CoCu nanowires containing different amounts of Co (up to 50% at. wt of Co) are made by electro-deposition (ED) method. CoCu nanowires were grown in AAO templates by varying the current density. The diameter of CoCu nanowires was around 40 nm. Therefore, the growing of CoCu nanowires was compacted with the diameter of AAO templates. The XRD patterns showed that all the CoCu nanowires fabricated via electro-deposition were polycrystalline. At low current density (1.32 mA/cm2), the intensity of Cu (111) peak was very strong. Increasing the current density can be led to increase the intensity of Co (100) peak. High resolution transmission electron microscopy (HRTEM) images of the highest Co content (50%at.) wires showed the existence of layers of polycrystalline heterogeneous CoCu alternating with layers of Cu. The magnetic properties showed that the highest coercivity (7.235 kOe) and squareness (0.754) were found in the unannealed nanowires having the highest Co content. PMID:24734653

  13. 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. PMID:17927999

  14. Interplay of bulk and surface on the magnetic properties of low temperature synthesized nanocrystalline cubic Cu1-xZnxFe2O4 (x=0.00, 0.02, 0.04 and 0.08)

    NASA Astrophysics Data System (ADS)

    Chatterjee, Biplab K.; Dey, Abhishek; Ghosh, Chandan K.; Chattopadhyay, Kalyan K.

    2014-10-01

    Synthesis of Cu1-xZnxFe2O4, (x=0.00, 0.02, 0.04 and 0.08) nanoparticles by a low-temperature combustion method is achieved and its structural and magnetic characterizations are performed. X-ray powder diffraction (XRD) study and high resolution transmission electron microscope (HRTEM) images confirm the formation of single cubic phase of nanocrystalline copper ferrite. The inter-planar spacing (d) and particle size increases with increasing Zn content. Cation distribution of mixed spinel Cu1-xZnxFe2O4 nanoparticles are estimated by Fourier transformed infrared (FTIR) spectroscopy, X-ray photoelectron spectroscopy (XPS) and further verified by 57Fe Mossbauer spectroscopy. Detailed magnetic properties are studied by means of Field Cooled (FC) - Zero Field Cooled (ZFC) magnetization measurements and hysteresis loops at various temperatures by the physical property measurement system (PPMS). A transition from superparamagnetic state to ferrimagnetic state is observed as the Zn concentration increases in Cu1-xZnxFe2O4 nanoparticles. The temperature dependence of intrinsic magnetic parameters, i.e., coercivity (HC), saturation magnetization (MS), effective anisotropy constant (Keff) and paramagnetic susceptibility (?p) of Cu1-xZnxFe2O4 reveals the existence of low-temperature spin-glass-like state, which is more prominent for smaller particles and starts to disappear with increasing Zn concentration.

  15. 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.

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

    SciTech Connect

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

    2008-11-15

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

  17. 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.

  18. 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.

  19. A comparative study of particle size dependency of IR and XRD methods for quartz analysis.

    PubMed

    Bhaskar, R; Li, J; Xu, L

    1994-07-01

    Quartz (SiO2) is considered a probable carcinogen. In order to enforce health and safety standards, techniques that can accurately determine the quartz content of materials are necessary. Currently, two techniques dominate quartz analysis--the infrared (IR) spectrophotometry method and the X-ray diffraction (XRD) method. Unfortunately, there are problems associated with these techniques, such as sample preparation and particle size effect. This study focuses on particle size effect on quartz determination by both IR and XRD. Seven size groups of pure quartz samples, with mean diameters from 1.5 to 20 microns, were used. A set of samples with different quartz masses was prepared for each size group and subjected to both IR and XRD analysis. Two sets of calibration curves, one each from IR and XRD, were obtained. It was found that both IR and XRD methods are size-dependent but in an opposite way. As particle size increases, IR peak height decreases and XRD peak height increases for the same quartz content (mass). Since both methods are particle size-dependent, it is important that the standard quartz sample and samples of interest have similar particle size distributions. Specifically, when coal dust samples are ashed before analysis, the after-ashing particle size distribution should be used. Particle size distribution will change after ashing and it is the after-ashed particles that directly affect the IR and XRD analysis. PMID:8053418

  20. Uniform hollow magnetite spheres: Facile synthesis, growth mechanism, and their magnetic properties

    SciTech Connect

    Zhou, Xing; Zhao, Guizhe; Liu, Yaqing

    2014-11-15

    Highlights: • Uniform Fe{sub 3}O{sub 4} hollow spheres with high saturation magnetization were synthesized through a simple solvothermal process. • Without using any hard templates or external magnetic field. • The as-prepared magnetite hollow spheres exhibit a ferromagnetic behavior with high Ms of ca. 85.9 emu/g at room temperature. • The morphology of Fe{sub 3}O{sub 4} with nanoparticles, hollow, and irregular structures could be adjusted by changing the reactive conditions. - Abstract: Hierarchical porous Fe{sub 3}O{sub 4} hollow spheres with high saturation magnetization were synthesized through a simple solvothermal process in ethylene glycol (EG) in the presence of Tetrabutylammonium chloride (TBAC) and urea. By investigating the effect of reaction temperature, time, the amount of urea, and concentration of iron ion on the formation of hollow spheres, it was proposed that the main formation mechanism of hollow spheres is Ostwald ripening process combined with assembly-then-inside-out evacuation process. Additionally, it is found that the morphology of Fe{sub 3}O{sub 4} with nanoparticles, hollow, and irregular structures could be adjusted by changing the above factors. The resulting products were characterized by means of scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray powder diffraction (XRD), high resolution transmission electron microscopy (HRTEM), energy dispersive X-ray spectroscopy (EDX), and vibrating sample magnetometer (VSM). The hierarchical porous Fe{sub 3}O{sub 4} hollow spheres exhibited enhanced saturation magnetization as compared with Fe{sub 3}O{sub 4} nanoparticles.

  1. Fluorescent and superparamagnetic hybrid quantum clusters for magnetic separation and imaging of cancer cells from blood

    NASA Astrophysics Data System (ADS)

    Durgadas, C. V.; Sharma, Chandra P.; Sreenivasan, K.

    2011-11-01

    We demonstrate here the generation of fluorescent superparamagnetic quantum clusters through a greener aqueous route by fusing highly fluorescent gold clusters with superparamagnetic nanoparticles. We conjugated transferrin onto the hybrid clusters to get cell accessibility and assessed their hemocompatibility and cytotoxicity. The ability of the clusters to selectively remove cancer cell lines (C6 glioma cells) from fluids including blood and the fluorescent imaging of the separated cells is demonstrated. The pattering of the clusters in response to an external magnetic field is also shown. Efficient cancer cell separation, imaging and magnetic pattering can be realized by the highly hemocompatible and noncytotoxic hybrid clusters reported here. It seems the probe has potential for further exploration in multimodal imaging of circulating cancer cells.We demonstrate here the generation of fluorescent superparamagnetic quantum clusters through a greener aqueous route by fusing highly fluorescent gold clusters with superparamagnetic nanoparticles. We conjugated transferrin onto the hybrid clusters to get cell accessibility and assessed their hemocompatibility and cytotoxicity. The ability of the clusters to selectively remove cancer cell lines (C6 glioma cells) from fluids including blood and the fluorescent imaging of the separated cells is demonstrated. The pattering of the clusters in response to an external magnetic field is also shown. Efficient cancer cell separation, imaging and magnetic pattering can be realized by the highly hemocompatible and noncytotoxic hybrid clusters reported here. It seems the probe has potential for further exploration in multimodal imaging of circulating cancer cells. Electronic supplementary information (ESI) available: HRTEM, FTIR spectra, XRD of the samples and fluorescent microscope images are showed in supporting information in the order they discussed in the text. See DOI: 10.1039/c1nr10900f

  2. 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.

  3. 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. PMID:21104235

  4. 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.

  5. In Situ XRD of Thin Film Tin Electrodes for Lithium Ion Batteries

    SciTech Connect

    Rhodes, Kevin J; Meisner, Roberta Ann; Kirkham, Melanie J; Dudney, Nancy J; Daniel, Claus

    2012-01-01

    Thin film electrodes for lithium ion batteries (LIB) poses several attractive advantages over traditional composite electrodes including size and shape constraints, operating temperature range, and volumetric energy density. Tin is an attractive candidate for LIB anode applications due to its exceptional specific capacity, cascading voltage profile, safety, wide availability, and low cost. Tin thin film electrodes were sputtered onto the current collector of a recently developed in situ X-ray diffraction (XRD) and were monitored continuously by XRD while cycling. A phase transformation from white tin, to Li2Sn5, to -LiSn, to Li22Sn5 was observed during lithiation with the same phases detected in reverse order during delithiation. Preferred orientation and crystallite size information for these phases was extracted from the XRD data in order to develop a clearer picture of how lithium enters and exits thin film tin electrodes.

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

    NASA Technical Reports Server (NTRS)

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

    2004-01-01

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

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

    SciTech Connect

    Don Pellinen and Michael Griffin

    2009-01-23

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

  8. 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.

  9. Magnetic

    NASA Astrophysics Data System (ADS)

    Aboud, Essam; El-Masry, Nabil; Qaddah, Atef; Alqahtani, Faisal; Moufti, Mohammed R. H.

    2015-06-01

    The Rahat volcanic field represents one of the widely distributed Cenozoic volcanic fields across the western regions of the Arabian Peninsula. Its human significance stems from the fact that its northern fringes, where the historical eruption of 1256 A.D. took place, are very close to the holy city of Al-Madinah Al-Monawarah. In the present work, we analyzed aeromagnetic data from the northern part of Rahat volcanic field as well as carried out a ground gravity survey. A joint interpretation and inversion of gravity and magnetic data were used to estimate the thickness of the lava flows, delineate the subsurface structures of the study area, and estimate the depth to basement using various geophysical methods, such as Tilt Derivative, Euler Deconvolution and 2D modeling inversion. Results indicated that the thickness of the lava flows in the study area ranges between 100 m (above Sea Level) at the eastern and western boundaries of Rahat Volcanic field and getting deeper at the middle as 300-500 m. It also showed that, major structural trend is in the NW direction (Red Sea trend) with some minor trends in EW direction.

  10. 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.

  11. 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.

  12. 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.

  13. 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.

  14. XRD, SEM and infrared study into the intercalation of sodium hexadecyl sulfate (SHS) into hydrocalumite.

    PubMed

    Zhang, Ping; Wang, Tianqi; Zhang, Longlong; Wu, Daishe; Frost, Ray L

    2015-12-01

    Hydrocalumite (CaAl-LDH-Cl) interacted with a natural anionic surfactant, sodium hexadecyl sulfate (SHS), was performed using an intercalation method. To understand the intercalation behavior and characterize the resulting products, powder X-ray diffraction (XRD), scan electron microscopy (SEM) and mid-infrared (MIR) spectroscopy combined with near-infrared (NIR) spectroscopy technique were used. The XRD analysis indicated that SHS was intercalated into CaAl-LDH-Cl successfully, resulting in an expansion of the interlayer (from 0.78 nm to 2.74 nm). The bands of C-H stretching vibrations of SHS were observed in the near-infrared spectra, which indicated that the resulting products were indeed CaAl-LDH-SHS. In addition, the bands of water stretching vibrations and OH groups shifted to higher wavenumbers when SHS was intercalated into CaAl-LDH-Cl interlayer space. PMID:26163791

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

    NASA Astrophysics Data System (ADS)

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

    2014-11-01

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

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

    SciTech Connect

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

    2014-12-15

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

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

    PubMed

    Ostrooumov, Mikhail

    2009-08-01

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

  18. Quantitative analysis of interfacial strain in InAs/GaSb superlattices by aberration-corrected HRTEM and HAADF-STEM.

    PubMed

    Mahalingam, Krishnamurthy; Haugan, Heather J; Brown, Gail J; Eyink, Kurt G

    2013-04-01

    The strain distribution across interfaces in InAs/GaSb superlattices grown on (100)-GaSb substrates is investigated by aberration corrected transmission electron microscopy. Atomic resolution images of interfaces were obtained by conventional high resolution transmission electron microscopy (HRTEM), using the negative spherical-aberration imaging mode, and by scanning transmission electron microscopy (STEM), using the high-angle annular dark-field (HAADF) imaging mode. The local atomic displacements across interfaces were determined from these images using the peak pair algorithm, from which strain maps were calculated with respect to a reference lattice extracted from the GaSb substrate region. Both techniques yield consistent results, which reveal that the InAs-on-GaSb interface is nearly strain balanced, whereas the GaSb-on-InAs interface is in tensile strain, indicating that the prevalent bond type at this interface is Ga-As. In addition, the GaSb layers in the superlattice are compressively strained indicating the incorporation of In into these layers. Further analysis of the HAADF-STEM images indicates an estimated 4% In content in the GaSb layers and that the GaSb-on-InAs interface contributes to about 27% of the overall superlattice strain. The strain measurements in the InAs layers are in good agreement with the theoretical values determined from elastic constants. Furthermore, the overall superlattice strain determined from this analysis is also in good agreement with the measurements determined by high-resolution X-ray diffraction. PMID:23298538

  19. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2016-05-01

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

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

    PubMed

    Ostrooumov, Mikhail; Hernández-Bernal, Maria del Sol

    2011-12-01

    The Raman (RMP), infrared (IR) and XRD analysis have been applied to the examination of mineralogical composition of El Pozo meteorite (an ordinary chondrite L5 type; village Valle of Allende, founded in State of Chihuahua, Mexico: 26°56'N and 105°24'W, 1998). RMP measurements in the range of 100-3500 cm(-1) revealed principal characteristic bands of the major minerals: olivine, two polymorph modifications of pyroxene (OPx and CPx) and plagioclase. Some bands of the minor minerals (hematite and goethite) were also identified. All these minerals were clearly distinguished using IR and XRD techniques. XRD technique has shown the presence of some metallic phases such as kamacite and taenite as well as troilite and chromite. These minerals do not have characteristic Raman spectra because Fe-Ni metals have no active modes for Raman spectroscopy and troilite is a weak Raman scatterer. Raman mapping microspectroscopy was a key part in the investigation of El Pozo meteorite's spatial distribution of the main minerals because these samples are structurally and chemically complex and heterogeneous. The mineral mapping by Raman spectroscopy has provided information for a certain spatial region on which a spatial distribution coexists of the three typical mineral assemblages: olivine; olivine+orthopyroxene; and orthopyroxene. PMID:21930423

  2. In-Situ Cold Temperature XRD of Calcium Phosphate Produced From Organic Phosphoric Acid

    NASA Astrophysics Data System (ADS)

    Yusoff, M. S. Meor; Paulus, Wilfred; Muslimin, Masliana

    2010-01-01

    In this study, we synthesized calcium phosphate from an organic phosphoric acid, diethylhexyl phosphoric acid (DEHPA) and calcium hydroxide solution. The reaction involves a sol-gel process with a whitish gel formed. In-situ XRD analysis was then performed on the sample from room temperature to -140° C. At room the XRD diffractogram shows the sample as an amorphous material and as the temperature was further lowered sharp peaks begins to form indicating that the material had becomes crystalline. The peaks were identified to be that calcium hydrogen phosphate (Ca(H2PO4)2) and this indicates that there is no hydroxyl group removal during the cooling process. The relative crystallinity values obtained for the different cooling temperatures show a slow exponential increase on the initial cooling of 0 to -100° C and at further cooling temperatures resulted fast and linear process. Also unlike the in-situ XRD analysis performs at high temperature no phase transformation occurred at this low temperature.

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

    NASA Astrophysics Data System (ADS)

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

    2013-06-01

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

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

    NASA Astrophysics Data System (ADS)

    Debelle, Aurélien; Declémy, Alain

    2010-05-01

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

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

    PubMed

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

    2014-09-01

    The recent discovery of conditions that induce nanoribbon structures of amelogenin protein in vitro raises questions about their role in enamel formation. Nanoribbons of recombinant human full-length amelogenin (rH174) are about 17 nm wide and self-align into parallel bundles; thus, they could act as templates for crystallization of nanofibrous apatite comprising dental enamel. Here we analyzed the secondary structures of nanoribbon amelogenin by x-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) and tested if the structural motif matches previous data on the organic matrix of enamel. XRD analysis showed that a peak corresponding to 4.7 Å is present in nanoribbons of amelogenin. In addition, FTIR analysis showed that amelogenin in the form of nanoribbons was comprised of β-sheets by up to 75%, while amelogenin nanospheres had predominantly random-coil structure. The observation of a 4.7-Å XRD spacing confirms the presence of β-sheets and illustrates structural parallels between the in vitro assemblies and structural motifs in developing enamel. PMID:25048248

  6. Matching 4.7-Å XRD Spacing in Amelogenin Nanoribbons and Enamel Matrix

    PubMed Central

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

    2014-01-01

    The recent discovery of conditions that induce nanoribbon structures of amelogenin protein in vitro raises questions about their role in enamel formation. Nanoribbons of recombinant human full-length amelogenin (rH174) are about 17 nm wide and self-align into parallel bundles; thus, they could act as templates for crystallization of nanofibrous apatite comprising dental enamel. Here we analyzed the secondary structures of nanoribbon amelogenin by x-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) and tested if the structural motif matches previous data on the organic matrix of enamel. XRD analysis showed that a peak corresponding to 4.7 Å is present in nanoribbons of amelogenin. In addition, FTIR analysis showed that amelogenin in the form of nanoribbons was comprised of β-sheets by up to 75%, while amelogenin nanospheres had predominantly random-coil structure. The observation of a 4.7-Å XRD spacing confirms the presence of β-sheets and illustrates structural parallels between the in vitro assemblies and structural motifs in developing enamel. PMID:25048248

  7. A Simple Combustion Synthesis and Optical Studies of Magnetic Zn1-xNi(x)Fe2O4 Nanostructures for Photoelectrochemical Applications.

    PubMed

    Manikandan, A; Antony, S Arul; Sridhar, R; Ramakrishna, Seeram; Bououdina, M

    2015-07-01

    Ni-doped ZnFe2O4 (Ni(X)Zn1-x,Fe2O4; x = 0.0 to 0.5) nanoparticles were synthesized by simple microwave combustion method. The X-ray diffraction (XRD) confirms that all compositions crystallize with cubic spinel ZnFe2O4. The lattice parameter decreases with increase in Ni content resulting in the reduction of lattice strain. High resolution scanning electron microscope (HR-SEM) and transmission electron microscope (HR-TEM) images revealed that the as-prepared samples are crystalline with particle size distribution in 42-50 nm range. Optical properties were determined by UV-Visible diffuse reflectance (DRS) and photoluminescence (PL) spectroscopy respectively. The saturation magnetization (Ms) shows the superparamagnetic nature of the sample for x = 0.0-0.2, whereas for x = 0.3-0.5, it shows ferromagnetic nature. The Ms value is 1.638 emu/g for pure ZnFe2O4 sample and it increases with increase in Ni content. Photoelectrochemical (PEC) measurements showed a significant increase of photocurrent density with increase in the Ni-dopant, and 0.5% Ni-doped ZnFe2O4 sample was found to show the better photoresponse than the other doping concentrations. PMID:26373061

  8. Highly ordered magnetic mesoporous silicas for effective elimination of carbon monoxide

    SciTech Connect

    Lee, Jiho; Ho Chang, Jeong

    2012-04-15

    Catalysts based on crystalline nanoparticles of Fe metal supported on mesoporous silica have been developed. The synthetic process involves hydrogen reduction processing for high abundant Fe metal nanoparticles within the mesopores, in which impregnated Fe salt in the inner nanopores of mesoporous silica is thermally treated under hydrogen at 500 Degree-Sign C. Detailed characterization was achieved by XRD, XPS, BET, and HR-TEM techniques. The catalytic efficiency was demonstrated as a function of the used amounts and reaction time. The results show that more than 90% of the carbon monoxide was eliminated at room temperature during a period 80 min with 0.5 g of catalyst. - Graphical abstract: Strategy for the preparation of highly abundant Fe nanoparticle embedded MS catalyst by hydrogen reduction process and HR-TEM images of cross-sectional and top view. Highlights: Black-Right-Pointing-Pointer MS based heterogeneous catalyst with Fe nanoparticles were demonstrated for CO elimination. Black-Right-Pointing-Pointer Highly Fe nanoparticle embedded MS catalyst prepared by hydrogen reduction process. Black-Right-Pointing-Pointer Systematic characterization was achieved by XRD, XPS, BET, and HR-TEM analyses. Black-Right-Pointing-Pointer More than 90% of the CO was eliminated at RT during 80 min with 0.5 g of catalyst.

  9. 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.

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

    PubMed

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

    2014-07-01

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

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

    PubMed

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

    2007-01-01

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

  12. 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.

  13. 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.

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

    NASA Technical Reports Server (NTRS)

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

    1986-01-01

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

  15. 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 the position of its 021 diffraction peak is similar to that reported for John Klein. In both cases, the amorphous component has low SiO2 and MgO and high FeO + Fe2O3, P2O5, and SO3 concentrations relative to bulk sample. The chemical composition of the bulk drill fines and XRD crystalline, smectite, and amorphous components implies alteration of an initially basaltic material under near neutral conditions (not acid sulfate), with the sulfate incorporated later as veins of CaSO4 injected into the mudstone.

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

    SciTech Connect

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

    1995-11-09

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

  17. 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 of its 02l diffraction peak is similar to that reported for John Klein. In both cases, the amorphous component has low SiO2 and MgO and high FeO + Fe2O3, P2O5, and SO3 concentrations relative to bulk sample. The chemical composition of the bulk drill fines and XRD crystalline, smectite, and amorphous components implies alteration of an initially basaltic material under near neutral conditions (not acid sulfate), with the sulfate incorporated later as veins of CaSO4 injected into the mudstone.

  18. 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.

  19. Pressure-induced structural modifications of metagermanates at room temperature : In situ XRD and EXAFS studies

    NASA Astrophysics Data System (ADS)

    Nagai, T.; Ohtaka, O.; Yoshiasa, A.; Yamanaka, T.; Shimomura, O.

    In situ X ray diffraction (XRD) and extended X ray absorption fine structure (EXAFS) measurements under high pressure and at room temperature were performed in order to verify the possibility of a pressure-induced amorphization of MgGeO3-high-clinoenstatite and CaGeO3-wollastonite. We found that the two metagermanates were transformed into new metastable phases without the amorphization. For MgGeO3-high-clinoenstatite, a new reflection, which could not be assigned as its known high-pressure polymorphs, could be observed above 23 GPa. For CaGeO3-wollastonite, EXAFS measurements under high pressure were conducted using MAX90. The observed pressure dependence of the Ge-O distance can suggest the existence of a metastable intermediate phase between wollastonite and perovskite. The intermediate phase corresponds to a rhodonite-like structure, which was proposed by a previous XRD experiments. These transitions, which were observed in the two metagermanates, suggest to be kinetically favored processes under room temperature compression. Such metastable pathways during phase transitions can be described as typical examples of the Ostwald step rule.

  20. 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.

  1. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2010-06-01

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

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

    PubMed

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

    2013-12-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2014-03-01

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

  5. 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.

  6. Copper(0) nanoparticles supported on silica-coated cobalt ferrite magnetic particles: cost effective catalyst in the hydrolysis of ammonia-borane with an exceptional reusability performance.

    PubMed

    Kaya, Murat; Zahmakiran, Mehmet; Ozkar, Saim; Volkan, Mürvet

    2012-08-01

    Herein we report the development of a new and cost-effective nanocomposite catalyst for the hydrolysis of ammonia-borane (NH(3)BH(3)), which is considered to be one of the most promising solid hydrogen carriers because of its high gravimetric hydrogen storage capacity (19.6% wt) and low molecular weight. The new catalyst system consisting of copper nanoparticles supported on magnetic SiO(2)/CoFe(2)O(4) particles was reproducibly prepared by wet-impregnation of Cu(II) ions on SiO(2)/CoFe(2)O(4) followed by in situ reduction of the Cu(II) ions on the surface of magnetic support during the hydrolysis of NH(3)BH(3) and characterized by ICP-MS, XRD, XPS, TEM, HR-TEM and N(2) adsorption-desorption technique. Copper nanoparticles supported on silica coated cobalt(II) ferrite SiO(2)/CoFe(2)O(4) (CuNPs@SCF) act as highly active catalyst in the hydrolysis of ammonia-borane, providing an initial turnover frequency of TOF = 2400 h(-1) at room temperature, which is not only higher than all the non-noble metal catalysts but also higher than the majority of the noble metal based homogeneous and heterogeneous catalysts employed in the same reaction. More importantly, they were easily recovered by using a permanent magnet in the reactor wall and reused for up to 10 recycles without losing their inherent catalytic activity significantly, which demonstrates the exceptional reusability of the CuNPs@SCF catalyst. PMID:22856878

  7. 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.

  8. 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.

  9. 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.

  10. DTA, powder XRD and SEM study of manganese-containing borate glasses

    SciTech Connect

    Shah, J.G.; Patki, V.A.; Raj, K.; Rao, U.R.K.

    1995-12-31

    Fixing in glass is one of the accepted modes of radioactive waste immobilization adopted all over the world. Several homogeneous glasses in the ternary SiO{sub 2}/B{sub 2}O{sub 3}/Na{sub 2}O containing MnO{sub 2} were investigated by powder XRD, DTA and SEM. The presence of a crystalline Mn{sub 7}SiO{sub 12} phase in the glasses which contain more than 20 mol% of MnO{sub 2} is confirmed. The crystalline compound could be synthesized in a pure form at 1,000 C at ambient pressure. No other crystalline phase in the ternary Si-Mn-O was detected in the otherwise homogeneous glass.

  11. 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.

  12. XRD analysis of undoped and Fe doped TiO2 nanoparticles by Williamson Hall method

    NASA Astrophysics Data System (ADS)

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

    2015-08-01

    Undoped and Fe doped titanium dioxide (TiO2) 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 TiO2 and Fe doped TiO2 nanoparticles were calculated by Scherer's formula, and was found to be 15 nm and 11 nm, respectively. Reduction in crystallite size of TiO2 with Fe doping was observed. The anatase phase of Fe-doped TiO2 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 TiO2 and tensile strain for Fe-TiO2 nanoparticles annealed at 500°C.

  13. Fabrication of hybrid magnetic Sr5xBa3x(PO4)3(OH)/Fe3O4 nanorod and its highly efficient adsorption performance for acid fuchsin dye

    NASA Astrophysics Data System (ADS)

    Yin, Xiaoju; Zhang, Fan; Zhang, Weihua

    2015-12-01

    The hybrid magnetic Sr5xBa3x(PO4)3(OH)/Fe3O4 (SBPF) nanorod was prepared and characterized using different techniques, such as SEM, EDS, TEM, SAED, HRTEM, XRD, and FT-IR. Adsorption studies of acid fuchsin (AF) from aqueous solution with respect to the pH, temperature, time, initial dye concentration, and sorbent dosage were investigated. The Freundlich adsorption model was applied to describe the equilibrium isotherms. The maximal AF uptake by SBPF was 1590 mg/g in the test. Kinetics parameters of the adsorption process indicated that it followed the pseudo-second order equation, and the maximum sorption capacity calculated from the pseudo-second-order rate equation was 909 mg/g which was close to the experimental value. Adsorption thermodynamics study indicated the spontaneous nature and exothermic of the adsorption process. The removal of AF was attributed to the hydrogen bond and ionic interactions. Moreover, SBPF was easily recovered, and the adsorption capacity was approximately 97.7% of the initial saturation adsorption capacity after being used five times.

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

    PubMed

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

    2015-11-28

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

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

    PubMed

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

    2015-09-21

    A series of mixed Mn-Zr oxides with different molar ratios Mn/Zr (0.1-9) have been prepared by coprecipitation of manganese and zirconium nitrates and characterized by X-ray diffraction (XRD) and BET methods. It has been found that at concentrations of Mn below 30 at%, the samples are single-phase solid solutions (MnxZr1-xO2-δ) based on a ZrO2 structure. X-ray photoelectron spectroscopy (XPS) measurements showed that manganese in these solutions exists mainly in the Mn(4+) state on the surface. An increase in Mn content mostly leads to an increase in the number of Mn cations in the structure of solid solutions; however, a part of the manganese cations form Mn2O3 and Mn3O4 in the crystalline and amorphous states. The reduction of these oxides with hydrogen was studied by a temperature-programmed reduction technique, in situ XRD, and near ambient pressure XPS in the temperature range from 100 to 650 °C. It was shown that the reduction of the solid solutions MnxZr1-xO2-δ proceeds via two stages. During the first stage, at temperatures between 100 and 500 °C, the Mn cations incorporated into the solid solutions MnxZr1-xO2-δ undergo partial reduction. During the second stage, at temperatures between 500 and 700 °C, Mn cations segregate on the surface of the solid solution. In the samples with more than 30 at% Mn, the reduction of manganese oxides was observed: Mn2O3 → Mn3O4 → MnO. PMID:26239114

  16. 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 Brnsted acid concentration decreases but this metal ion exchange does not totally remove Brnsted 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 Brnsted 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 of the zeolite catalysts during reaction since their catalytic performance was retained after use.

  17. 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.

  18. Coupling XRD, EXAFS, and 13C NMR to study the effect of the carbon stoichiometry on the local structure of UC(1±x).

    PubMed

    Carvajal Nuñez, U; Martel, L; Prieur, D; Lopez Honorato, E; Eloirdi, R; Farnan, I; Vitova, T; Somers, J

    2013-10-01

    A series of uranium carbide samples, prepared by arc melting with a C/U ratio ranging from 0.96 to 1.04, has been studied by X-ray diffraction (XRD), (13)C nuclear magnetic resonance (NMR), and extended X-ray absorption fine structure (EXAFS). XRD determines phase uniqueness and the increase of the lattice parameter versus the carbon content. In contrast, (13)C NMR detects the different carbon environments in the lattice and in this study, clearly identifies the presence of discrete peaks for carbon in the octahedral lattice site in UC and an additional peak associated with excess carbon in hyperstoichiometric samples. Two peaks associated with different levels of carbon deficiency are detected for all hypostoichiometric compositions. More than one carbon environment is always detected by (13)C NMR. This exemplifies the difficulty in obtaining a perfect stoichiometric uranium monocarbide UC(1.00). The (13)C MAS spectra of uranium carbides exhibit the effects resulting from the carbon content on both the broadening of the peaks and on the Knight shift. An abrupt spectral change occurs between hypo- and hyperstoichiometric samples. The results obtained by EXAFS highlight subtle differences between the different stoichiometries, and in the hyperstoichiometric samples, the EXAFS results are consistent with the excess carbon atoms being in the tetrahedral interstitial position. PMID:24063301

  19. 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 synthetic diffraction data to estimate detection limits as a function of resolution and count times; and (d) trade-off studies of synthetic multilayer optics versus crystal monochromators. We will also report on environmental factors which affect (both positively and negatively) the likely instrument performance, including sample and atmosphere X-ray attenuation lengths. Summary: The proposed IMPs will be able to identify any crystalline substances (including organic polymers) present on Titan's surface at > 1 wt % levels, and quantify their relative abundance [2,3], as well as, in principle, estimate the abundance of any amorphous material. The focusing geometry maximises the flux and resolution obtainable from radioisotope sources and also has the advantage of illuminating a relatively large sample volume (compared to other mini-XRD designs); this improves the measured powder statistics. Most of the mass, and all of the power use is confined to the detector system (which is cooled passively by Titan's atmosphere) and data rates will be very small. The robustness of the technique renders it the method of choice for unambiguous determination of Titan's surface mineralogy. References: [1] Coustenis, A., et al. (2008) paper in press Astrophys. Instr. Methods. [2] Rietveld, H. (1969) J. Appl. Cryst. 2, 65-71. [3] Hill, R. J. & C. J. Howard (1987) J. Appl. Cryst. 20, 467-474.

  20. 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 composition was not observed when the treatment was analyzed individually or when analyzed under the possible synergic effect with other treatments. However, the radiation dose to which specimens were exposed is only a fraction of the accumulated dose in cement paste until complete decay of some sources. Therefore, in the short term, the conditions deemed to prevail in the repository environment may not influence the properties of cement paste at detectable levels. Under the conditions presented in this work, it is not possible to predict the long term evolution of these properties. (authors)

  1. 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 <150 microns, and delivered to instruments in the body of the rover. A drilled sample of sediment in outcrop is anticipated. At the time of writing this abstract, promising outcrops are in range and this talk will provide an update on data collected with the CheMin instrument.

  2. Synthesis, XRD characterization and electrochemical performance of overlithiated LiNiO 2

    NASA Astrophysics Data System (ADS)

    Moshtev, R.; Zlatilova, P.; Vasilev, S.; Bakalova, I.; Kozawa, A.

    The synthesis and XRD characterization of overlithiated LiNiO 2 samples is briefly described. The effect of the extraction of the residual LiOH from the samples after their synthesis is studied. The extraction in water even at a low liquid/solid ratio leads to a considerable chemical delithiation accompanied by the loss of oxygen from the crystal lattice of LiNiO 2. It is supposed that oxygen vacancies are formed in part of the NiO 6 octahedra. The defective octahedra cannot release electrons whereby the number of Li + which can be deintercalated during the electrochemical delithiation of the cathodes prepared with chemically delithiated LiNiO 2 samples are reduced. Although the fast XRD characterization here employed shows negligible change in the criterial parameters, the cycling test reveals a considerable decrease in the charge capacity and consequently in the next discharge capacity. The change in the crystal structure of the water extracted samples is more clearly observed in the VA-grams showing a considerable shift of the first R 1/M peaks in anodic direction and a strong reduction in the areas of the R 2/R 3 peaks. Ethanol as a nonaqueous solvent was found to extract the residual LiOH without causing any chemical delithiation of the LiNiO 2 samples, thus, preserving their good electrochemical characteristics. The effect of storage of the LiNiO 2 powdered samples in the ambient atmosphere was investigated. The results revealed that the ethanol extracted samples are more resistant to chemical delithiation by the water vapours in the air than those containing residual LiOH. A beneficial effect on the cycling characteristics of LiNiO 2 cathodes containing 10% of the newly developed UFC (ultra-fine carbon) conductive material is established. The cycling by potentiostatic charging to 4.20 V with initial limited current of 60 mA/g was found to contribute substantially to the discharge capacity and cycling stability of the LiNiO 2 cathodes, yielding more than 170 mA h/g after 50 cycles between 3.00 and 4.20 V.

  3. 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.

  4. 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.

  5. In-situ XRD Investigations of the Solid--state Synthesis of Doped Thermoelectric Cobalt Oxides

    NASA Astrophysics Data System (ADS)

    Chen, Haiyan; Bai, Jianming; Tyson, Trevor

    2010-03-01

    Thermoelectric materials are important in converting waste heat into electricity or electrical power directly into cooling or heating. Calcium cobalt oxide has been shown to posses large figure of merit and is considered an excellent candidate for high temperature thermoelectric applications. Doping with other metal oxides is one way to improve thermoelectric properties of this family of materials. To understand the synthesis of these materials, we have carried out time resolved in-situ XRD study of the solid state reactions involved in the production of calcium cobalt oxide and doped calcium cobalt oxide from metal carbonate and metal oxides. In this presentation, observed phase transitions, intermediates, and phase evolutions will be reported and discussed. These results will be helpful in the understanding of reaction mechanisms and can provide insights into the doping mechanism involved in the improvement of the thermoelectric characteristics of calcium cobalt oxides. This work is supported by DOE Grant DE-FG02-07ER46402 and NSF Instrumentation grant DMR MRI-0722730.

  6. 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.

  7. 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)

  8. 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.

  9. Investigation by XRF and XRD of Zn and Fe in Fex Zn1-x thin films

    NASA Astrophysics Data System (ADS)

    Söğüt, Ö.; Bütün, H.; Karahan, İ. H.; Tıraşoğlu, E.; Apaydın, G.

    2008-12-01

    FexZn1-x alloys were electrochemically deposited on aluminum substrates from a sulfate bath. The Kβ/Kα x-ray intensity ratios of Zn and Fe in FexZn1-x thin films have been experimentally studied. The energy dispersive x-ray fluorescence (EDXRF) technique was used to measure K x-ray photons. Samples were excited by using 59.5 keV photons emitted by a 50 mCi 241Am radioactive source. The emitted K x-rays were detected by an Ultra-LEGe detector having a resolution of 150 eV at 5.9 keV. In addition, the effect of bath composition on the phase structure was investigated by x-ray diffraction (XRD) analysis. The composition of the thin films was analyzed by atomic absorption spectrometry analysis. Iron content was shown to strongly affect the structure of Zn-Fe alloys. It was found that the K-shell x-ray intensity ratio changed in FexZn1-x thin films for different values of x. The reason for this change may be that the electronegativity of iron is higher than that of zinc and that electron transfer from zinc to the outermost orbital of iron occurs. In conclusion, in FexZn1-x thin films, intensity ratio increases with increasing concentration of Zn but decreases with increasing concentration of Fe.

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

    PubMed

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

    2014-12-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2011-11-01

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

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

    PubMed

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

    2012-12-01

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

  13. 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.

  14. 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.

  15. 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.

  16. 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.

  17. 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 primary slits of Max80 were exchanged by 4-blade high precision slits of Advanced Design Consulting, Inc. Some recent results on the non-quenchable high-P AƒA_A,A¿A,A 1/2 low-P clinoenstatite transition and to the quartz-coesite transition will be given to discuss the different interferometric techniques, including the XRD-data and X-radiography results, necessary to detect the phase transitions under in situ conditions and to measure the sample deformation. Li, B.; Chen, K.; Kung, J.; Liebermann, R.C.; Weidner, D.J., J. Phys.: Condens. Matter 14, 11337-11342, (2002). Mueller, H.J.; Lathe, C.; Wunder, B., In: J. Chen, Y. Wang, T. Duffy, G. Shen, L. Dobrzhinetskaya (eds.), Frontiers in High Pressure Research, Elsevier Science, submitted, (2004a). Mueller, H.J.; Schilling, F.R.; Lathe, C.; Lauterjung, J., In: J. Chen, Y. Wang, T. Duffy, G. Shen, L. Dobrzhinetskaya (eds.), Frontiers in High Pressure Research, Elsevier Science, in press, (2004b).

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

    NASA Astrophysics Data System (ADS)

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

    2014-05-01

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

  19. 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.

  20. 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.

  1. New magnetic nanoparticles for biotechnology.

    PubMed

    Hütten, Andreas; Sudfeld, Daniela; Ennen, Inga; Reiss, Günter; Hachmann, Wiebke; Heinzmann, Ulrich; Wojczykowski, Klaus; Jutzi, Peter; Saikaly, Wahib; Thomas, Gareth

    2004-08-26

    Paramagnetic carriers, which are linked to antibodies enable highly specific biological cell separations. With the colloidal synthesis of superparamagnetic Co and FeCo nanocrystals with superior magnetic moments the question about their potential to replace magnetite as the magnetically responsive component of magnetic beads is addressed. Starting from a magnetic analysis of the corresponding magnetophoretic mobility of Co and FeCo based alloys their synthesis and resulting microstructural and magnetic properties as function of the underlying particle size distribution are discussed in detail. The stability of the oleic acid ligand of Co nanocrystals has been investigated. The oxidation kinetics were quantified using magnetic measurements. As a result, this ligand system provides sufficient protection against oxidation. Furthermore, the kinetics of the synthesis of Fe(50)Co(50) nanoparticles has been monitored employing Fourier transform infra red (FT-IR) spectroscopy and is modeled using a consecutive decomposition and growth model. This model predicts the experimentally realized FeCo nanoparticle composition as a function of the particle size fairly well. High-resolution transmission electron microscopy (HRTEM) was performed to uncover the resulting microstructure and composition on a nanometer scale. PMID:15288940

  2. 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.

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

    PubMed

    Finck, Nicolas; Dardenne, Kathy

    2016-05-01

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

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

    NASA Astrophysics Data System (ADS)

    Finck, Nicolas; Dardenne, Kathy

    2016-05-01

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

  5. 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.

  6. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2015-11-01

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

  8. Synthesis and XRD/PL Studies of Pure and Sb2O3 Doped ZnO Nanophases

    SciTech Connect

    Boulares, N.; Guergouri, K.; Tabet, N.; Monty, C.

    2007-08-22

    Pure and Sb2O3 (0 to 5% molar fraction) doped ZnO nanophases were synthesized using a sublimation-condensation method in a solar furnace. The initial and final powders were characterized by X-ray diffraction (XRD) and photoluminescence (PL) techniques. XRD results showed no significant change in the lattice parameters and the presence of a new phase Zn7O2Sb12 in the highly doped micropowders but not in the nanopowders. The photoluminescence spectra showed a strong donor-acceptor pair (DAP) emission in the pure untreated ZnO micropowder which is drastically reduced in pure and doped nanopowders. The donor-bound excitonic band (DX) includes three well resolved peaks in the PL spectra of the doped micropowders while the spectra of doped nanopowders showed a broader band. Furthermore, the free exciton emission was absent in all doped samples.

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

    NASA Astrophysics Data System (ADS)

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

    1999-04-01

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

  10. 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.

  11. Investigation on the sulfur state and phase transformation of spent and regenerated S zorb sorbents using XPS and XRD

    NASA Astrophysics Data System (ADS)

    Qiu, Limei; Zou, Kang; Xu, Guangtong

    2013-02-01

    A series of industrial S zorb sorbents extracted from production line were characterized by XPS and XRD. The formation of ZnAl2O4 and Zn2SiO4 is the major reason for the deactivation of spent sorbent. The stability of the Zn-containing spinel species leads to the decrease of the desulfurization efficiency of regenerated sorbent. The chemical states of sulfur atom were examined by XPS. The depth distribution of sulfur species and the reductive behavior of sulfate in H2 atmosphere were explored using Ar+ etching XPS and in situ XPS. The formation of sulfate species in the regeneration process decreases the content of ZnO in the surface significantly and should be avoided. XPS and XRD are excellent tools to follow the sulfur chemical states and phase evolution of S zorb sorbent, respectively, which provide important information for the investigation of deactivation pathways and regenerated mechanisms for S zorb sorbent.

  12. Crystal Structure and Morphology Dependence of the Phase of Mollusc Shell: A Case Study of XRD, SEM and ESR

    NASA Astrophysics Data System (ADS)

    Siriprom, W.; Kaewkhao, J.; Phachana, K.; Limsuwan, P.

    2011-01-01

    The aim of this study is to investigate the physical properties in the Paphia undulate and Amusium pleuronectes shells collected from the coastal area of Chonburi province, Thailand. The crystal structure of the shells was studied by x-ray diffraction (XRD). The XRD patterns spectra reveal that the Paphia undulate shells and Amusium pleuronectes shells are made of a pure aragonite phase, and a mixture phase of aragonite and calcite, respectively, the identification and quantitative analysis were performed by using the Rietveld method. In this study, we also used the scanning electron microscope (SEM) to study the Morphology of the Paphia undulate shells and Amusium pleuronectes shells. The results on SEM micrographs agree well with those of XRD. In addition, the ions in the shell samples were also studied by Electron Spin Resonance Spectroscopy (ESR). The ESR spectra show that the samples of both shells were consisting of Mn2+ ions. The pattern of the ESR spectrum is thus strongly influenced by the environment of the paramagnetic ions, and then it can be used to identification of crystal structure of mollusc shell

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

    SciTech Connect

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

    1990-12-01

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

  14. Versatility of electrospinning in the fabrication of fibrous mat and mesh nanostructures of bismuth ferrite (BiFeO3) and their magnetic and photocatalytic activities.

    PubMed

    Bharathkumar, S; Sakar, M; K, Rohith Vinod; Balakumar, S

    2015-07-21

    This study demonstrates the fabrication of electrospun bismuth ferrite (BiFeO3/BFO) fiber mat and fibrous mesh nanostructures consisting of aligned and random fibers respectively. The formation of these one dimensional (1D) nanostructures was mediated by the drum and plate collectors in the electrospinning process that yielded aligned and random nanofibers of BFO respectively. The single phase and rhombohedral crystal structure of the fabricated 1D BFO nanostructures are confirmed through X-ray diffraction (XRD) studies. X-ray photoelectron spectroscopy (XPS) studies indicated that the fabricated fibers are stoichiometric BFO with native oxidation states +3. The surface texture and morphology are analyzed using the field emission scanning electron microscopy (FESEM) and high resolution transmission electron microscopy (HRTEM) techniques. The average size of fibers in mat and mesh nanostructures is found to be 200 nm and 150 nm respectively. The band gap energy of BFO mat and mesh deduced from their UV diffuse reflectance spectra (UV-DRS) was found to be 2.44 eV and 2.39 eV, respectively, which evidenced the improved visible light receptivity of BFO mesh compared to that of the mat. Magnetization studies using a super conducting quantum interference device (SQUID) magnetometer revealed the weak ferromagnetic properties of BFO mesh and mat nanostructures that could emerge due to the dimension induced suppression of cycloidal spin structures. The photocatalytic degradation properties of the fibrous mesh are found to be enhanced compared to that of the mat. This could be attributed to the reduced band gap energy and an improved semiconductor band-bending phenomenon in the mesh that favoured the transportation of excited charge carriers to the photocatalyst-dye interfaces and the production of more number of reactive species that lead to the effective degradation of the dye molecules. PMID:26083677

  15. 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 determine the types and abundances of amorphous phases in the martian rocks and sand shadow. These models suggest that the rocks and sand shadow are composed of approx 30% amorphous phases. Sulfate-adsorbed allophane and ferrihydrite were measured by EGA to further understand the speciation of the sulfur present in the amorphous component. These data indicate that sulfate adsorbed onto the surfaces of amorphous phases could explain a portion of the SO2 evolution in the Rocknest SAM data. The additional constraints placed on the mineralogy and chemistry of the aqueous alteration phases through our laboratory measurements can help us better understand the nature of the fluids that affected the different samples and devise a history of aqueous alteration for the Sheepbed Member of the Yellowknife Bay Fm. at Gale crater.

  16. 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 components.

  17. 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.

  18. 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. PMID:26206215

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

    PubMed

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

    2014-08-01

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

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

    PubMed

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

    2014-08-01

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

  1. 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. Copyright © 2015 John Wiley & Sons, Ltd. PMID:26687421

  2. 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.

  3. A comprehensive review of the XRD data of the primary and secondary phases present in the BSCCO superconductor system

    SciTech Connect

    Reardon, B.J.; Hubbard, C.R.

    1992-02-01

    X-ray powder patterns for the phases in the CaO-SrO-PbO ternary system, along with the corresponding crystal structures, were obtained from the literature and from the Powder Diffraction File (PDF). Available X-ray diffraction (XRD) patterns were compared with each other and, when possible, with a calculated pattern for each phase, yielding a recommended reference pattern. The simulated powder patterns presented here deal with the phases found within the (Ca,Sr){sub 2}PbO{sub 4} solid solution series and are recommended for the PDF.

  4. 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...

  5. 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.

  6. 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.

  7. 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.

  8. Process monitoring and control with CHEMIN, a miniaturized CCD-based instrument for simultaneous XRD/XRF analysis

    NASA Astrophysics Data System (ADS)

    Vaniman, David T.; Bish, D.; Guthrie, G.; Chipera, S.; Blake, David E.; Collins, S. Andy; Elliott, S. T.; Sarrazin, P.

    1999-10-01

    There is a large variety of mining and manufacturing operations where process monitoring and control can benefit from on-site analysis of both chemical and mineralogic constituents. CHEMIN is a CCD-based instrument capable of both X-ray fluorescence (XRF; chemical) and X-ray diffraction (XRD; mineralogic) analysis. Monitoring and control with an instrument like CHEMIN can be applied to feedstocks, intermediate materials, and final products to optimize production. Examples include control of cement feedstock, of ore for smelting, and of minerals that pose inhalation hazards in the workplace. The combined XRD/XRF capability of CHEMIN can be used wherever a desired commodity is associated with unwanted constituents that may be similar in chemistry or structure but not both (e.g., Ca in both gypsum and feldspar, where only the gypsum is desired to make wallboard). In the mining industry, CHEMIN can determine mineral abundances on the spot and enable more economical mining by providing the means to assay when is being mined, quickly and frequently, at minimal cost. In manufacturing, CHEMIN could be used to spot-check the chemical composition and crystalline makeup of a product at any stage of production. Analysis by CHEMIN can be used as feedback in manufacturing processes where rates of heating, process temperature, mixture of feedstocks, and other variables must be adjusted in real time to correct structure and/or chemistry of the product (e.g., prevention of periclase and alkali sulfate coproduction in cement manufacture).

  9. Characterization of stabilized/solidified refinery oily sludge and incinerated refinery sludge with cement using XRD, SEM and EXAFS.

    PubMed

    Karamalidis, Athanasios K; Psycharis, Vasileios; Nicolis, Ioannis; Pavlidou, Eleni; Benazeth, Simone; Voudrias, Evangelos A

    2008-08-01

    Solidification/stabilization (S/S) of refinery oily sludge and incinerated oily sludge (ash) with cement type I42.5 and II42.5 was investigated using, X-Ray Diffraction (XRD), Scanning Electron Microscopy (SEM) combined with Energy Dispersive Spectroscopy (EDS) and Extended X-ray Absorption Fine Structure (EXAFS). The results showed that delayed ettringite formation (DEF) and major cement hydration reactions occurred. XRD analysis of S/S oily sludge samples revealed cement-bearing solid phases, such as portlandite, calcite, C(3)S, C(2)S and C(4)AF. SEM analysis, confirmed ettringite at solidified oily sludge samples. Solidified ash samples contained ettringite substituted by chromates. However, solid phases found in solidified ash samples with I42.5 cement showed minor variation in type and structure compared to those observed in solidified ash samples with II42.5 cement. Fe K edge EXAFS analysis revealed the presence of iron oxides in both S/S wastes. The comparison between spectra of the S/S resulting materials and the ones of their original components, showed that the first sphere Fe-O distances were longer than in the pure iron oxide thereby providing evidence that the resulting materials were not simple mixtures, but products of a reaction that modified the local environment of iron. PMID:18584430

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

    PubMed

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

    2014-10-15

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

  11. Anisotropically structured magnetic aerogel monoliths

    NASA Astrophysics Data System (ADS)

    Heiligtag, Florian J.; Airaghi Leccardi, Marta J. I.; Erdem, Derya; Süess, Martin J.; Niederberger, Markus

    2014-10-01

    Texturing of magnetic ceramics and composites by aligning and fixing of colloidal particles in a magnetic field is a powerful strategy to induce anisotropic chemical, physical and especially mechanical properties into bulk materials. If porosity could be introduced, anisotropically structured magnetic materials would be the perfect supports for magnetic separations in biotechnology or for magnetic field-assisted chemical reactions. Aerogels, combining high porosity with nanoscale structural features, offer an exceptionally large surface area, but they are difficult to magnetically texture. Here we present the preparation of anatase-magnetite aerogel monoliths via the assembly of preformed nanocrystallites. Different approaches are proposed to produce macroscopic bodies with gradient-like magnetic segmentation or with strongly anisotropic magnetic texture.Texturing of magnetic ceramics and composites by aligning and fixing of colloidal particles in a magnetic field is a powerful strategy to induce anisotropic chemical, physical and especially mechanical properties into bulk materials. If porosity could be introduced, anisotropically structured magnetic materials would be the perfect supports for magnetic separations in biotechnology or for magnetic field-assisted chemical reactions. Aerogels, combining high porosity with nanoscale structural features, offer an exceptionally large surface area, but they are difficult to magnetically texture. Here we present the preparation of anatase-magnetite aerogel monoliths via the assembly of preformed nanocrystallites. Different approaches are proposed to produce macroscopic bodies with gradient-like magnetic segmentation or with strongly anisotropic magnetic texture. Electronic supplementary information (ESI) available: Digital photographs of dispersions and gels with different water-to-ethanol ratios; magnetic measurements of an anatase aerogel containing 0.25 mol% Fe3O4 nanoparticles; XRD patterns of the iron oxide and titania nanoparticles. See DOI: 10.1039/c4nr04694c

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

    NASA Astrophysics Data System (ADS)

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

    2003-04-01

    Recent experimental and theoretical studies suggest that the lower mantle is significantly anelastic. The origin of this anelasticity remains uncertain, however. One possible cause is the viscous motion of twin domain walls. Here we use a combination of dynamical mechanical analysis (DMA) and stroboscopic X-ray diffraction (XRD) to study the effect of domain walls on seismic-frequency anelasticity in perovskite at high temperature. We apply the technique to single crystal LaAlO_3, a close structural analogue of the MgSiO_3 perovskite phase believed to make up more than 70% of the Earth's lower mantle. We demonstrate that superelastic behaviour associated with the motion of domain walls dominates the mechanical response over a temperature range spanning several hundred degrees. This is accompanied by a factor-of-ten decrease in the effective Young's modulus below the cubic to rhombohedral phase transition and a rapid increase in attenuation. Freezing of domain walls at lower temperatures leads to mechanical stiffening and a broad peak in attenuation (tand >0.9 at 200^oC and 1 Hz). The observations indicate that domain walls are strongly pinned by oxygen vacancies. The combination of DMA and XRD permits the response of domain walls to a dynamic force to be observed in-situ for the very first time. The XRD-DMA machine consists of a standard Perkin-Elmer DMA-7e in three-point bend geometry, combined with a conventional X-ray source and position sensitive detector. The X-ray source is movable, allowing X-rays to be focused on the underside of the sample at a wide range of incident angles. Measuring diffracted intensity as a function of incident angle results in a conventional rocking curve, permitting the twin microstructure to be quantified. During a DMA measurement, X-rays are binned into four separate spectra, which are synchronised to four different stages of the dynamic force cycle. In this way, changes in microstructure which occur directly in response to the dynamic force can be resolved on a timescale of 0.1-50 Hz. The first results of this technique applied to LaAlO_3 are presented. Clear differences in the rocking curves corresponding to the maximum and minimum dynamic force can be resolved in the temperature range where superelastic softening is observed. The changes correspond to a shift in the position of the diffraction peaks. This shift is thought to be caused by the compatibility strain which develops as the domain walls are forced to rotate away from their preferred orientations.

  13. 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 discrimination of diffracted and fluoresced X rays. The ability to accumulate and integrate the entire circumference of each complete Debye diffraction ring compensates for poor powder preparations, as might be produced by robotic sampling systems. With CHEMIN, a wide range of minerals can be uniquely identified. Using Rietveld analysis of the XRD results, mineral quantification is also possible. Expanded capabilities in phase analysis and constrained data solutions using quantitative XRD and XRF are within reach. PMID:11542260

  14. 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.

  15. 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. PMID:19559899

  16. FTIR and XRD investigations on the thermal stability of hydroxyapatite during hot pressing and pressureless sintering processes

    NASA Astrophysics Data System (ADS)

    Rapacz-Kmita, A.; Paluszkiewicz, C.; ?lsarczyk, A.; Paszkiewicz, Z.

    2005-06-01

    Performance of hydroxyapatite material in a living body depends on a number of factors. Stability of hydroxyapatite structure, which is influenced by both, preparation conditions of the starting precursor powders and fabrication method of the implant materials, is an important one. Inappropriate preparation conditions of synthesis, calcination of powder and sintering of formed samples result in dehydroxylation and even in decomposition of HAp which lead to the change in the physicochemical properties of implants. In the work samples of hydroxyapatite ceramics have been obtained by two methods, i.e. by hot pressing and by pressureless sintering in the temperature range of 1150-1300 C. The materials prepared have been studied using FTIR and XRD in order to identify the dehydroxylation processes and the possible hydroxyapatite decomposition during thermal treatment. The usefulness of both methods in identification of thermal stability of hydroxyapatite was confirmed.

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

    PubMed

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

    2012-11-01

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

  18. 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 surface’s 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.

  19. 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.

  20. 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. PMID:22447060

  1. The use of combined synchrotron radiation micro FT-IR and XRD for the characterization of Romanesque wall paintings

    NASA Astrophysics Data System (ADS)

    Salvadó, N.; Butí, S.; Pantos, E.; Bahrami, F.; Labrador, A.; Pradell, T.

    2008-01-01

    The high analytical sensitivity and high spatial resolution of synchrotron radiation-based techniques, in particular SR-XRD and SR-FT-IR, allows the identification of complex micrometric mixtures of compounds that constitute the different layers of ancient paintings. The reliability of the measurements even with an extremely small amount of sampled material is very high, and this is particularly important when analyzing art works. Furthermore, the micro size (10×10μm for FT-IR and 30 to 50 μm squared spot size for XRD) of the beam enables one to obtain detailed compositional profiles from the different chromatic and preparation layers. The sensitivity of the techniques is high enough for the determination of minor and trace compounds, such as reaction and weathering compounds. We report here the identification of pigments in the Romanesque wall paintings found in situ in the church of Saint Eulàlia of Unha place in the Aran valley (central Pyrenees). During the first centuries of the second millennium numerous religious buildings were built in Western Europe in the Romanesque style. In particular, a great number of churches were built in the Pyrenees, most of which were decorated with wall paintings. Although only a few of these paintings have survived, they represent one of the most important collections of Romanesque art, both for their quantity and quality. A full identification of the pigments, binder, supports, and reaction and weathering compounds has been obtained. The results obtained, in particular aerinite as a pigment, indicate a clear connection between the paintings found in this Occitanian church and the Catalan Romanesque paintings from the south bound of the Pyrenees.

  2. Characterisation of 1,3-diammonium propylselenate monohydrate by XRD, FT-IR, FT-Raman, DSC and DFT studies

    NASA Astrophysics Data System (ADS)

    Thirunarayanan, S.; Arjunan, V.; Marchewka, M. K.; Mohan, S.; Atalay, Yusuf

    2016-03-01

    The crystals of 1,3-diammonium propylselenate monohydrate (DAPS) were prepared and characterised X-ray diffraction (XRD), FT-IR, FT-Raman spectroscopy, and DFT/B3LYP methods. It comprises protonated propyl ammonium moieties (diammonium propyl cations), selenate anions and water molecule which are held together by a number of hydrogen bonds and form infinite chains. The XRD data confirm the transfer of two protons from selenic acid to 1,3-diaminopropane molecule. The DAPS complex is stabilised by the presence of O-H···O and N-H···O hydrogen bonds and the electrostatic interactions as well. The N···O and O···O bond distances are 2.82-2.91 and 2.77 Å, respectively. The FT-IR and FT-Raman spectra of 1,3-diammonium propyl selenate monohydrate are recorded and the complete vibrational assignments have been discussed. The geometry is optimised by B3LYP method using 6-311G, 6-311+G and 6-311+G* basis sets and the energy, structural parameters, vibrational frequencies, IR and Raman intensities are determined. Differential scanning colorimetry (DSC) data were also presented to analyse the possibility of the phase transition. Complete natural bonding orbital (NBO) analysis is carried out to analyse the intramolecular electronic interactions and their stabilisation energies. The electrostatic potential of the complex lies in the range +1.902e × 10-2 to -1.902e × 10-2. The limits of total electron density of the complex is +8.43e × 10-2 to -8.43e × 10-2.

  3. Radiometric, SEM and XRD investigation of black sands at Chituc placer deposit North of the City of Navodari, Romania

    NASA Astrophysics Data System (ADS)

    Duliu, Octavian G.; Blebea-Apostu, Ana-Maria; Gomoiu, Claudia; Margineanu, Romul M.; Costea, Constantin; Dumitras, Delia; Ion, Adriana

    2014-05-01

    The black sand of the Chituc marine sandbank situated northern of the city of Navodari (Romania), displayed anomalous high ambient dose rates. Field measurements performed during 2013 Summer campaign recorded in some places dose rate up to 200 nSv/h, significantly overpassing the average value of 44 ± 20 nSv/h recorded along the entire Southern sector of Romanian Black Sea shore. Here, the sand presented a black-brownish hue, different by the usual white yellowish colour. Gamma ray spectrometry performed on both Slanic-Prahove Underground Low Background Laboratory and Gological Institute Radiometric Facilities showed with clarity the dominance of 228-Ac radioisotope in the 50 microns fraction together with the 226-Ra and traces of 40-K. No significant amount of anthropogenic 137-Cs were identified. The other granulometric fractions, i.e. 315, 200 as well 100 microns presented a significant lower level of radioactivity. X-ray diffraction (XRD) as well as Scanning Electron Microsopy (SEM) data attested the presence of monazite, zircon, magnetite, ilmenite, andradite, quartz, aragonite and albite in different proportions, the monazite and zircon being preponderant in the 50 microns, the most radioactive fraction. Based on both radiometric and XRD determinations we come to the conclusion that the evidenced radioactivity could be attributed to both uranium and thorium series in the zircon and monazite fractions and to a lesser extent in the garnet fraction. By its position with respect to Danube Delta, the Chituc marine sandbank could be regarded as a placer where heavy minerals discharged in the Black Sea by the Danube River and transported southward by the Great Black Sea Rim are deposited by gravity separation during sedimentary processes. The implications of the Chituc levee radioactive anomaly for any further human activity are analysed and discussed. Acknowledgement: Work done within the BS ERA NET 041 project in the frame of BS-ERA.NET Pilot Joint CAll 2010-2011.

  4. A comparison between magnetic and reflection loss characteristics of substituted strontium ferrite and nanocomposites of ferrite/carbon nanotubes

    NASA Astrophysics Data System (ADS)

    Ghasemi, Ali; Shirsath, Sagar E.; Liu, Xiaoxi; Morisako, Akimitsu

    2012-04-01

    Large-scale carbon nanotubes (CNTs)/substituted strontium ferrite nanocomposites have been fabricated by hetero-coagulation. The structure and morphology of nanoparticles and nanocomposites were evaluated by high-resolution transmission electron microscopy (HRTEM). HRTEM confirmed that strontium ferrite was successfully attached to carbon nanotubes. The vibrating sample magnetometer (VSM) confirmed the relatively strong dependence of saturation magnetization with the volume percentage of multi-walled carbon nanotubes (MWCNTs). Reflection loss of nanocomposites at 12-18 GHz was evidently enhanced, as compared to that of strontium ferrite nanoparticles. The maximum reflection loss increased significantly with an increase in volume percentage of MWCNTs. It was proved that the microwave absorbing bandwidth was modulated simply by manipulating the thickness of nanocomposites. Reflection loss evaluations indicate that the nanocomposites display a great potential application as wide-band electromagnetic wave absorbers.

  5. 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 límite norte del Terreno Piedra Alta (Uruguay). Importancia de la faja milonítica sinestral de Colonia. Actas XVI Congreso Argentino de Geología, de La Plata. Gaucher, C., Poiré, D.G., Finney, S.C., Valencia, V.a., Blanco, G., Pamoukaghlian, K., Gómez Peral, L. (2008). Detrital zircón ages of Neoproterozoic sedimentary successions in Uruguay and Argentina: Insights into the geological evolution of the Rio de la Plata Craton. Precambrian Research. Hartmann, L.A., Campal, N., Santos, J.O., Mc. Neughton, N.J., Schipilov, A., Lafon, J.M. (2001). Archean crust in the Rio de la Plata Craton, Uruguay - SHRIMP U-Pb zircon reconnaissance geochronology. Journal of South American Earth Science, 14, 557-570. Pamoukaghlian, K., Gaucher, C., Bossi, J., Sial, N., Poire, D.G. (2006). First C and O isotopic data for the Piedras de Afilar Formation, Tandilia Terrane, Uruguay: their bearing on correlation and age. Fifth South American Symposium on Isotope Geology, Punta del Este.

  6. 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

    Recent orbital investigations have revealed that aqueous alteration on early Mars took place in diverse alteration environments indicated by distinctive assemblages of minerals (Murchie et al., 2009, JGR). There is growing evidence for past diagenetic or low-temperature/pressure hydrothermal activity on Mars at neutral to alkaline pH, indicated by the presence of Fe/Mg smectites, chlorite, prehnite, serpentine, opaline silica, and zeolites such as analcime in Noachian terrains (Ehlmann et al., 2009, JGR). In recent investigations of terrestrial Mars analog sites, neutral to alkaline pH alteration of basalt, both pedogenic and hydrothermal, has been understudied in favor of sulfur-rich, acidic systems including those at the Hawaiian volcanoes and Rio Tinto, Spain. We began study of the alteration of basalt lava flows in Iceland as a geochemical analog for Noachian Mars. Because the basaltic bedrock is recently formed (<16Ma) with few localities of more highly evolved composition and has poorly formed soils and spare vegetation, the ground and surface waters are broadly similar to those which might have existed on Noachian Mars. Iceland has a variety of geothermal spring systems--low T, low S; low T, high S; and high T, high S--each of which creates distinctive mineralogic assemblages. Here we examine rocks of the Hvalfjordur peninsula, collected from basalt flows that were in some places altered at the surface by pedogenesis and in other locations were hydrothermally altered by non-sulfurous groundwater circulation (low T, low S) following the emplacement of a later hot basalt flow. Rock samples were surveyed in the field using a portable VNIR spectrometer. Altered and unaltered rocks that were typical for the locality were collected as were altered rocks whose spectra were most similar to those measured by CRISM from Mars orbit. Ten rocks were ultimately selected for detailed laboratory analyses: zeolitized basaltic rocks bearing minerals including analcime and 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.

  7. Mineralogical Capabilities of the CheMin XRD/XRF instrument on Mars Science Laboratory (MSL ’11)

    NASA Astrophysics Data System (ADS)

    Blake, D. F.; Vaniman, D. T.; Yen, A. S.; Chen, C.; Sarrazin, P.; Bish, D. L.; Chipera, S.; Morris, R. V.

    2009-12-01

    A principal goal of the Mars Science Laboratory (MSL ‘11) mission is to identify and characterize present or past habitable environments on Mars. By determining the mineralogical composition of rocks or soil, one can often deduce the conditions under which they formed, or their subsequent diagenetic or metamorphic history. The CheMin mineralogical instrument [1-3] will return quantitative X-ray diffraction data (XRD) and qualitative X-ray fluorescence data (XRF; 14 < Z < 92) from scooped soils and drilled rock powders collected from the Mars surface. Small amounts (45-65 mm3) of sample material sieved to <150 µm will be delivered through a funnel to one of 27 reuseable sample cells located on a sample wheel. Sample cells are 8-mm diameter discs bounded by 7-µm thick Mylar or Kapton windows spaced 170 µm apart. Within this volume, the sample is shaken by piezoelectric vibration at sonic frequencies, causing the powder to flow past a narrow, collimated X-ray beam in random orientations during the course of an analysis. CheMin is designed to have a Minimum Detection Limit (MDL) of <3% by mass, accuracy better than 15% and precision better than 10% for phases present in concentrations >4X MDL (12%). CheMin uses a Co X-ray tube so that absorption in iron-rich samples is minimized. The resolution of the diffraction patterns is <0.35° 2θ, and the angular measurement range is 4-55° 2θ. The capabilities of the FM instrument were tested during ThermoVac using mineral and ceramic standards contained on the FM sample wheel. Standards include 88:12 and 97:3 mixtures of beryl:quartz for assessment of the accuracy and precision of quantitative analyses, miminum detection limits, 2θ range and 2θ resolution; a compositionally diverse ceramic material for XRF evaluation; arcanite (K2SO4); and an amphibole. Analyses were performed under Mars atmospheric pressure at a range of Rover Avionics Mounting Platform (RAMP) temperatures from -40C to +26C. Within the predicted Mars RAMP operating temperatures of 0C to +20C, peak-to-background ratios in the XRD pattern and FWHM of elemental peaks in XRF spectra were within proscribed limits. The beryl:quartz mixtures show some anomalous phase segregation during sample shaking that is being investigated. Mineral detection and energy resolution capabilites meet or exceed requirements. References: [1] http://msl-scicorner.jpl.nasa.gov/Instruments/CheMin/. [2] LPSC40 #1484 (2009). [3] Martian Phyllosilicates: Recorders of Aqueous Processes #7006 (2008).

  8. Surface mediated Ag-Hg alloy formation under ambient and vacuum conditions—AFM and XRD investigations

    NASA Astrophysics Data System (ADS)

    Nowakowski, Robert; Pielaszek, Jerzy; Duś, Ryszard

    2002-10-01

    Thin Ag films deposited under UHV conditions on a glass support were exposed to Hg vapor at 298 K under two different conditions: vacuum, and ambient atmosphere. The influence of the amalgamation process on film topography was studied by the atomic force microscopy (AFM) method, while the composition of the amalgams was determined by means of X-ray diffraction (XRD). The obtained results indicated the different mechanism of Ag 2Hg 3 alloy formation depending on whether the amalgam is formed in a vacuum or under ambient atmosphere. This is discussed as a consequence of the influence of oxygen and different kinetics of the amalgamation process performed under both conditions. Heating of amalgam leads to gradual reconstruction of the alloy (370 K) and finally its decomposition (500 K), leaving strongly modified, discontinuous silver film. The ultimate nanostructure of the film depends on the transport mechanism of the silver nanounits during the amalgamation process. Therefore, Ag-Hg alloy formation and decomposition seems to be a practical and promising method for the preparation of discontinuous thin silver films of significant thickness and mesoscopic structure.

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

    NASA Astrophysics Data System (ADS)

    Salvad, Nati; But, Salvador; Cotte, Marine; Cinque, Gianfelice; Pradell, Trinitat

    2013-04-01

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

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

    SciTech Connect

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

    1995-12-31

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

  11. 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.

  12. 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.

  13. In Situ XAS and XRD Studies of Substituted Spinel Lithium Manganese Oxides in the 4-5 V Region

    SciTech Connect

    McBreen, J.; Mukerjee, S.; Yang, X. Q.; Sun, X.; Ein-Eli, Y.

    1998-11-01

    Partial substitution of Mn in lithium manganese oxide spinel materials by Cu and Ni greatly affects the electrochemistry and the phase behavior of the cathode. Substitution with either metal or with a combination of both shortens the 4.2 V plateau and results in higher voltage plateaus. In situ x-ray absorption (XAS) studies indicate that the higher voltage plateaus are related to redox processes on the substituents. In situ x-ray diffraction (XRD) on LiCu{sub 0.5}Mn{sub 1.5}O{sub 4} shows single phase behavior during the charge and discharge process. Three phases are observed for LiNi{sub 0.5}Mn{sub 1.5}O{sub 4} and two phases are observed in the case of LiNi{sub 0.25}Cu{sub 0.25}Mn{sub 1.5}O{sub 4}. The electrolyte stability is dependent on both the operating voltage and the cathode composition. Even though Ni substituted materials have lower voltages, the electrolyte is more stable in cells with the Cu substituted materials.

  14. Reactivity of fluoro-substituted bis(thiocarbonyl) donors with diiodine: an XRD, FT-Raman, and DFT investigation.

    PubMed

    Mancini, Annalisa; Aragoni, M Carla; Bingham, Ann L; Castellano, Carlo; Coles, Susanne L; Demartin, Francesco; Hursthouse, Michael B; Isaia, Francesco; Lippolis, Vito; Maninchedda, Giuseppe; Pintus, Anna; Arca, Massimiliano

    2013-12-01

    The reactions of 1,3,8,10-tetrakis(4'-fluorophenyl)-4,5,6,7-tetrathiocino[1,2-b:3,4-b']diimidazolyl-2,9-dithione (4) and molecular diiodine afforded spoke adducts with stoichiometries 4·I2 and 4·3I2 , isolated in the compound 4·3I2·xCH2Cl2·(1-x)I2 (x=0.70), and characterized by single-crystal XRD and FT-Raman spectroscopy. The nature of the reaction products was investigated under the prism of theoretical calculations carried out at the DFT level. The structural data, FT-Raman spectroscopy, and quantum mechanical calculations agree in indicating that the introduction of fluorophenyl substituents results in a lowering of the Lewis basicity of this class of bis(thiocarbonyl) donors compared with alkyl-substituted tetrathiocino donors and fluorine allows for extended interactions that are responsible for solid-state crystal packing. PMID:24027238

  15. 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. © 2015 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater, 104B: 546-553, 2016. PMID:25952407

  16. Adsorption of Lysine on Na-Montmorillonite and Competition with Ca(2+): A Combined XRD and ATR-FTIR Study.

    PubMed

    Yang, Yanli; Wang, Shengrui; Liu, Jingyang; Xu, Yisheng; Zhou, Xiaoyun

    2016-05-17

    Lysine adsorption at clay/aqueous interfaces plays an important role in the mobility, bioavailability, and degradation of amino acids in the environment. Knowledge of these interfacial interactions facilitates our full understanding of the fate and transport of amino acids. Here, X-ray diffraction (XRD) and attenuated total reflectance Fourier-transform infrared spectroscopy (ATR-FTIR) measurements were used to explore the dynamic process of lysine adsorption on montmorillonite and the competition with Ca(2+) at the molecular level. Density functional theory (DFT) calculations were employed to determine the peak assignments of dissolved lysine in the solution phase. Three surface complexes, including dicationic, cationic, and zwitterionic structures, were observed to attach to the clay edge sites and penetrate the interlayer space. The increased surface coverage and Ca(2+) competition did not affect the interfacial lysine structures at a certain pH, whereas an elevated lysine concentration contributed to zwitterionic-type coordination at pH 10. Moreover, clay dissolution at pH 4 could be inhibited at a higher surface coverage with 5 and 10 mM lysine, whereas the inhibition effect was inconspicuous or undetected at pH 7 and 10. The presence of Ca(2+) not only could remove a part of the adsorbed lysine but also could facilitate the readsorption of dissolved Si(4+) and Al(3+) and surface protonation. Our results provide new insights into the process of lysine adsorption and its effects on montmorillonite surface sites. PMID:27118104

  17. 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.

  18. Microanalysis (micro-XRF, micro-XANES, and micro-XRD) of a tertiary sediment using microfocused synchrotron radiation.

    PubMed

    Denecke, Melissa A; Somogyi, Andrea; Janssens, Koen; Simon, Rolf; Dardenne, Kathy; Noseck, Ulrich

    2007-06-01

    Micro-focused synchrotron radiation techniques to investigate actinide elements in geological samples are becoming an increasingly used tool in nuclear waste disposal research. In this article, results using mu-focus techniques are presented from a bore core section of a U-rich tertiary sediment collected from Ruprechtov, Czech Republic, a natural analog to nuclear waste repository scenarios in deep geological formations. Different methods are applied to obtain various, complementary information. Elemental and element chemical state distributions are obtained from micro-XRF measurements, oxidation states of As determined from micro-XANES, and the crystalline structure of selected regions are studied by means of micro-XRD. We find that preparation of the thin section created an As oxidation state artifact; it apparently changed the As valence in some regions of the sample. Results support our previously proposed hypothesis of the mechanism for U-enrichment in the sediment. AsFeS coating on framboid Fe nodules in the sediment reduced mobile groundwater-dissolved U(VI) to less-soluble U(IV), thereby immobilizing the uranium in the sediment. PMID:17490498

  19. 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.

  20. Effect of annealing temperature on the structural, photoluminescence and magnetic properties of sol-gel derived Magnetoplumbite-type (M-type) hexagonal strontium ferrite

    NASA Astrophysics Data System (ADS)

    Teh, Geok Bee; Wong, Yat Choy; Tilley, Richard D.

    2011-09-01

    Magnetoplumbite-type (M-type) hexagonal strontium ferrite particles were synthesized via sol-gel technique employing ethylene glycol as the gel precursor at two different calcination temperatures (800 and 1000 °C). Structural properties were systematically investigated via X-ray diffraction (XRD), field emission scanning electron microscopy, high resolution transmission electron microscopy (HRTEM), energy dispersive spectroscopy (EDS), thermogravimetric analysis (TGA), photoluminescence spectrophotometry and superconducting quantum interference device magnetometer. XRD results showed that the sample synthesized at 1000 °C was of single-phase with a space group of P6 3/mmc and lattice cell parameter values of a=5.882 Å and c=23.048 Å. EDS confirmed the composition of strontium ferrite calcined at 1000 °C being mainly of M-type SrFe 12O 19 with HRTEM micrographs confirming the ferrites exhibiting M-type long range ordering along the c-axis of the crystal structure. The photoluminescence (PL) property of strontium ferrite was examined at excitation wavelengths of 260 and 270 nm with significant PL emission peaks centered at 350 nm being detected. Strontium ferrite annealed at higher temperature (1000 °C) was found to have grown into larger particle size, having higher content of oxygen vacancies and exhibited 83-85% more intense PL. Both the as-prepared strontium ferrites exhibited significant oxygen vacancies defect structures, which were verified via TGA. Higher calcination temperature turned strontium ferrite into a softer ferrite.

  1. 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.

  2. 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.

  3. 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 in the soil samples were cinnabar (HgS), metacinnabar, corderoite (Hg3S2Cl2), and amorphous Hg-S-Cl phases, in different proportions. The presence of these amorphous forms was suggested by EXAFS and XRD structural analyses. The speciation obtained is also in agreement with the chemical behaviour of the soil samples as assessed by sequential extractions and thermal desorption analyses. The chemical species identified are typical of soils contaminated with wastes produced by chlor-alkali plants. Actually, a chlor-alkali plant was active in the area during the 1960-80's, and now is no more existing. In conclusion, notwithstanding the diffuse Hg-pollution in the investigated area, it seems that Hg is speciated in scarcely soluble and hardly mobilisable forms. The determination of the chemical forms of toxic elements in polluted soils is an indispensable step to identify the source of pollution, to formulate a correct risk assessment and to develop effective remediation strategies.

  4. 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.

  5. 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

  6. SR-XRD and SR-FTIR study of the alteration of silver foils in medieval paintings.

    PubMed

    Salvadó, Nati; Butí, Salvador; Labrador, Ana; Cinque, Gianfelice; Emerich, Hermann; Pradell, Trinitat

    2011-03-01

    Altarpieces and polychrome carved wood from the fifteenth century AD usually exhibit golden and silvery areas by the application of a very thin foil of metal. The metal foils were normally protected from the atmosphere by a varnish or resin which maybe either preserved or absent. Moreover, they were glued to the background surface by adhesive substances (egg yolk, drying oil or animal glue). The high proportion of the glueing substances often renders the development of reaction compounds. With time, silver alters blacken or simply disappear completely. In this paper, we study the alterations to metal foils from a selection of fifteenth century artworks showing different glueing agents, organic coatings and several degrees of conservation of the organic coatings and metal leafs. The submillimetric layered structure and the high variability and low amount of most of the compounds present in the different layers, as well as their differing nature (organic and inorganic) make the use of micron-sensitive high-resolution techniques essential for their study. In particular, the high resolution, high brilliance and small footprint renders synchrotron radiation most adequate for their study. SR-XRD was performed to identify the reaction compounds formed in the different layers; μFTIR was used at to identify the silver protecting organic coatings, the metal foil glueing layers and the corresponding reaction compounds. The results obtained suggest that atmospheric corrosion is the dominant mechanism, and therefore that the degree of corrosion of the metal foils is mainly related to the conservation state of the protecting coatings. PMID:21079931

  7. Microstructure characterization and magnetic properties of nanomaterials

    NASA Astrophysics Data System (ADS)

    Sun, Xiang-Cheng

    The microstructure and superparamagnetic properties of two systems of magnetic nanoparticles are reviewed. A new type of magnetic core-shell Ni-Ce nanocomposite particle (15-50nm) has been prepared. Typical HREM images and FFT patterns of HREM images showed that many planar defects (nanotwins and stacking faults) exist in the large Ni core zone (10-45nm). The shell layers (3-5nm) consist of an innermost Ni-Ce alloy and an outermost NiO oxide. FFT patterns from different regions of typical HREM images show well defined spots characteristic of core-shell nanocomposite materials. Magnetization measurements as a function of magnetic field and temperature showed that superparamagnetic behaviour is exhibited above the average block temperature (TB = 170K). This superparamagnetic relaxation was found to be modified by interparticle interactions that depend on the applied field and size distribution. In addition, antiferromagnetic order occurred with a Nel temperature TN of about 11K. A spin-flip transition was observed below TN at a certain applied field. Novel carbon encapsulated Ni nanoparticles assemblies have been synthesized by modified arc-discharge under a methane atmosphere. The presence of carbon encapsulation is confirmed by HR-TEM lattice imaging, and nanodiffraction. The intimate and contiguous carbon fringe around these Ni nanoparticles is good evidence for complete encapsulation by carbon shell layers. Superparamagnetic property studies show that the blocking temperature TB is around 115K at 0.1T applied field. Above TB, the magnetization M(H,T) can be described by the classical Langevin function L using the relation M|Ms(T= 0)=coth ( wH/kT ) - kT / ?H. The particle size can be inferred from the Langevin fit (particle moment ?), which is a little larger than the HR-TEM observation. It is suggested that these assemblies of carbon encapsulated Ni nanoparticles have typical single-domain, field-dependent superparamagnetic relaxation properties, and this typical superparamagnetic behaviour is consistent with the Stoner-Wohlfarth theory of single-domain particles.

  8. New two in one magnetic fluorescent nanocomposites

    NASA Astrophysics Data System (ADS)

    Corr, Serena A.; Gun'ko, Yurii K.; Byrne, Stephen J.; Douvalis, Alexios P.; Venkatesan, Munuswamy; Gunning, Robert D.

    2005-06-01

    Magnetite nanoparticles have been coated by a porphyrin derivative to produce new magnetic materials with fluorescent properties. The magnetic nanoparticles were prepared using two different methods, one based on sol-gel techniques and ultrasonic processing, and the other via a controlled chemical co-precipitation. Different types of porphyrin functionalised magnetic nanoparticles have been prepared and have been characterised by electron microscopy (TEM and SEM), XRD, FTIR, Raman, UV-vis, and fluorescence spectroscopy. Microscopy results showed the formation of core-shell nanostructures, with IR and photoluminescence spectroscopy results confirming the presence of porphyrin in the shell.

  9. Structural and Magnetic Characterization of the ``Gaspar'' Meteorite from Betéitiva, Boyacá, Colombia

    NASA Astrophysics Data System (ADS)

    Flor, L. M.; Pérez, G. A.

    2013-09-01

    In this work we reported the structural and magnetic characterization of the “Gaspar” meteorite from Beteitiva, Boyacá, Colombia. The meteorite was characterized by XRD, Mössbauer spectrometry and scanning electron microscopy.

  10. 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.

  11. 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 Grneisen 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.

  12. 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.

  13. 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.

  14. 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.

  15. Sol-gel synthesis of Fe-Co nanoparticles and magnetization study

    NASA Astrophysics Data System (ADS)

    Nautiyal, Pranjal; Seikh, Md. Motin; Lebedev, Oleg I.; Kundu, Asish K.

    2015-03-01

    We report the synthesis of carbon encapsulated Fe-Co nanoparticles using conventional sol-gel route and its magnetization studies. The x-ray diffraction indicates the formation of the single phase body centered cubic alloy Fe-Co phase with cell parameter of 2.857 Å. Nanoparticles are highly crystalline and exhibit low index faceting as determined from high-resolution transmission electron microscopy (HRTEM) investigation. The observed orthogonal lattice planes with lattice distance of 2.86 Å are attributed to (100) and (010). HRTEM image confirms the cube like Fe-Co nanoparticles with core-shell structure of carbon encapsulation, composed of carbon and graphite materials. The magnetometry results of the carbon encapsulated alloy Fe-Co nanoparticles with core-shell structure designate as a ferromagnetically ordered soft magnet with coercive field of 890 Oe (at 5 K). The coercive field and magnetization value depend on the size of nanoparticles as well as the diamagnetic contribution of carbon encapsulation.

  16. In situ XRD investigation of the evolution of alumina-supported cobalt catalysts under realistic conditions of Fischer-Tropsch synthesis.

    PubMed

    Karaca, Héline; Hong, Jingping; Fongarland, Pascal; Roussel, Pascal; Griboval-Constant, Anne; Lacroix, Maxime; Hortmann, Kai; Safonova, Olga V; Khodakov, Andrei Y

    2010-02-01

    The structure-activity relations in the alumina-supported cobalt catalysts are studied at the realistic conditions of Fischer-Tropsch synthesis using in situ time-resolved XRD and catalytic measurements. Cobalt sintering during the first 3-5 h of the reaction and cobalt carbidisation at a longer time on stream (>8 h) coincide with catalyst deactivation. PMID:20087521

  17. 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 agreement with estimates of the mean thickness of fundamental particles obtained both TEM measurements and from fixed cations content, up to a mean value of 20 layers. Correction for instrumental broadening under the conditions employed here is unnecessary for this range of thicknesses.

  18. 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.

  19. 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.

  20. Interplay of structural, optical and magnetic properties in Gd doped CeO2

    NASA Astrophysics Data System (ADS)

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

    2015-06-01

    In this research wok systematic investigation on the synthesis, characterization, optical and magnetic properties of Ce1-xGdxO2 (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 CeO2 samples. Magnetic studies showed that the Gd doped polycrystalline samples display room temperature ferromagnetism and the ferromagnetic ordering strengthens with the Gd concentration.

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

    NASA Astrophysics Data System (ADS)

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

    2013-12-01

    A field portable X-ray Diffraction (XRD) instrument was used at White Sands National Monument to perform in-situ measurements followed by laboratory analyses of the gypsum-rich dunes and to determine its modal mineralogy. The field instrument is a Terra XRD (Olympus NDT) based on the technology of the CheMin (Chemistry and Mineralogy) instrument onboard the Mars Science Laboratory (MSL) rover Curiosity which is providing the mineralogical and chemical composition of scooped soil samples and drilled rock powders collected at Gale Crater [1]. Using Terra at White Sands will contribute to 'ground truth' for gypsum-bearing environments on Mars. Together with data provided by VNIR spectra [2], this study clarifies our understanding of the origin and history of gypsum-rich sand dunes discovered near the northern polar region of Mars [3]. The results obtained from the field analyses performed by XRD and VNIR spectroscopy in four dunes at White Sands revealed the presence of quartz and dolomite. Their relative abundance has been estimated using the Reference Intensity Ratio (RIR) method. For this study, particulate samples of pure natural gypsum, quartz and dolomite were used to prepare calibration mixtures of gypsum-quartz and gypsum-dolomite with the 90-150μm size fractions. All single phases and mixtures were analyzed by XRD and RIR factors were calculated. Using this method, the relative abundance of quartz and dolomite has been estimated from the data collected in the field. Quartz appears to be present in low amounts (2-5 wt.%) while dolomite is present at percentages up to 80 wt.%. Samples from four dunes were collected and prepared for subsequent XRD analysis in the lab to estimate their composition and illustrate the changes in mineralogy with respect to location and grain size. Gypsum-dolomite mixtures: The dolomite XRD pattern is dominated by an intense diffraction peak at 2θ≈36 deg. which overlaps a peak of gypsum, This makes low concentrations of dolomite difficult to quantify in mixtures with high concentration of gypsum. Dolomite has been detected in some locations at dune 3 as high as 80 wt.%. Gypsum-quartz mixtures: The intensity of the main diffraction peak of quartz at 2θ≈31 deg. decreases progressively with the decrease of the amount of quartz in the mixtures. Samples from dune 1 and 2 show quartz abundance at 5.6 and 2.6 wt.% respectively . [1] Blake et al. Space Sci. Rev. (2012). doi:10.1007/s11214-012-9905-1. [2] King et al. (2013) AGU, submitted. [3] Langevin et al. (2005). Science 307, 1584-1586.

  2. 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.

  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. Relation between electronic structure and magnetic anisotropy in amorphous TbCo films probed by x-ray magnetic circular dichroism

    NASA Astrophysics Data System (ADS)

    Ueno, T.; Inami, N.; Sagayama, R.; Wen, Z.; Hayashi, M.; Mitani, S.; Kumai, R.; Ono, K.

    2016-05-01

    Magnetic anisotropy of amorphous TbCo films was investigated by x-ray absorption spectroscopy (XAS), x-ray magnetic circular dichroism (XMCD) and synchrotron radiation x-ray diffraction (XRD). The easy magnetization axis was out-of-plane and in-plane for the as-deposited and annealed films, respectively. Remarkable features observed with regard to annealing were a peak-energy shift and increased asymmetry in the Co L 2,3 XMCD spectra and variations of the fine structures in the Tb M 4,5 XMCD spectra. A quantitative analysis of the XMCD results revealed that the Co 3d spin magnetic moment decreased and the orbital magnetic moment increased with annealing. On the other hand, both Tb 4f spin and orbital magnetic moments decreased with annealing. In contrast to the clear change in XAS and XMCD by annealing, no significant change in the amorphous structure was detected by XRD.

  5. Study on industrial wastewater treatment using superconducting magnetic separation

    NASA Astrophysics Data System (ADS)

    Zhang, Hao; Zhao, Zhengquan; Xu, Xiangdong; Li, Laifeng

    2011-06-01

    The mechanism of industrial wastewater treatment using superconducting magnetic separation is investigated. Fe 3O 4 nanoparticles were prepared by liquid precipitation and characterized by X-ray diffraction (XRD). Polyacrylic acid (PAA) film was coated on the magnetic particles using plasma coating technique. Transmission electron microscope (TEM) observation and infrared spectrum measurement indicate that the particle surface is well coated with PAA, and the film thickness is around 1 nm. Practical paper factory wastewater treatment using the modified magnetic seeds in a superconducting magnet (SCM) was carried out. The results show that the maximum removal rate of chemical oxygen demand (COD) by SCM method can reach 76%.

  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. 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)

  8. 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.

  9. 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.

  10. 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.

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

    PubMed

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

    2016-04-19

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

  12. The coercivity mechanism of sintered SM(CobalFe0.245Cu0.07Zr0.02)7.8 permanent magnets with different isothermal annealing time

    NASA Astrophysics Data System (ADS)

    Sun, Wei; Zhu, Minggang; Guo, Zhaohui; Fang, Yikun; Li, Wei

    2015-11-01

    Precipitation-hardened 2:17-type SmCo permanent magnet has attracted much attention due to its high Curie temperature and excellent magnetic properties. Sm(CobalFe0.245Cu0.07Zr0.02)7.8 (at%) sintered magnets with high remanence (Br ~1.15 T) were prepared using a traditional powder metallurgy method. The intrinsic coercivity Hcj of the magnets was increased from 429 to 994 kA m-1 with isothermal annealing time increasing from 10 to 40 h, which is different from the phenomenon that increasing aging time leads to a reduced coercivity mentioned in the Ref. [16]. In consideration of rarely report about the microstructure of the final magnet isothermally annealed for 40 h, we have tried to originally analyze the relationship between the microstructure and the magnetic properties. Besides, the lattice constants of sintered Sm(CobalFe0.245Cu0.07Zr0.02)7.8 permanent magnet isothermally annealed for 40 h have been given by indexing the HRTEM results including the selected area electron diffraction (SAED) and HRTEM images.

  13. Synthesis and study of quantum size effect, XRD and IR spectral properties of PbS nanocrystals doped in SiO 2 xerogel matrix

    NASA Astrophysics Data System (ADS)

    Parvathy, N. N.; Pajonk, G. M.; Rao, A. Venkateswara

    1997-08-01

    PbS nanocrystallites with a diameter smaller than 15 nm have been prepared in a pure silica matrix by sol-gel route. Silica xerogels containing 0.01-3 wt% of PbS were prepared by hydrolysis and polycondensation of methanolic tetramethyl orthosilicate [TMOS, Si(OCH 3) 4] in the presence of ammonium hydroxide (NH 4OH) catalyst and lead nitrate Pb(NO 3) 2 and subsequent reaction with Na 2S to form PbS nanocrystals. These PbS-nanocrystals-doped xerogels were characterised by optical absorption, X-ray diffraction (XRD) and infra-red spectroscopy (IR). Blue shift in optical absorption threshold indicate that the PbS crystallite size reduced from 16 to 5 nm with a decrease in the PbS wt% from 3 to 0.01. It was found from the XRD studies that weak and broad peaks are obtained because of nanocrystalline state of PbS. The PbS crystallite structure was found to be cubic in the SiO 2 matrix by observing the peak positions in the XRD pattern. In the IR spectra, the peaks related to PbS bonds were obtained and they are weak. It was observed that there was no change in peak position related to the SiO 2 matrix in the presence of PbS in between the SiO 2 network.

  14. Surface properties of CuCl 2/AC catalysts with various Cu contents: XRD, SEM, TG/DSC and CO-TPD analyses

    NASA Astrophysics Data System (ADS)

    Han, Man Seok; Lee, Byung Gwon; Ahn, Byoung Sung; Moon, Dong Ju; Hong, Suk In

    2003-04-01

    Surface properties of CuCl 2/activated carbon (AC) catalyst for dimethyl carbonate synthesis were studied by CO-TPD, XRD, SEM and thermogravimetry (TG)/differential scanning calorimetry (DSC) with varying Cu contents. CuCl 2/AC catalysts were prepared by impregnating AC with CuCl 2-ethanol solution in the range of Cu content from 2.8 to 18.7 wt.%. CuCl 2·2H 2O crystalline phase as active sites was gradually increased with an increase in Cu content. Appearance of CuCl 2·2H 2O was clearly identified by XRD and SEM. In relatively low Cu contents, 4.6 and 9.9 wt.%, CuCl 2·2H 2O was not detected in XRD. This indicates the formation of good dispersion of CuCl 2 compounds on activated carbon. However, DSC result revealed that CuCl 2·2H 2O was formed in multi-layers for the catalyst with Cu content more than 9.9 wt.%, which limit the catalyst activity. This fact was also strongly supported by CO-TPD experiment. The two CuCl 2/AC catalysts having Cu contents of 4.6 and 9.9 wt.% showed no difference in CO adsorption amount in TPD experiments.

  15. X-ray diffraction microtomography (XRD-CT), a novel tool for non-invasive mapping of phase development in cement materials.

    PubMed

    Artioli, G; Cerulli, T; Cruciani, G; Dalconi, M C; Ferrari, G; Parisatto, M; Rack, A; Tucoulou, R

    2010-07-01

    A recently developed synchrotron-based imaging technique, X-ray diffraction microtomography (XRD-CT), has been applied here for the first time to a complex system, the hydrating Portland cement paste, in order to monitor the evolution of microstructure and phase formation with a 3D non-invasive imaging approach. The ettringite-XRD-peak-based image reconstructions, combined with transmission microtomography (X-microCT) images, allowed to assess the ubiquitous distribution of this phase, which appears early in the hydration process and showed its preferential concentration in the relatively less compact regions of the paste. The comparison of greyscale histograms for cement pastes after 9 and 58 h from hydration showed an increase of ettringite content with age, in agreement with the quantitative Rietveld analysis of the sum patterns. By renormalizing the greyscale histograms to the relative weight fraction, as obtained from Rietveld refinements, a new technique which allows estimation of phase contents with spatial resolution has been developed. The results achievable by combining XRD-CT, X-microCT and Rietveld appear very promising to provide experimental snapshots of the cement hydration process to be compared with results obtained from computer simulations. PMID:20358183

  16. 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 determine the types and abundances of amorphous phases in the martian rocks and sand shadow. These models suggest that the rocks and sand shadow are composed of ~30% amorphous phases. Sulfate-adsorbed allophane and ferrihydrite were measured by EGA to further understand the speciation of the sulfur present in the amorphous component. These data indicate that sulfate adsorbed onto the surfaces of amorphous phases could explain a portion of the SO2 evolution in the Rocknest SAM data. The additional constraints placed on the mineralogy and chemistry of the aqueous alteration phases through our laboratory measurements can help us better understand the nature of the fluids that affected the different samples and devise a history of aqueous alteration for the Sheepbed Member of the Yellowknife Bay Fm. at Gale crater.

  17. 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…

  18. 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

  19. 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…

  20. Mössbauer and XRD Studies of N0.6Cu0.2Zn0.2Ce(x)Fe2-xO4 Ferrites by Sol-Gel Auto-Combustion.

    PubMed

    Lin, Qing; Lei, Chengiong; He, Yun; Xu, JianmeI; Wang, Ruijun

    2015-04-01

    In this work, stoichiometric Ni0.6Cu0.2Zn0.2Ce(x)Fe2-xO4 ferrites with 0 ≤ x ≤ 0.85 have been prepared by Sol-Gel auto-combustion method and we have investigated the effect of impurity CeO2 phase to the microstructure and hyperfine magnetic field in spinel ferrite. The results of XRD patterns confirm that the average crystallite size of samples decreases with Ce3+ substitution increasing and the lattice parameters vary as a function of x content. 57Fe Mössbuaer spectra at room temperature for all samples confirm the [Fe(3+)-O2-Fe3+] super exchange interaction decrease due to cerium substitution. For low temperature auto-combustion samples it reveals one normal sextet line and one doublet line x ≤ 0.25, which show well-resolved ferromagnetic order. Lattice defects are determined and Mössbuaer spectrums vary from magnetic sextet to relaxation doublet at x > 0.45 due to a mass of CeO2 phase. In contrast, the Mössbuaer spectra for the samples sintered at 800 °C/3 h detect the secondary phase-Fe2O3 where the cation distribution occurs and it collapses to paramagnetic doublet (x ≥ 0.85). So Ce3+ substitution has its maximum limit values of super exchange interaction and high sintering temperature will affect this interaction. SEM shows the crystallite of the un-doped specimen sintered at 800 °C/3 h form well. PMID:26353526

  1. High-resolution transmission electron microscopy observations on textured rapidly quenched NdFeB permanent magnets

    NASA Astrophysics Data System (ADS)

    Li, Lin; Luzzi, D. E.; Graham, C. D., Jr.

    1991-11-01

    High-resolution transmission electron microscopy (HRTEM) has been used to examine the microstructures of NdFeB magnets made by rapid solidification. The samples were General Motors MQ-3 magnets, and also MQ-3 magnets that had been recompressed perpendicular to the original compression axis. A major finding is that the Nd-rich grain-boundary phase is not uniformly distributed on all grain boundaries of the Nd2Fe14B phase. Some boundaries are completely clean, and where the Nd-rich phase does appear, its thickness varies widely. The grain-boundary phase (whose structure has been variously identified) is partially ordered at room temperature after slow cooling. Ordered domains and antiphase boundaries have been observed in this phase by HRTEM. Using the Nd2Fe14B fringe spacing as calibration, the lattice parameter of the grain-boundary phase is found to be 5.58 Å. In the completely ordered state, this phase is neither bcc nor fcc; it is simple cubic with a lower-symmetry space group Pm3m.

  2. 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.

  3. 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.

  4. Electrochemical fabrication of nanocomposite films containing magnetic metal nanoparticles

    NASA Astrophysics Data System (ADS)

    Hayashi, Yoshiaki; Hashi, Shuichiro; Kura, Hiroaki; Yanai, Takeshi; Ogawa, Tomoyuki; Ishiyama, Kazushi; Nakano, Masaki; Fukunaga, Hirotoshi

    2015-07-01

    Controlling the structure composed of soft and hard magnetic phases at the nanoscale is the key to fabricating nanocomposite magnets with efficient exchange coupling. In our previous study, nanocomposite films containing ferrite nanoparticles were fabricated by a combination of electrophoretic deposition and electroplating to show one possibility of controlling the structure of nanocomposite magnets three-dimensionally by applying self-assembly of magnetic nanoparticles. To expand this combination method to the fabrication of nanocomposite magnets, the use of magnetic metal nanoparticles is desired. In this paper, we attempted to fabricate nanocomposite films composed of Fe-Co nanoparticles in a Fe-Pt matrix by this combination method. Through cross-sectional observation and XRD analysis, a nanostructure composed of Fe-Co nanoparticles embedded in a L10 Fe-Pt matrix was confirmed. These results indicate that this method is capable of producing composite materials containing metal magnetic nanoparticles.

  5. Characterization of Magnetic Nano-Crystalline Systems

    NASA Astrophysics Data System (ADS)

    Ghominezhad, M.; Sebt, A.; Akhavan, M.

    2000-09-01

    Preparation of fine magnetic particles of iron oxide is investigated Production process is based on quick chemical growth of magnetic oxide by dehydration of salt solution of Fe2+ and Fe3+ salts in different molar ratio. The STEM photographs obtained the true physical diameter of magnetic particles which is about 12 nm, and the XRD patterns is used in obtaining the DRX, another evidence for physical diameter, that is about 9-13 nm. In order to investigate the magnetic size and susceptibility of particles, the production of magnetic oxides has been followed by ferrofluid production through dispersion of particles by surface-active agent adsorption. There was more attention given to bilayer ferrofluids with Oleate as first layer and sodium dodecyle sulfate (SDS) as second layer surfactants. The magnetic particle size, DM, was determined through magnetic measurements by VSM system and is about 11-13 nm. The data of VSM and XRD show that DRX is a little less, and DM is a little greater than the true physical diameter due to the presence of surface anisotropy and the existence of a size distribution in the magnetic dispersed phase. There is a local maximum in the magnetic oxide concentration versus SDS concentration near the critical micellization concentration (CMC) of SDS, because of high tendency in making micelles after this point. The ferrofluids produced are superparamagnetic with reduced initial susceptibility of about 310 -3 - 5 10 -3 Oe -1. Titration by KMnO 4 and interpretation of XRD patterns of oxides show that the closest stoichiometery of Fe3O4 can be achieved by increasing the Fe3+/Fe2+ molar ratio up to 2/3 with extra acidifying for prevention of uncontrolled Fe2+ oxidation. The adsorption of the first layer of surfactants on particles is also investigated by infrared spectroscopy. The disappearance of free Oleate peaks in IR spectrum show that to adsorb second layer, we have to make a true monolayer of Oleate by stirring the magnetic layers particles until complete separation in a solvent of Oleate has taken place.

  6. 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.

  7. 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 ultrasonic drill were analyzed and the results were compared to carefully prepared powders obtained using a laboratory bench scale Retsch mill.

  8. A comprehensive review of the XRD data of the primary and secondary phases present in the BSCCO superconductor system. Part 2, Ca-Sr-Pb oxides

    SciTech Connect

    Reardon, B.J.; Hubbard, C.R.

    1992-02-01

    X-ray powder patterns for the phases in the CaO-SrO-PbO ternary system, along with the corresponding crystal structures, were obtained from the literature and from the Powder Diffraction File (PDF). Available X-ray diffraction (XRD) patterns were compared with each other and, when possible, with a calculated pattern for each phase, yielding a recommended reference pattern. The simulated powder patterns presented here deal with the phases found within the (Ca,Sr){sub 2}PbO{sub 4} solid solution series and are recommended for the PDF.

  9. 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.

  10. 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.

  11. Synthesis, structural and vibrational investigation on 2-phenyl-N-(pyrazin-2-yl)acetamide combining XRD diffraction, FT-IR and NMR spectroscopies with DFT calculations.

    PubMed

    Lukose, Jilu; Yohannan Panicker, C; Nayak, Prakash S; Narayana, B; Sarojini, B K; Van Alsenoy, C; Al-Saadi, Abdulaziz A

    2015-01-25

    The optimized molecular structure, vibrational frequencies, corresponding vibrational assignments of 2-phenyl-N-(pyrazin-2-yl)acetamide have been investigated experimentally and theoretically using Gaussian09 software package. The title compound was optimized by using the HF/6-31G(6D,7F) and B3LYP/6-31G(6D,7F) calculations. The geometrical parameters are in agreement with the XRD data. The stability of the molecule arising from hyper-conjugative interaction and charge delocalization has been analyzed using NBO analysis. Gauge-including atomic orbital (1)H-NMR chemical shifts calculations were carried out and compared with experimental data. The HOMO and LUMO analysis is used to determine the charge transfer within the molecule. Molecular electrostatic potential was performed by the DFT method. First hyperpolarizability is calculated in order to find its role in non linear optics. From the XRD data, in the crystal, molecules are held together by strong C-H⋯O and N-H⋯O intermolecular interactions. PMID:25124846

  12. 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.

  13. 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.

  14. 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.

  15. Combined In-Situ XRD and In-Situ XANES Studies on the Reduction Behavior of a Rhenium Promoted Cobalt Catalyst

    SciTech Connect

    Kumar, Nitin; Payzant, E Andrew; Jothimurugesan, K; Spivey, James J

    2011-01-01

    A 10% Co 4% Re/(2% Zr/SiO2) catalyst was prepared by co-impregnation using a silica support modified by 2% Zr. The catalyst was characterized by temperature programmed reduction (TPR), in situ XRD and in situ XANES analysis where it was simultaneously exposed to H2 using a temperature programmed ramp. The results showed the two step reduction of large crystalline Co3O4 with CoO as an intermediate. TPR results showed that the reduction of highly dispersed Co3O4 was facilitated by reduced rhenium by a H2-spillover mechanism. In situ XRD results showed the presence of both, Co-hcp and Co-fcc phases in the reduced catalyst at 400 C. However, the Co-hcp phase was more abundant, which is thought to be the more active phase as compared to the Co-fcc phase for CO hydrogenation. CO hydrogenation at 270 C and 5 bar pressure produces no detectable change in the phases during the time of experiment. In situ XANES results showed a decrease in the metallic cobalt in the presence of H2/CO, which can be attributed due to oxidation of the catalyst by reaction under these conditions.

  16. In-situ investigation of stress conditions during expansion of bare metal stents and PLLA-coated stents using the XRD sin(2)ψ-technique.

    PubMed

    Kowalski, Wolfgang; Dammer, Markus; Bakczewitz, Frank; Schmitz, Klaus-Peter; Grabow, Niels; Kessler, Olaf

    2015-09-01

    Drug eluting stents (DES) consist of platform, coating and drug. The platform often is a balloon-expandable bare metal stent made of the CoCr alloy L-605 or stainless steel 316 L. The function of the coating, typically a permanent polymer, is to hold and release the drug, which should improve therapeutic outcome. Before implantation, DES are compressed (crimped) to allow implantation in the human body. During implantation, DES are expanded by balloon inflation. Crimping, as well as expansion, causes high stresses and high strains locally in the DES struts, as well as in the polymer coating. These stresses and strains are important design criteria of DES. Usually, they are calculated numerically by finite element analysis (FEA), but experimental results for validation are hardly available. In this work, the X-ray diffraction (XRD) sin(2)ψ-technique is applied to in-situ determination of stress conditions of bare metal L-605 stents, and Poly-(L-lactide) (PLLA) coated stents. This provides a realistic characterization of the near-surface stress state and a validation option of the numerical FEA. XRD-results from terminal stent struts of the bare metal stent show an increasing compressive load stress in tangential direction with increasing stent expansion. These findings correlate with numerical FEA results. The PLLA-coating also bears increasing compressive load stress during expansion. PMID:25974098

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

    NASA Astrophysics Data System (ADS)

    Pham, Van-Thai; Fulton, John L.

    2013-01-01

    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 the hydration and ion pair structure of CaCl2 and RbBr salts in concentrated aqueous solutions. The XADSR method combines the x-ray absorption fine structure (XAFS) spectral analysis of both the cation and anion as a probe of their short-range structure with an x-ray diffraction (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 0.26 Ca2+-Cl- CIP's separated by about 2.71 , while there are 3.4 SSIP's separated by about 4.98 . In contrast XADSR analysis of 6 m aqueous RbBr yields about 0.7 pair CIP at a bond length of 3.51 . 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.

  18. In situ characterization of uranium and americium oxide solid solution formation for CRMP process: first combination of in situ XRD and XANES measurements.

    PubMed

    Caisso, Marie; Picart, Sébastien; Belin, Renaud C; Lebreton, Florent; Martin, Philippe M; Dardenne, Kathy; Rothe, Jörg; Neuville, Daniel R; Delahaye, Thibaud; Ayral, André

    2015-04-14

    Transmutation of americium in heterogeneous mode through the use of U1-xAmxO2±δ ceramic pellets, also known as Americium Bearing Blankets (AmBB), has become a major research axis. Nevertheless, in order to consider future large-scale deployment, the processes involved in AmBB fabrication have to minimize fine particle dissemination, due to the presence of americium, which considerably increases the risk of contamination. New synthesis routes avoiding the use of pulverulent precursors are thus currently under development, such as the Calcined Resin Microsphere Pelletization (CRMP) process. It is based on the use of weak-acid resin (WAR) microspheres as precursors, loaded with actinide cations. After two specific calcinations under controlled atmospheres, resin microspheres are converted into oxide microspheres composed of a monophasic U1-xAmxO2±δ phase. Understanding the different mechanisms during thermal conversion, that lead to the release of organic matter and the formation of a solid solution, appear essential. By combining in situ techniques such as XRD and XAS, it has become possible to identify the key temperatures for oxide formation, and the corresponding oxidation states taken by uranium and americium during mineralization. This paper thus presents the first results on the mineralization of (U,Am) loaded resin microspheres into a solid solution, through in situ XAS analysis correlated with HT-XRD. PMID:25742991

  19. Superconducting magnets

    SciTech Connect

    Not Available

    1994-08-01

    This report discusses the following topics on superconducting magnets: D19B and -C: The next steps for a record-setting magnet; D20: The push beyond 10 T: Beyond D20: Speculations on the 16-T regime; other advanced magnets for accelerators; spinoff applications; APC materials development; cable and cabling-machine development; and high-{Tc} superconductor at low temperature.

  20. Preparation and magnetic property of Fe nanowire array

    NASA Astrophysics Data System (ADS)

    Yang, Shaoguang; Zhu, Hao; Yu, Dongliang; Jin, Zhiqiang; Tang, Shaolong; Du, Youwei

    2000-12-01

    Fe was electrodeposited into the holes of porous anodic aluminium oxide (AAO) which was prepared electrochemically. X-ray diffraction (XRD) spectra illustrated that the deposited material was α-Fe. TEM observation showed that the aspect ratio of the nanowires was larger than 1000. The diameter of the wire was about 35 nm corresponding to that of the holes in the AAO. Magnetic measurements of the Fe nanowire array showed that its easy magnetization direction is perpendicular to the sample plane. This kind of nanowire array has potential applications in perpendicular magnetic recording.

  1. A new magnetic expanded graphite for removal of oil leakage.

    PubMed

    Ding, Xiaohui; Wang, Rong; Zhang, Xin; Zhang, Yanzong; Deng, Shihuai; Shen, Fei; Zhang, Xiaohong; Xiao, Hong; Wang, Lilin

    2014-04-15

    Magnetic expanded graphite (MEG) was prepared using the blended calcination method under a nitrogen atmosphere. MEG was characterized by scanning electron microscope (SEM), X-ray powder diffraction (XRD), Raman spectroscopy, and vibrating sample magnetization (VSM). Results show that the cobalt ferrite nanoparticles were uniformly and efficiently deposited on expanded graphite (EG). The saturation magnetization reached 55.05 emu g(-1), and the adsorption capacity of MEG under the optimal condition was 35.72 g g(-1) for crude oil. PMID:24559739

  2. Magnetic Properties of Fe/Metal/Fe Trilayer Films

    NASA Astrophysics Data System (ADS)

    Zolanvari, A.; Sadeghi, H.; Nezamdost, J.; Jafari, M. R.

    2011-12-01

    In this paper, magnetic properties of Fe/Cu/Fe, Fe/Cr/Fe Fe/Al/Fe (Ferromagnetic/Metal/Ferromagnetic) sandwitch thin films have been studied. The magnetic properties were investigated by magnetic force microscopy (MFM) alternative gradient force magnetometery (AGFM) analysis. The structure of the mentioned sandwiches was investigated using X-ray diffraction (XRD) analysis. An X-ray diffractometer with Cu-Kα radiation (λ = 1.5405 Å) was used, in a Bragg-Brentano arrangement and atomic force microscopy. Morphological and structural studies show that the nanoparticles grow in a well-defined nanostructured pattern.

  3. Magnetization Study of CoxCu1-x Nanoparticles

    NASA Astrophysics Data System (ADS)

    Dhara, Susmita; Chowdhury, Rajeswari Roy; Bandyopadhyay, Bilwadal

    Nanostructured CoCu granular alloys have been prepared by chemical reduction method using NaBH4 as a reducing agent and characterized by inductively coupled plasma optical emission spectroscopy (ICPOES), x-ray diffraction (XRD) and transmission electron microscopy (TEM) studies. Zero-field cooled and field cooled (ZFC/FC) magnetization study shows a blocking temperature distribution resulting from particle size distribution which is a characteristic of superparamagnetism. Magnetization study reveals that at low Co concentration, the alloy particles are superparamagnetic. At higher Co concentration the magnetization is combination of ferromagnetism (FM) and superparamagnetism (SPM). The coercive field is independent of Co concentration.

  4. 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 demonstrated in iron-bearing phyllosilicates in both naturally and artificially damaged samples. Alterations in mineral structure and chemistry will have implications for the phases' efficiency as a barrier material. 1. Pattrick, R A D et al., (2013) Min. Mag., 77, 2867-2882. 2. Bower et al., unpubl.

  5. Effect of deposition pressure on the structural and magnetic properties of cobalt ferrite thin films

    SciTech Connect

    Nongjai, R.; Khan, S.; Ahmad, H.; Khan, I.; Asokan, K.

    2013-06-03

    We present the influence of deposition pressure on the structural and magnetic properties of cobalt ferrite thin films. Thin films of Co ferrite were deposited by rf sputtering on Si (100) substrate and characterized by X - Ray Diffraction (XRD), Atomic Force Microscopy (AFM) and Vibrating Sample Magnetometer (VSM). The XRD patterns showed the formation of crystalline single phase of the films. The particle size and surface roughness of the films were strongly influence by gas pressure. Hysteresis loops measured at room temperature showed the enhancement of magnetic properties with the increase of gas pressure which is attributed to the decrease of particle size.

  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. Fe-based bulk metallic glasses used for magnetic shielding

    NASA Astrophysics Data System (ADS)

    Şerban, Va; Codrean, C.; Uţu, D.; Ercuţa, A.

    2009-01-01

    The casting in complex shapes (tubullar) and the main magnetic properties of bulk metallic glasses (BMG) alloys from the ferromagnetic Fe-Cr-Ni-Ga-P-Si-C system, with a small adittion of Ni (3%) were studied. Samples as rods and sockets having the thickness up to 1 mm were obtained from master alloys by melt injection by low cooling rates into a Cu mold and annealed in order to ensure adequate magnetic requirements. The structure was examined by X-ray diffraction (XRD) and the basic magnetic properties (coercivity, magnetic remanence, initial susceptibility, etc.) were determined by conventional low frequency induction method. The experimental investigations on producing of BMG ferromagnetic alloys with 3% Ni show the possibility to obtain magnetic shields of complex shape with satisfactory magnetic properties. The presence of Ni does not affect the glass forming ability, but reduce the shielding capacity.

  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. PMID:26353670

  9. Magnetic nanostructures.

    PubMed

    Bennemann, K

    2010-06-23

    Characteristic results of magnetism in small particles, thin films and tunnel junctions are presented. As a consequence of the reduced atomic coordination in small clusters and thin films the electronic states and density of states are modified. Thus, magnetic moments and magnetization are affected. Generally, in clusters and thin films magnetic anisotropy plays a special role. In tunnel junctions the interplay of magnetism, spin currents and superconductivity are of particular interest. In ring-like mesoscopic systems Aharonov-Bohm-induced currents are studied. Results are given for single transition metal clusters, cluster ensembles, thin films, mesoscopic structures and tunnel systems. PMID:21393778

  10. 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 emphasize the strength of the different techniques and the working synergy of the three different techniques together for planetary space missions.

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

    NASA Astrophysics Data System (ADS)

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

    2012-04-01

    Polycrystalline Mg2GeO4-olivine has been deformed (strain rates from 2.10-4/s to 10-5/s) in the deformation-DIA in 13-BM-D at GSECARS (Advanced Photon Source) at ca. 2 GPa confining pressure for temperatures between 973 and 1573 K (i.e., in the Mg2GeO4-ringwoodite field). Stress, advancement of transformation, and strain were measured in-situ using X-ray diffraction (XRD) and imaging, and acoustic emissions (AE) were recorded simultaneously. When differential stress is applied (ca. 1- to 2 GPa) and temperature is increased, the very beginning of the transformation to the ringwoodite structure (as evidenced by in situ XRD) is accompanied by AE bursts which locate within the sample. At high strain rates (>10-4/s) and low temperatures (800-900 degrees C), the number of AEs is comparable, if not larger, to that observed during the cold compression of quartz grains. The largest events always occur at a temperature slightly below that of appearance of the ringwoodite-structure phase on the XRD images patterns. This suggests that AEs are generated while the transition is still nucleation controlled (pseudo-martensitic stage). During stress-relaxation periods, the rate of AE triggering decreases, but does not completely vanish. Importantly, we still observed very large AEs at strain rates as low as approx. 10-5/ s, while at these early stages of the transformation, the samples did not show any macroscopic rheological weakening. Focal mechanism analysis of the largest AEs showed that they are all of shear type, some being even pure double couple. They radiate about the same amount of energy as typically recorded during fast crack propagation in amorphous glass material. Microstructural analysis (SEM, EBSD and TEM) highlights the presence of thin transformation bands, with plausible evidence of shear (grain distortion and grain size reduction). These bands are made of incoherent spinel and olivine nano-grains which run across germanium-olivine grain boundaries. These bands are all oriented near perpendicular to the principal compressive stress. In samples for which no AEs were recorded (hydrostatic conditions and higher temperatures and reaction progress), microstructure is different with incoherent grain growth at GB (hydrostatic conditions) and spinel-lamellae within a single germanium olivine crystal (fast reaction rate under deviatoric stress). Our observations point out that under high deviatoric stress, the olivine - spinel transition is a source of mechanical instability, which produces nano-seismicity. This may have important consequences for the understanding of deep-focus earthquakes occurring in cold and metastable olivine within the transition zone.

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

    NASA Astrophysics Data System (ADS)

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

    2011-12-01

    Polycrystalline Mg2GeO4-olivine has been deformed (strain rates from 2.10-4/s to 10-5/s) in the deformation-DIA in 13-BM-D at GSECARS (Advanced Photon Source) at ca. 2 GPa confining pressure for temperatures between 973 and 1573 K (i.e., in the Mg2GeO4-ringwoodite field). Stress, advancement of transformation, and strain were measured in-situ using X-ray diffraction (XRD) and imaging, and acoustic emissions (AE) were recorded simultaneously. When differential stress is applied (ca. 1- to 2 GPa) and temperature is increased, the very beginning of the transformation to the ringwoodite structure (as evidenced by in situ XRD) is accompanied by AE bursts which locate within the sample. At high strain rates (>10-4/s) and low temperatures (800-900 degrees C), the number of AEs is comparable, if not larger, to that observed during the cold compression of quartz grains. The largest events always occur at a temperature slightly below that of appearance of the ringwoodite-structure phase on the XRD images patterns. This suggests that AEs are generated while the transition is still nucleation controlled (pseudo-martensitic stage). During stress-relaxation periods, the rate of AE triggering decreases, but does not completely vanish. Importantly, we still observed very large AEs at strain rates as low as approx. 10-5/ s, while at these early stages of the transformation, the samples did not show any macroscopic rheological weakening. Focal mechanism analysis of the largest AEs showed that they are all of shear type, some being even pure double couple. They radiate about the same amount of energy as typically recorded during fast crack propagation in amorphous glass material. Microstructural analysis (SEM, EBSD and TEM) highlights the presence of thin transformation bands, with plausible evidence of shear (grain distortion and grain size reduction). These bands are made of incoherent spinel and olivine nano-grains which run across germanium-olivine grain boundaries. These bands are all oriented near perpendicular to the principal compressive stress. In samples for which no AEs were recorded (hydrostatic conditions and higher temperatures and reaction progress), microstructure is different with incoherent grain growth at GB (hydrostatic conditions) and spinel-lamellae within a single germanium olivine crystal (fast reaction rate under deviatoric stress). Our observations point out that under high deviatoric stress, the olivine - spinel transition is a source of mechanical instability, which produces nano-seismicity. This may have important consequences for the understanding of deep-focus earthquakes occurring in cold and metastable olivine within the transition zone.

  13. A comprehensive review of the XRD data of the primary and secondary phases present in the BSCCO superconductor system: Part 1, Ca-Sr-Cu oxides

    SciTech Connect

    Reardon, B.J.; Hubbard, C.R.

    1992-01-01

    X-ray powder patterns for the phases in the CaO-SrO-CuO ternary system, along with the corresponding crystal structures, were obtained from the literature and from the Powder Diffraction File (PDF). Available X-ray diffraction (XRD) patterns were compared with each other and, when possible, with a simulated pattern for each phase, yielding a recommended reference pattern. The simulated powder patterns presented here deal with the phases found within the (Ca, Sr)O, (Ca,Sr){sub 2}CuO{sub 3}, (Ca,Sr){sub 14}Cu{sub 24}O{sub 41}, (Ca,Sr)CuO{sub 2}, (Ca,Sr)Cu{sub 2}O{sub 3}, and (Ca,Sr)Cu{sub 2}O{sub 2} solid solution series and are recommended for the PDF.

  14. 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.

  15. [X-ray diffraction (XRD) and near infrared spectrum (NIR) analysis of the soil overlying the Bairendaba deposit of the Inner Mongolia Grassland].

    PubMed

    Luo, Song-ying; Cao, Jian-jin; Wu, Zheng-quan

    2014-08-01

    The soil samples uniformly overlying the Bairendaba deposit of the Inner Mongolia grassland were collected, and ana- lyzed with X-ray diffraction (XRD) and near infrared spectrum (NIR), for exploring the origins of the soil from the, grassland mining area and the relationship with the underground rock. The results show that the samp]s consist of quartz, graphite, carbonate, hornblende, mica, chlorite, montmorillonite, illite, berlinite, diaspore, azurite, hen tite, etc. These indicate that the soil samples were not only from the weathering products of the surface rock, but also from the underground rock mass and the alteration of the wall rock. The azurite and the hematite contained in the soil, mainly coming from the oxidation zone of the orebodies, can be used as the prospecting marks. The alteration mineral assemblage is mainly chlorite-illite-montmorillonite and it experienced the alteration process of potassic alteration-->silicification-->carbonatization-->silk greisenization-->clayization. Also, the wall rock alteration and the physical weathering processes can be accurately restored by analyzing the combination of the alteration minerals, which can provide important reference information for the deep ore prospecting and the ore deposit genesis study, improving the rate of the prospecting. The XRD and NIR with the characteristics of the economy and quickness can be used for the identification of mineral composition of soil, and in the study of mineral and mineral deposits. Especially, NIR has its unique superiority, that is, its sample request is low, and it can analyze a batch of samples quickly. With the development of INR, it will be more and more widely applied in geological field, and can play an important role in the ore exploration. PMID:25474975

  16. [X-ray diffraction (XRD) and near infrared spectrum (NIR) analysis of the soil overlying the Bairendaba deposit of the Inner Mongolia Grassland].

    PubMed

    Luo, Song-ying; Cao, Jian-jin; Wu, Zheng-quan

    2014-08-01

    The soil samples uniformly overlying the Bairendaba deposit of the Inner Mongolia grassland were collected, and ana- lyzed with X-ray diffraction (XRD) and near infrared spectrum (NIR), for exploring the origins of the soil from the, grassland mining area and the relationship with the underground rock. The results show that the samp]s consist of quartz, graphite, carbonate, hornblende, mica, chlorite, montmorillonite, illite, berlinite, diaspore, azurite, hen tite, etc. These indicate that the soil samples were not only from the weathering products of the surface rock, but also from the underground rock mass and the alteration of the wall rock. The azurite and the hematite contained in the soil, mainly coming from the oxidation zone of the orebodies, can be used as the prospecting marks. The alteration mineral assemblage is mainly chlorite-illite-montmorillonite and it experienced the alteration process of potassic alteration-->silicification-->carbonatization-->silk greisenization-->clayization. Also, the wall rock alteration and the physical weathering processes can be accurately restored by analyzing the combination of the alteration minerals, which can provide important reference information for the deep ore prospecting and the ore deposit genesis study, improving the rate of the prospecting. The XRD and NIR with the characteristics of the economy and quickness can be used for the identification of mineral composition of soil, and in the study of mineral and mineral deposits. Especially, NIR has its unique superiority, that is, its sample request is low, and it can analyze a batch of samples quickly. With the development of INR, it will be more and more widely applied in geological field, and can play an important role in the ore exploration. PMID:25508754

  17. Ion-pairing in aqueous CaCl2 and RbBr solutions: simultaneous structural refinement of XAFS and XRD data

    SciTech Connect

    Pham, Thai V.; Fulton, John L.

    2013-01-28

    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- CIPs, but there are approximately 3.4 SSIPs separated by about 4.99 . In contrast XADSR analysis of aqueous RbBr yields about 0.7 pair CIP at a bond length 3.51 . 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.

  18. 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.

  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. 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.

  1. Planetary Magnetism

    SciTech Connect

    Russell, C.T.

    1980-02-01

    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.

  2. Magnetic materials

    NASA Astrophysics Data System (ADS)

    1985-03-01

    The report describes the fundamental role that magnetic materials play in many of the electrical and electronic systems used by modern society. It reviews the status of magnetic materials in their current engineering applications and identifies technical issues whose resolution would lead to improved performance in such applications as well as for new applications of these materials. The report recommends more research in the areas of rare-earth permanent magnets, amorphous magnetic materials and recording media and lists a number of scientific challenges.

  3. 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.

  4. 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.

  5. 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.

  6. Permanent magnets

    NASA Astrophysics Data System (ADS)

    Rossignol, Michel-François; Yonnet, Jean-Paul

    The number of materials systems used to make magnets on an industrial scale is limited. They are, in chronological order of appearance, AlNiCo (late 1930s), hard ferrites (1950s), the family of Sm-Co magnets which gave rise to two different magnet groups, SmCo 5 (late 1960s) and Sm(CoFeCuZr) 7-8 , often referred to as the "2-17" type magnets (late 1970s), and the neodymium-iron-boron or NdFeB family (mid-1980s).

  7. Electroplating hard magnetic SmCo for magnetic microactuator applications

    SciTech Connect

    Chen Jue; Rissing, Lutz

    2011-04-01

    Patterned SmCo thin films were electroplated from an aqueous solute containing glycine by using dc and pulse dc current on the beaker level. Micromolds prepared by photolithography allow an accurate pattern transfer for patterned deposition of the material. A flux guide of a magnetic microactuator was chosen as a pattern, and Al{sub 2}O{sub 3} was used as the substrate. Au and Cr were investigated as seed layer materials. The content of Sm in the SmCo films is strongly dependent on the applied cathodic current density. A relative Sm content of up to 13.8 at. % could be determined by energy dispersive x-ray (EDX) spectroscopy. The SmCo thin films were annealed at 560 deg. C in a vacuum oven. Vibrating sample magnetometer (VSM) measurements were applied to characterize the magnetic properties. This film features hard magnetic properties with an intrinsic coercivity H{sub ci} of up to 44 kA/m. Electron probe microanalysis (EPMA) measurements showed that up to 40 at. % of O may be integrated in these films. The phases in the deposited films were determined by applying X-ray diffraction (XRD) measurements. These films consist of a mixture of SmCo alloy, Sm oxide, and Co.

  8. Probing magnetic properties of ferrofluids using temperature dependent magnetic hyperthermia studies

    NASA Astrophysics Data System (ADS)

    Nemala, Humeshkar; Thakur, Jagdish; Naik, Vaman; Naik, Ratna

    2014-03-01

    Tuning the properties of magnetic nanoparticles is essential for biomedical and technological applications. An important phenomenon displayed by these nanoparticles is the generation of heat in the presence of an external oscillating magnetic field and is known as magnetic hyperthermia (MHT). The heat dissipation by the magnetic nanoparticles occurs via Neel relaxation (the flip of the internal magnetic moment of the nanoparticles) and Brownian relaxation (the physical rotation of the nanoparticles in the suspended media). Dextran coated iron oxide (Fe3O4) nanoparticles were synthesized using the co-precipitation method and characterized using XRD, TEM and DC magnetometry measurements. Roughly spherical in shape the particles have an average size of 13nm and a saturation magnetization of 65 emu/g. The MHT properties of these nanoparticles suspended in a weakly basic solution (ferrofluid) have been investigated as a function of the frequency and amplitude of magnetic field by incorporating a complete thermodynamical analysis of the experimental set-up. The heat generation is quantified using the specific power loss (SPL) and compared with the predictions of linear response theory. This analysis sheds light on important physical and magnetic properties of the nanoparticles.

  9. Structural and magnetic properties of chromium doped zinc ferrite

    NASA Astrophysics Data System (ADS)

    Sebastian, Rintu Mary; Thankachan, Smitha; Xavier, Sheena; Joseph, Shaji; Mohammed, E. M.

    2014-01-01

    Zinc chromium ferrites with chemical formula ZnCrxFe2-xO4 (x = 0.0, 0.2, 0.4, 0.6, 0.8, 1.0) were prepared by Sol - Gel technique. The structural as well as magnetic properties of the synthesized samples have been studied and reported here. The structural characterizations of the samples were analyzed by using X - Ray Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR), Scanning Electron Microscope (SEM), and Transmission Electron Microscope (TEM). The single phase spinel cubic structure of all the prepared samples was tested by XRD and FTIR. The particle size was observed to decrease from 18.636 nm to 6.125 nm by chromium doping and induced a tensile strain in all the zinc chromium mixed ferrites. The magnetic properties of few samples (x = 0.0, 0.4, 1.0) were investigated using Vibrating Sample Magnetometer (VSM).

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

    NASA Astrophysics Data System (ADS)

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

    2010-12-01

    Polycrystalline Mg2GeO4-olivine has been deformed (strain rates from 2.10-4/s to 10-5/s) in the deformation-DIA in 13-BM-D at GSECARS (Advanced Photon Source) at ca. 2 GPa confining pressure for temperatures between 973 and 1573 K (i.e., in the Mg2GeO4-ringwoodite field). Stress, advancement of transformation, and strain were measured in-situ using X-ray diffraction (XRD) and imaging, and acoustic emissions (AE) full waveforms were recorded simultaneously. When differential stress is applied (ca. 1- to 2 GPa) and temperature is increased, the very beginning of the transformation to the ringwoodite structure (as evidenced by in situ XRD) is accompanied by AE bursts which locate within the sample. At high strain rates (>10-4/s) and low temperatures (800-900 degrees C), the number of AEs is comparable, if not larger, to that observed during the cold compression of quartz grains. The largest events always occur at a temperature slightly below that of appearance of the ringwoodite-structure phase on the XRD images patterns. This suggests that AEs are generated while the transition is still nucleation controlled (pseudo-martensitic stage). During stress-relaxation periods, the rate of AE triggering decreases, but does not completely vanish. The AE production rate increases again as soon as deformation is started again. Importantly, we still observed very large AEs at strain rates as low as approx. 10-5/ s. At these early stages of the transformation, the samples did not show any macroscopic rheological weakening. Focal mechanism analysis of the largest AEs showed that they are all of shear type, some being even pure double couple. They radiate about the same amount of energy as typically recorded during fast crack propagation in amorphous glass material. This suggests that they cannot only originate from the martensitic nucleation of oriented spinel-lamellae within a single germanium olivine crystal. Preliminary microstructural analysis (SEM and EBSD) highlights the presence of thin transformation bands made of incoherent spinel micro-grains which, possibly, run across germanium-olivine grain boundaries. These bands are all oriented near perpendicular to the principal compressive stress. Our observations point out that under high deviatoric stress, the olivine - spinel transition is a source of instability which produces micro-sismicity (no AEs were recorded in a similar experiment performed hydrostatically). These instabilities might eventually be precursor to brittle fracturing as observed by Green and Burnley (1989) in their deformation experiments on very similar samples. Both types of study emphasize the potential of phase transitions (with negative volume variations) in triggering brittle failure. Obviously, this has important consequences for the understanding of deep-focus earthquakes occurring in cold and metastable olivine within the transition zone.

  11. 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.

  12. Magnet Healing?

    NASA Astrophysics Data System (ADS)

    Finegold, Leonard

    2000-03-01

    Many people are convinced that static magnets—applied to their skin—will heal ills, and many businesses sell such magnets. The biophysics of such healing was reviewed [1] together with the general biophysics of static fields. Birds and insects do use the earth’s magnetic field for navigation. While insect and frog egg development can clearly be influenced by high fields (7 T and 17 T respectively), there is no experimental evidence that small magnetic fields (of less than 0.5 T) might heal, and much evidence that they cannot heal. A puzzle to the physics community is: How to show laypersons that simple magnets (very probably) do not heal, however attractive that idea might be. [1] L. Finegold, The Physics of "Alternative Medicine": Magnet Therapy, The Scientific Review of Alternative Medicine 3:26-33 (1999).

  13. 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.

  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 important persistent sources of U(VI) to the associated uranium groundwater plume in Hanford Area 300. PMID:19244994

  15. 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 temperature is reached. Supported Co 3O4 was reduced at 350°C to CoO and Co metal (hcp). Addition of modifiers increases the ratio of cobalt metal obtained as calculated by X-ray intensity ratios.

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

    DOE PAGESBeta

    Bak, Seong -Min; Hu, Enyuan; Zhou, Yongning; Yu, Xiqian; Senanayake, Sanjaya D.; Cho, Sung -Jin; Kim, Kwang -Bum; Chung, Kyung Yoon; Yang, Xiao -Qing; Nam, Kyung -Wan

    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

  17. 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 carried out at the National Synchrotron Light Source (NSLS) at Brookhaven National Laboratory (BNL). NSLS is a national scientific user facility supported by the US DOE.

  18. Fabrication, characterization, and magnetic behavior of porous ZnFe2O4 hollow microspheres

    NASA Astrophysics Data System (ADS)

    Matli, Penchal Reddy; Zhou, Xiaobing; Shiyu, Du; Huang, Qing

    2015-12-01

    Porous ZnFe2O4 hollow microspheres with a diameter of about 100-210 nm were successfully prepared by simple template-free hydrothermal route in ethylene glycol (EG) solution. The formation mechanism and properties have been also demonstrated. The structural, morphological, and magnetic properties of ZnFe2O4 hollow microspheres were investigated by means of X-ray powder diffraction (XRD), field emission scanning electron microscopy, Fourier transform infrared spectroscopy, and physical properties measurements system. The surface area was determined using the BET method. XRD and IR analyses confirm the cubic spinel phase of ZnFe2O4 hollow microspheres. Every magnetic microsphere is made up of many ultrafine ZnFe2O4 nanoparticles with porous structure. The as-prepared porous magnetic hollow spheres have higher surface area and excellent magnetic properties at room temperature.

  19. Preparation and Properties of Various Magnetic Nanoparticles

    PubMed Central

    Drbohlavova, Jana; Hrdy, Radim; Adam, Vojtech; Kizek, Rene; Schneeweiss, Oldrich; Hubalek, Jaromir

    2009-01-01

    The fabrications of iron oxides nanoparticles using co-precipitation and gadolinium nanoparticles using water in oil microemulsion method are reported in this paper. Results of detailed phase analysis by XRD and Mössbauer spectroscopy are discussed. XRD analysis revealed that the crystallite size (mean coherence length) of iron oxides (mainly γ-Fe2O3) in the Fe2O3 sample was 30 nm, while in Fe2O3/SiO2 where the ε-Fe2O3 phase dominated it was only 14 nm. Gd/SiO2 nanoparticles were found to be completely amorphous, according to XRD. The samples showed various shapes of hysteresis loops and different coercivities. Differences in the saturation magnetization (MS) correspond to the chemical and phase composition of the sample materials. However, we observed that MS was not reached in the case of Fe2O3/SiO2, while for Gd/SiO2 sample the MS value was extremely low. Therefore we conclude that only unmodified Fe2O3 nanoparticles are suitable for intended biosensing application in vitro (e.g. detection of viral nucleic acids) and the phase purification of this sample for this purpose is not necessary. PMID:22574017

  20. Preparation of magnetically responsive albumin nanospheres and in vitro drug release studies.

    PubMed

    Ak, Güliz; Yɪlmaz, Habibe; Sanlɪer, Senay Hamarat

    2014-02-01

    In this work, doxorubicin (DOX)-loaded magnetic albumin nanospheres were prepared using desolvation method in order to develop magnetically responsive nanocarrier system. Nanoparticles were characterized with zetasizer, SEM, AFM, XRD and magnetometer. In vitro DOX release was also investigated. It was found that nanoparticles had spherical shape with narrow size distributions and had magnetic responsiveness. In addition, slower drug release was observed with nanoparticulate system compared with free DOX. Moreover, the release rate should accelerate at target sites (cancer cells or tissue) where proteolytic enzymes are more abundant as known; therefore, magnetic albumin nanospheres can be effective potential DOX carrier with targeting ability. PMID:23419121

  1. Effect of Gd substitution on structure and magnetic properties of BiFeO3

    NASA Astrophysics Data System (ADS)

    Suresh, Pittala; Srinath, S.

    2015-02-01

    Multiferroic ceramic samples of GdxB1-xFeO3 (x = 0 - 0.35) have been prepared by solid state reaction method. The results of XRD show a transition from rhombohedral to orthorhombic structure with increase in composition. Ferromagnetic order is observed with an enhanced magnetization (M) and coercivity (Hc) for all the doped samples. Maximum magnetization is observed at the field of 5T for x = 0.3. The temperature dependant magnetization shows the anomalous magnetic behaviour in this system. A minimum in the M-T curve and double hysteresis loop behaviour were observed for the samples with x=0.1 and 0.2

  2. HRTEM study comparing naturally and experimentally weathered pyroxenoids

    NASA Astrophysics Data System (ADS)

    Banfield, Jillian F.; Ferruzzi, Giulio G.; Casey, William H.; Westrich, Henry R.

    1995-01-01

    The mineralogy and chemistry of both naturally and experimentally weathered MnSiO3 chain silicate minerals (rhodonite and pyroxmangite) were compared. In natural MnSiO3, 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 (Ca0.3Mn2.2Zn0.4Al0.1Si4O10(OH)2) also develops in larger etches at grain boundaries. The Zn apparently released by weathering of coexisting sphalerite, may facilitate crystallization of manganesesmectite; rhodochrosite is also an initial product. X-ray diffraction patterns from highly altered materials reveal only rhodochrosite and quartz. Simplified reactions are H2CO3(aq)+4MnSiO3(s)=Mn3Si4O((s)+MnCO3(s) accompanied by 3H2CO3(aq)+Mn3Si4O((s)=3MnCO3(s)+4SiO2(s)+4H2O(1) Pyroxenoid dissolution is incongruent under experimental conditions. A 3-7 nm-thic layer of amorphous silica is present at the mineral surface after ˜ 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. Both natural and experimental reactions produce secondary products by direct modification of the pyroxenoid surface. Manganese does not change oxidation state in the early stages of weathering in either setting. Unlike orthosilicates, compositional variations exert only a secondary control on chain silicate dissolution rates. For all chain silicate minerals, depolymerization of the silicate anion probably limits overall dissolution rates. As the thickness of the modified layer increases, rates may be further suppressed by diffusion (through the leached surface in the case of experimental reactions, and through secondary minerals in the case of natural weathering). The rates for wollastonite are exceptional in that the mineral dissolves more rapidly than other chain silicates and because leaching reactions are more pronounced. Natural surface modification reactions appear to be distinctive in that they occur in the presence of higher concentrations of metal cations. Clay mineral formation may be promoted by periodic drying.

  3. 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.

  4. 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.

  5. Synthesis, spectral, stereochemical, single crystal XRD and biological studies of 3t-pentyl-2r,6c-diarylpiperidin-4-one picrate derivatives

    NASA Astrophysics Data System (ADS)

    Savithiri, S.; Arockia doss, M.; Rajarajan, G.; Thanikachalam, V.

    2014-10-01

    Various substituted 3t-pentyl-2r,6c-diphenylpiperidin-4-one picrates (1-7) were synthesised and characterised by elemental analysis, FT-IR and NMR spectral studies. NMR spectral assignments were made unambiguously by their one dimensional (1H NMR and 13C NMR) and two dimensional (1H-1H COSY, HSQC, HMBC, NOESY, DEPT) NMR spectra. Single crystal XRD analysis of the compound (1) has confirmed that the complex crystallized in monoclinic system with P21/n space group. The difference in the chemical shifts between equatorial methylene proton and axial proton at C(5) [Δ = δeq - δax] is highly negative in compounds 1-7 in contrast to the value observed for the corresponding parent piperidine-4-one and is indicative of the 1,3-diaxial interaction between the axial NH bond and axial hydrogen at C(5). The chemical shifts of the heterocyclic ring protons are influenced by the picrate anion. All the synthesised compounds exhibited good activity against S. aureus-Staphylococcus aureus bacterial strains and C. albicans fungal strains.

  6. Measurement methods for surface oxides on SUS 316L in simulated light water reactor coolant environments using synchrotron XRD and XRF

    NASA Astrophysics Data System (ADS)

    Watanabe, Masashi; Yonezawa, Toshio; Shobu, Takahisa; Shoji, Tetsuo

    2013-03-01

    Synchrotron X-ray diffraction (XRD) and X-ray fluorescent (XRF) measurement techniques have been used for non-destructive characterization of surface oxide films on Type 316L austenitic stainless steels that were exposed to simulated primary water environments of pressurized water reactors (PWR) and boiling water reactors (BWR). The layer structures of the surface spinel oxides were revealed ex situ after oxidation by measurements made as a function of depth. The layer structure of spinel oxides formed in simulated PWR primary water should normally be different from that formed in simulated BWR water. After oxidation in the simulated BWR environment, the spinel oxide was observed to contain NiFe2O4 at shallow depths, and FeCr2O4 and Fe3O4 at deeper depths. By contrast, after oxidation in the simulated PWR primary water environment, a Fe3O4 type spinel was observed near the surface and FeCr2O4 type spinel near the interface with the metal substrate. Furthermore, by in situ measurements during oxidation in the simulated BWR environment, it was also demonstrated that the ratio between spinel and hematite Fe2O3 can be changed depending on the water condition such as BWR normal water chemistry or BWR hydrogen water chemistry.

  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. Determinants for Tight and Selective Binding of a Medicinal Dicarbene Gold(I) Complex to a Telomeric DNA G-Quadruplex: a Joint ESI MS and XRD Investigation.

    PubMed

    Bazzicalupi, Carla; Ferraroni, Marta; Papi, Francesco; Massai, Lara; Bertrand, Benoît; Messori, Luigi; Gratteri, Paola; Casini, Angela

    2016-03-18

    The dicarbene gold(I) complex [Au(9-methylcaffein-8-ylidene)2 ]BF4 is an exceptional organometallic compound of profound interest as a prospective anticancer agent. This gold(I) complex was previously reported to be highly cytotoxic toward various cancer cell lines in vitro and behaves as a selective G-quadruplex stabilizer. Interactions of the gold complex with various telomeric DNA models have been analyzed by a combined ESI MS and X-ray diffraction (XRD) approach. ESI MS measurements confirmed formation of stable adducts between the intact gold(I) complex and Tel 23 DNA sequence. The crystal structure of the adduct formed between [Au(9-methylcaffein-8-ylidene)2 ](+) and Tel 23 DNA G-quadruplex was solved. Tel 23 maintains a characteristic propeller conformation while binding three gold(I) dicarbene moieties at two distinct sites. Stacking interactions appear to drive noncovalent binding of the gold(I) complex. The structural basis for tight gold(I) complex/G-quadruplex recognition and its selectivity are described. PMID:26929051

  9. 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. PMID:26450690

  10. 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

    2015-08-01

    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. PMID:26073651

  11. Effect of light elements (S, Si, C, O) on liquid iron alloys structural properties under high pressure studied by XRD, XANES and molecular dynamics

    NASA Astrophysics Data System (ADS)

    Morard, G.; Andrault, D.; Antonangeli, D.; Siebert, J.; Guyot, F. J.; Auzende, A. L.; Lord, O. T.; Bouchet, J.; Harmand, M.; Cochain, B.; Garbarino, G.; Kantor, I.; Torchio, R.; Boulard, E.; Mezouar, N.

    2014-12-01

    The liquid core of the Earth extends between 2900 km and 5150 km depth accounting for 18% of the total planetary volume. Although mostly composed of iron, it contains impurities that lower its density and melting point with respect to pure Fe. Knowledge of the nature and content of the light elements (O, S, Si, C) in the core has major implications for establishing the bulk composition of the Earth and for building models of Earth's differentiation. We will present XRD and XANES experimental results on liquid iron alloys measured using the Laser-Heated Diamond Anvil Cell (LH-DAC) up to megabar conditions, obtained respectively on ESRF beamlines ID27 and ID24. Measurements have been performed on different samples : Fe-10 wt%O ; Fe-10wt% Si ; Fe-5wt%Ni-12wt%S ; Fe-1.5wt% C. Using this dataset, we are able to probe the electronic structure and crystallographic structures of these iron alloys from solid phases up to the liquid state. Comparison between these measurements and ab initio calculations of the local structure of these liquids, allows us to discuss how the different light elements S, Si, O and C affect the properties of liquid iron alloys.

  12. A conjoint XRD-ND analysis of the crystal structures of austenitic and martensitic Ti 0.64Zr 0.36Ni hydrides

    NASA Astrophysics Data System (ADS)

    Cuevas, F.; Latroche, M.; Bourée-Vigneron, F.; Percheron-Guégan, A.

    2006-11-01

    The crystal structures of the hydrides of austenitic and martensitic Ti 0.64Zr 0.36Ni alloy have been investigated by conjoint X-ray diffraction (XRD)-neutron diffraction (ND) analysis. Austenitic Ti 0.64Zr 0.36Ni alloy with cubic CsCl-type structure preserves its metal sublattice structure after deuteration. It forms a Ti 0.64Zr 0.36NiD 1.5 deuteride with D-atoms occupying half of the octahedrally coordinated 3 d sites. On the contrary, the monoclinic TiNi-type structure of martensitic Ti 0.64Zr 0.36Ni alloy is modified after deuterium absorption. At P=103 Pa and T=298 K, two deuterides coexist with orthorhombic CrB-type structure for the metal sublattice and compositions Ti 0.64Zr 0.36NiD ( β-deuteride) and Ti 0.64Zr 0.36NiD 2.6 ( γ-deuteride). For the β-monodeuteride, deuterium atoms are tetrahedrally coordinated by (Ti,Zr) atoms. For the γ-deuteride, D-atoms fully occupy tetrahedrally coordinated (Ti,Zr) 3Ni 8 f sites and partially occupy pyramidal (Ti,Zr) 3Ni 2 4 c sites. At higher pressures, deuterium solution occurs in the γ-phase with a partial occupancy of octahedrally coordinated (Ti,Zr) 2Ni 4 4 a sites.

  13. 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. PMID:15701375

  14. 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.

  15. GREGÓRIO LOPES painting workshop: characterization by X-ray based techniques. Analysis by EDXRF, μ-XRD and SEM-EDS

    NASA Astrophysics Data System (ADS)

    Antunes, V.; Candeias, A.; Carvalho, M. L.; Oliveira, M. J.; Manso, M.; Seruya, A. I.; Coroado, J.; Dias, L.; Mirão, J.; Longelin, S.; Serrão, V.

    2014-05-01

    Gregório Lopes is one of the most famous Portuguese painters of the 15th-16th centuries. This work is a contribution to the study of his painting technique, specifically addressing the methodology used in the preparation of ground layers, which has never been carried out previously with this multianalytical method. For this purpose characterization of the ground layers of a selection of his paintings was carried out by micro-Energy Dispersive X-ray Fluorescence spectroscopy (μ-EDXRF), micro-X-ray Diffraction (μ-XRD), Scanning Electron Microscopy - Energy Dispersive Spectroscopy (SEM-EDS) and complemented by micro-Raman spectroscopy. This work presents the results obtained on two altarpieces (c.1544) produced at the same period by this Portuguese artist. Ground layers are composed mainly of calcium sulfate — anhydrite and gypsum — and other compounds such as dolomite. Reference samples were prepared to obtain diffraction pattern of different percentage of gypsum and anhydrite and compared with the results from historical samples.

  16. 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. PMID:24096063

  17. 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.

  18. A Highly Sensitive and Efficient Functionalized Magnetic Chemosensor for Cu2+ Removal

    NASA Astrophysics Data System (ADS)

    Kong, Xiangfeng; Chen, Yuxiang; Yang, Zaixiang; Wang, Shixing; Zhou, Yang

    Fe3O4 nanoparticles were covalently functionalized by N-(quinoline-8-yl)-2-(3-triethoxysilyl-propylamino)- acetamide (QTPA), and finally utilized to be magnetic chemosensor for sensitive and efficient Cu2+ removal in aqueous solution. Fourier FT-IR, TEM, XRD and XPS results showed that QTPA was bonded to the surface of Fe3O4 nanoparticles. At room temperature, the magnetic chemosensor exhibited high removal efficiency towards Cu2+.

  19. 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.

  20. 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.

  1. Magnetic disk

    NASA Technical Reports Server (NTRS)

    Mallinson, John C.

    1991-01-01

    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 has halved and doubled, respectively every 2 to 2 1/2 years. Today, the cost per byte is lower than 10(exp -6) dollars per byte and area densities exceed 100 x 10(exp 6) bits per square inch. The recent achievements in magnetic disk recording will first be surveyed briefly. Then the principal areas of current technical development will be outlined. Finally, some comments will be made about the future of magnetic disk recording.

  2. Magnetic Properties of Core/Shell Structured Iron/Iron-oxide Nanoparticles Dispersed in Polymer Matrix

    NASA Astrophysics Data System (ADS)

    Nemati Porshokouh, Zohreh; Khurshid, Hafsa; Phan, Manh-Huong; Srikanth, Hariharan

    2014-03-01

    Iron-based nanoparticles (NPs) show interesting magnetic properties for a wide range of applications; however rapid oxidation of iron limits its practical use. Protecting iron with a thin layer of iron-oxide is a possible way to prevent oxidation, forming core/shell (CS) iron/iron-oxide. Due to the different diffusivity rates of the two materials, a gap appears between the core and shell after a period of time (Kirkendall effect), degrading the magnetic properties of the sample. We minimize the Kirkendall effect while retaining good magnetic properties of ~12.5 nm CS iron/iron-oxide NPs by dispersing them into a polymer matrix. Magnetic measurements reveal that after a period of 3 months the blocking temperature (TB) of as-made CS NPs decreases from 107 K to 90 K. The change in TB marks the formation of a gap between the core and shell, which is also evident from HRTEM studies. By contrast, NPs dispersed in RP show no change in TB over the same time period. We repeated experiments with ~10.5 nm CS NPs and the results are consistent. Our study shows the importance of dispersing CS NPs in polymers to preserve desirable magnetic properties for practical applications, ranging from RF sensors and microwave devices to bioengineering.

  3. Magnetization and stability study of a cobalt-ferrite-based ferrofluid

    NASA Astrophysics Data System (ADS)

    Kamali, Saeed; Pouryazdan, Mohsen; Ghafari, Mohammad; Itou, Masayoshi; Rahman, Masoud; Stroeve, Pieter; Hahn, Horst; Sakurai, Yoshiharu

    2016-04-01

    In this study the structural and magnetization properties of a CoFe2O4-based ferrofluid was investigated using x-ray diffraction (XRD), transmission electron microscopy (TEM), energy dispersive x-ray spectroscopy (EDS), Mössbauer spectroscopy, and magnetic Compton scattering (MCS) measurements. The XRD diagram indicates that the nanoparticles in the ferrofluid are inverse spinel and TEM graph shows that the ferrofluid consists of spherical nanoparticles with an average diameter of 18± 1 nm, in good agreement with the size, 19.4 nm, extracted from line broadening of the XRD peaks. According to EDS measurements the composition of the nanoparticles is CoFe2O4. Mössbauer spectroscopy shows that the cation distributions are (Co0.38Fe0.62)[Co0.62Fe1.38]O4. The MCS measurement, performed at 10 K, indicates that the magnetization of the nanoparticles is similar to magnetization of maghemite and magnetite. While the magnetization of the inverse spinels are in [111] direction, interestingly, the magnetization deduced from MCS is in [100] direction. The CoFe2O4-based ferrofluid is found to be stable at ambient conditions, which is important for applications.

  4. 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.

  5. 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)

  6. 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)

  7. Ferro- and antiferro-magnetism in (Np, Pu)BC

    NASA Astrophysics Data System (ADS)

    Klimczuk, T.; Shick, A. B.; Kozub, A. L.; Griveau, J.-C.; Colineau, E.; Falmbigl, M.; Wastin, F.; Rogl, P.

    2015-04-01

    Two new transuranium metal boron carbides, NpBC and PuBC, have been synthesized. Rietveld refinements of powder XRD patterns of {Np,Pu}BC confirmed in both cases isotypism with the structure type of UBC. Temperature dependent magnetic susceptibility data reveal antiferromagnetic ordering for PuBC below TN = 44 K, whereas ferromagnetic ordering was found for NpBC below TC = 61 K. Heat capacity measurements prove the bulk character of the observed magnetic transition for both compounds. The total energy electronic band structure calculations support formation of the ferromagnetic ground state for NpBC and the antiferromagnetic ground state for PuBC.

  8. Magnetic properties of graphite oxide and reduced graphene oxide

    NASA Astrophysics Data System (ADS)

    Sarkar, S. K.; Raul, K. K.; Pradhan, S. S.; Basu, S.; Nayak, A.

    2014-11-01

    Graphite oxide (GO) and reduced graphene oxide (RGO) have been prepared using standard chemical methods. The formations of the oxides are characterized by X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) studies. Both the oxides exhibit weak superparamagnetism and hysteresis for the first time at room temperature. Magnetic moment for RGO is comparatively smaller than that of GO sample. The superparamagnetism in these oxides is attributed to the presence of single domains, each domain being cluster of defect induced magnetic moments coupled by ferromagnetic interaction. Apart from these single domain clusters there are other defect induced moments coupled by ferromagnetic interaction which show ferromagnetism and hysteresis.

  9. 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.

  10. Three-dimensional atom probe analysis and magnetic properties of Fe85Cu1Si2B8P4 melt spun ribbons

    NASA Astrophysics Data System (ADS)

    Jafari, S.; Beitollahi, A.; Eftekhari Yekta, B.; Ohkubo, T.; Budinsky, Viktoria; Marsilius, Mie; Mollazadeh, S.; Herzer, Giselher; Hono, K.

    2016-03-01

    The effect of phosphorous on the microstructure and magnetic properties of as-spun and flash annealed (389-535 °C for 7 s) Fe85Cu1Si2B8P4 melt spun ribbons were investigated by three-dimensional atom probe (3DAP) and high resolution transmission electron microscopy (HRTEM) techniques. The formation of quasi-amorphous α -Fe clusters of 3-5 nm size in an amorphous matrix were detected by HRTEM, despite the high quenching rate applied by high wheel speed used. Flash annealing of the as-spun ribbons gave rise to the formation of nanocrystalline α-Fe (Si) phase in amorphous matrix containing Fe, Si, B and P elements as detected by 3DAP. Comparing 3DAP analysis of the samples annealed at 445 °C and 535 °C revealed that the concentration of P and B in amorphous matrix were increased for the latter. Further, it was shown that P hardly solidified into nanocrystalline phase and partitioned in amorphous phase alongside B atoms leading to the further stabilization of amorphous matrix as confirmed by 3DAP analysis. The highest magnitude of saturation magnetic induction (Bs~1.85 T) and the lowest coercive field (~10-20 A/m) were obtained for the samples annealed above 445 °C, for which noticeable reduction of saturation magnetostriction (λ s) were also detected.

  11. 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.

  12. 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

    2016-01-01

    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 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. PMID:26616162

  13. Magnetic mineralogy of heavy metals-contaminated soils

    NASA Astrophysics Data System (ADS)

    Shenggao, L.

    2012-04-01

    Soils around mine and in urban areas are often contaminated by heavy metals derived from industrial and human activities [1, 2]. These contaminated soils are often characterized by a magnetic enhancement on topsoils. Many studies demonstrated that there are significant correlations between heavy metals and various magnetic parameters in contaminated soils, indicating a strong affinity of heavy metals to magnetic minerals. The magnetic particles in contaminated soils were separated by a magnetic separation technique. The rock magnetism, XRD, field emission scanning electron microscopy equiped with an energy-dispersive X-ray analyzer (FESEM/EDX) were used to characterize their magnetic mineralogy. Results of XRD analysis indicated that the magnetic particles separated from heavy metal-contaminated soils are composed of quartz, magnetite, and hematite. Based on the X-ray diffraction peak intensity, the Fe3O4 was identified as the predominant magnetic mineral phase. The high-temperature magnetization (Ms-T) curves of magnetic particles extracted from contaminated soils show a sharp Ms decrease at about 580C (the Curie temperature of magnetite), suggesting that magnetite is the dominant magnetic carrier. The hysteresis loops of contaminated soils are closed at about 100-200 mT which is consistent with the presence of a dominant ferrimagnetic mineral phase. The FESEM analysis showed a great variety of shapes of magnetic particles in contaminated soils. The most common morphology are observed in the form of spherules, with the sizes ranging from 20 to 100 um. The chemical composition of magnetic particles consist mainly of Fe, Si, Al, and Ca with minor heavy metal elements (Cu, Zn, Hg, and Cr). The semi-quantitative Fe content identified by FESEM/EDX ranged from 40 to 90%. Combined studies of rock magnetism, XRD, and FESEM/EDX indicated that magnetic mineral phases responsible for the magnetic enhancement of contaminated soils are anthropogenic origin which are coarse-grained multi-domain (MD) ferrimagnetic minerals. These spherical magnetic particles in contaminated soils are most likely related to airborne particles from coal combusition and industrial activities. Coal burning, metallurgical and industrial dusts contain a significant fraction of ferrimagnetic minerals. The magnetic particles in fly ash from coal-burning power plant have a typical spherical morphology, ranging from 10 to 100 μm. Vehicle emissions have been suggested to be another source of magnetic particles. These anthropogenic ferrimagnetic mineral phases are directly responsible for the magnetic enhancement in the contaminated soils. Therefore, the strong magnetic signature in contaminated soils can be used as an effective tool for identifying pollution sources and quantifying pollution level of heavy metals. Acknowledgements: This research was supported by National Nature Science Foundation of China (No. 41171182 and 40971131) and the Ph.D. Programs Foundation of Ministry of Education of China (20090101110088). [1] Lu, S.G. & Bai, S.Q. (2006) J. Appl. Geophys., 60, 1-12. [2] Lu, S.G., Bai, S.Q. & Xue, Q.F. (2007) Geophys. J. Inter., 171, 568-580.

  14. 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 provide accurate and definitive mineralogical data of complex multi-mineral mixtures. Definitive mineralogical data will be highly useful in interpreting brine chemistry and the nature and extent of the ancient habitable zone that existed there. [1]. MER Rover web site (http://www.jpl.nasa.gov/mer2004/rover-images/mar-02-2004/images-3-2-04.html [2]. Kerr, R. A. (2004), "A wet early Mars seen in salty deposits," Science 303, 1450. [3]. Feldman, W. C., et al. (2003), "The global distribution of near-surface hydrogen on Mars," In: Sixth Int. Conf. on Mars, abstract #3218, Lunar and Planetary Institute, Houston (CD-ROM). [4]. Blake, D.F., P. Sarrazin, D.L. Bish, S. Feldman, S.J. Chipera, D.T. Vaniman, and S.A. Collins (2004), "Definitive Mineralogical Analysis of Mars Analogs Using the CheMin XRD/XRF Instrument," Lunar and Planetary Science Conf XXXV, abstr. #1373 (CD-ROM).

  15. Mercury Retention and Accumulation by Plants at the Abandoned New Idria Mine Site - a Preliminary micro-XRF and micro-XRD Study

    NASA Astrophysics Data System (ADS)

    Siebner, H.; Webb, S. M.; Brown, G. E.

    2008-12-01

    Due to its high toxicity and increasing levels in ecosystems, Hg pollution has become a serious global problem. A lot of research has been conducted with regard to Hg biogeochemical cycles in aquatic systems. Much less is known about terrestrial Hg-cycles in general and in plants specifically. Plants play an important role in these cycles; they are known to be an important sink for both atmospheric and soil Hg, the vegetative cover significantly influences soil erosion and migration of contaminants into aquatic systems. However, the processes involved in the interactions of Hg with plants and plants products are poorly studied. Information concerning the interaction of Hg in plants at the molecular level is sparse. The present study is intended to provide new information on Hg retention, translocation, and accumulation in plants associated with mercury mine wastes in central California. We present here preliminary results of Hg distribution in root and leave samples, taken from different plant species, which have adapted to the hostile environment at the New Idria site. Samples were taken at two locations that differ in water acidity and flooding regime. The distribution of Hg appears to be affected by plant species, growing conditions, and development stage. Micro-XRF images of root sections show that Hg is mainly associated with Fe plaque at the outer surfaces and epidermis, but is distributed differently in roots of the two plants. Micro-XRD showed evidence for mineralogical changes in the plaque through the sections. Mercury in leaves was found to be highly diffuse in its distribution, and is not associated with Fe-rich particles attached to the outer surface of the leaf. This finding implies that Hg is assimilated in the leaf tissue. Further examination of Fe plaque characteristics and associated Hg, as well as Hg speciation in the different organs of these plants, is being conducted in our lab.

  16. Single crystal XRD, vibrational spectra, quantum chemical and thermal studies on a new semi-organic crystal: 4-Aminium antipyrine chloride

    NASA Astrophysics Data System (ADS)

    Chitradevi, A.; Suresh Kumar, S.; Athimoolam, S.; Asath Bahadur, S.; Sridhar, B.

    2015-11-01

    The new semi-organic crystal of 4-aminium antipyrine chloride was grown as a single crystal by slow evaporation solution growth method. The crystal and molecular structure of the grown crystal was determined by single crystal diffraction techniques. The single crystal XRD studies reveal that the phenyl ring and pyrazolone ring of the cation has been inclined at an angle of 52.3 (1)°. The molecular aggregations were stabilized through intricate three dimensional hydrogen bonding network formed by the classical N-H⋯O and N-H⋯Cl hydrogen bonds. The cationic dimer R22(10) motif formed through N-H⋯O intermolecular hydrogen bonds was observed around the inversion center of the unit cell. The amino group from the cation and the chlorine anion was linked through N-H⋯Cl intermolecular hydrogen bond leading to a R24 (8) ring motif. These two ring motifs were extended along the a-axis of the unit cell and forms a hydrophilic layer at z = 0 and 1, which is sandwiched between the hydrophobic layer at z = 1/2. Geometry optimization of the molecules was done by Density Functional Theory (DFT) using the B3LYP function and Hartree-Fock (HF) level with 6-311++G(d,p) basis set. The optimized molecular geometry and computed vibrational spectra were compared with experimental results which show a significant agreement. The natural bond orbital (NBO) analysis was carried out to interpret hyperconjucative interaction and intramolecular charge transfer (ICT). The chemical hardness, electro-negativity and chemical potential of the molecule were carried out by HOMO-LUMO plot. The lower band gap value of the frontier orbitals shows the possible bioactivity of the molecule.

  17. 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.

  18. A MS, SEM-EDX and XRD study of Ti or Cu-doped zinc ferrites as regenerable sorbents for hot coal gas desulfurization

    NASA Astrophysics Data System (ADS)

    Ahmed, M. A.; García, E.; Alonso, L.; Palacios, J. M.

    2000-02-01

    Kinetic studies in thermobalance carried out by several authors previously have shown that small concentrations of TiO 2 or CuO can increase substantially the overall sulfidation rate of zinc ferrites, as regenerable sorbents for hot coal gas desulfurization. These oxides modify the textural properties of both the fresh or regenerated and the sulfided sorbent, modifying consequently the sulfidation rate because it is a partially diffusion-controlled process. However, by using grain models it is shown that most of the observed changes are due to changes in the intrinsic reactivity of the sorbent. Detailed studies of characterization in previous papers using different techniques have failed in revealing differential chemical changes that could be associated with a different behavior. In fact, the only significant changes observed in these studies were an apparent disappearance in fresh sorbents calcined at very high temperatures of the Raman effect, and a slight shift of the XPS binding energy of Fe levels, indicating a probable site migration and/or a change of the oxidation state. These characterization results, however, were not completely conclusive and additional efforts should be undertaken. In this paper more sensitive techniques such as Mössbauer spectroscopy (MS), powder X-ray diffraction (XRD) and scanning electron microscopy (SEM-EDX), have been used for the characterization of fresh, regenerated and sulfided sorbents. The study shows that the addition of TiO 2 or CuO induce substantial structural changes in zinc ferrites that can explain their apparent enhancing effect on the overall sulfidation reactivity. Additionally, this effect is decreased as the number of sulfidation-regeneration cycles increases, probably explaining the performance decay exhibited by these sorbents in multicycle tests in a fixed bed reactor.

  19. Synthesis and detection the oxidization of Co cores of Co@SiO2 core-shell nanoparticles by in situ XRD and EXAFS.

    PubMed

    Zhang, Kunhao; Zhao, Ziyan; Wu, Zhonghua; Zhou, Ying

    2015-01-01

    In this paper, the Co@SiO2 core-shell nanoparticles were prepared by the sol-gel method. The oxidization of Co core nanoparticles was studied by the synchrotron radiation-based techniques including in situ X-ray diffraction (XRD) and X-ray absorption fine structure (XAFS) up to 800°C in air and N2 protection conditions, respectively. It was found that the oxidization of Co cores is undergoing three steps regardless of being in air or in N2 protection condition. In the first step ranging from room temperature to 200°C, the Co cores were dominated by Co(0) state as well as small amount of Co(2+) ions. When temperature was above 300°C, the interface between Co cores and SiO2 shells was gradually oxidized into Co(2+), and the CoO layer was observed. As the temperature increasing to 800°C, the Co cores were oxidized to Co3O4 or Co3O4/CoO. Nevertheless, the oxidization kinetics of Co cores is different for the Co@SiO2 in air and N2 gas conditions. Generally, the O2 in the air could get through the SiO2 shells easily onto the Co core surface and induce the oxidization of the Co cores due to the mesoporous nature of the SiO2 shells. However, in N2 gas condition, the O atoms can only be from the SiO2 shells, so the diffusion effect of O atoms in the interface between Co core and SiO2 shell plays a key role. PMID:25852334

  20. Adsorption and separation of light gases on an amino-functionalized metal-organic framework: an adsorption and in situ XRD study.

    PubMed

    Couck, Sarah; Gobechiya, Elena; Kirschhock, Christine E A; Serra-Crespo, Pablo; Juan-Alcañiz, Jana; Martinez Joaristi, Alberto; Stavitski, Eli; Gascon, Jorge; Kapteijn, Freek; Baron, Gino V; Denayer, Joeri F M

    2012-04-01

    The NH(2)-MIL-53(Al) metal-organic framework was studied for its use in the separation of CO(2) from CH(4), H(2), N(2)C(2)H(6) and C(3)H(8) mixtures. Isotherms of methane, ethane, propane, hydrogen, nitrogen, and CO(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(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(2) interacted much more strongly and was adsorbed in significant amounts at low pressure. This gives the material excellent properties to separate CO(2) from other gases. The separation of CO(2) from methane, nitrogen, hydrogen, or a combination of these gases has been demonstrated by breakthrough experiments using pellets of NH(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(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(2)-MIL-53(Al) pellets retained their selectivity and capacity for more than two years. PMID:22378615

  1. 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.

  2. Optical response and magnetic characteristic of samarium doped zinc phosphate glasses containing nickel nanoparticles

    NASA Astrophysics Data System (ADS)

    Azmi, Siti Amlah M.; Sahar, M. R.

    2015-11-01

    A magnetic glass of composition 40ZnO-(58-x) P2O5-1Sm2O3-xNiO, with x=0.0, 1.0, 1.5 and 2.0 mol% is prepared by melt-quenching technique. The glass is characterized by X-ray diffraction, high-resolution transmission electron microscope (HRTEM), photoluminescence (PL) spectroscopy and vibrating sample magnetometer (VSM) analysis. The X-rays diffraction confirms the amorphous nature of the glass while the HRTEM analysis reveals the presence of nickel nanoparticles in the glass samples. High-resolution TEM reveals that the lattice spacing of nickel nanoparticles is 0.35 nm at (100) plane. Photoluminescence emission shows the existence of four peaks that correspond to the transition from the upper level of 4G5/2 to the lower level of 6H5/2, 6H7/2, 6H9/2, and 6H11/2. It is observed that all peaks experience significant quenching effect with the increasing concentration of nickel nanoparticles, suggesting a strong energy transfer from excited samarium ions to the nickel ions. The glass magnetization and susceptibility at 12 kOe at room temperature are found to be in the range of (3.87±0.17×10-2-7.19±0.39×10-2) emu/g and (3.24±0.16×10-6-5.99±0.29×10-6) emu/Oe g respectively. The obtained hysteresis curve indicates that the glass samples are paramagnetic materials. The studied glass can be further used towards the development of magneto-optical functional glass.

  3. Comparison of two kinds of magnetic nanoparticles in vivo and in vitro.

    PubMed

    Wang, Liu; Zhang, Yu; Li, Shijun; Wang, Yujuan; Wang, Kaiping

    2012-06-01

    This study compared a new type of polysaccharide-coated magnetic nanoparticles (in which the polysaccharide is derived from Angelica sinensis) with the dextran magnetic nanoparticles in terms of preparation, biocompatibility and tissue distribution in vivo and in vitro in order to examine the potential application of Angelica polysaccharide as a novel carrier in magnetic drug targeting (MDT). Magnetic nanoparticles were prepared by chemical co-precipitation. Their physical and chemical properties were determined by using the transmission electron microscope (TEM), laser particle size analyzer (DLS) and vibrating sample magnetometer (VSM), and their purity and structure by using X-ray diffractometer (XRD) and Fourier transform infrared spectroscopy (FTIR). The atomic absorption spectrometric method was performed for quantification of the iron content in different tissues. Histological sections were stained by Prussian blue staining to observe the disposition of magnetic nanoparticles in the liver and kidney. The results showed that both kinds of magnetic nanoparticles possessed small particle size, good dispersion and good magnetic properties. XRD showed the main component of the two magnetic nanoparticles was Fe(3)O(4) crystals, and FTIR proved Fe(3)O(4) was successfully coated by each polysaccharide, respectively. In vivo, Fe(3)O(4)-dextran accumulated in the liver, spleen and lung and Fe(3)O(4)-Angelica polysaccharide only in the spleen and lung. It was concluded that Angelica polysaccharide may be applied as a novel carrier in the preparation of magnetic nanoparticles. PMID:22684573

  4. Preparation and characterization of magnetic levan particles as matrix for trypsin immobilization

    NASA Astrophysics Data System (ADS)

    Maciel, J. C.; Andrad, P. L.; Neri, D. F. M.; Carvalho, L. B.; Cardoso, C. A.; Calazans, G. M. T.; Albino Aguiar, J.; Silva, M. P. C.

    2012-04-01

    Magnetic levan was synthesized by co-precipitating D-fructofuranosyl homopolysaccharide with a solution containing Fe2+ and Fe3+ in alkaline conditions at 100 °C. The magnetic levan particles were characterized by scanning electron microscopy (SEM), magnetization measurements, X-ray diffractometry (XRD) and infrared spectroscopy (IR). Afterwards, magnetic levan particles were functionalized by NaIO4 oxidation and used as matrices for trypsin covalent immobilization. Magnetite and magnetic levan particles were both heterogeneous in shape and levan-magnetite presented bigger sizes compared to magnetite according to SEM images. Magnetic levan particles exhibited a magnetization 10 times lower as compared to magnetite ones, probably, due to the coating layer. XRD diffractogram showed that magnetite is the dominant phase in the magnetic levan. Infrared spectroscopy showed characteristics absorption bands of levan and magnetite (O-H, C-O-C and Fe-O bonds). The immobilized trypsin derivative was reused 10 times and lost 16% of its initial specific activity only. Therefore, these magnetic levan particles can be proposed as an alternative matrices for enzyme immobilization.

  5. Magnetism. Blowing magnetic skyrmion bubbles.

    PubMed

    Jiang, Wanjun; Upadhyaya, Pramey; Zhang, Wei; Yu, Guoqiang; Jungfleisch, M Benjamin; Fradin, Frank Y; Pearson, John E; Tserkovnyak, Yaroslav; Wang, Kang L; Heinonen, Olle; te Velthuis, Suzanne G E; Hoffmann, Axel

    2015-07-17

    The formation of soap bubbles from thin films is accompanied by topological transitions. Here we show how a magnetic topological structure, a skyrmion bubble, can be generated in a solid-state system in a similar manner. Using an inhomogeneous in-plane current in a system with broken inversion symmetry, we experimentally "blow" magnetic skyrmion bubbles from a geometrical constriction. The presence of a spatially divergent spin-orbit torque gives rise to instabilities of the magnetic domain structures that are reminiscent of Rayleigh-Plateau instabilities in fluid flows. We determine a phase diagram for skyrmion formation and reveal the efficient manipulation of these dynamically created skyrmions, including depinning and motion. The demonstrated current-driven transformation from stripe domains to magnetic skyrmion bubbles could lead to progress in skyrmion-based spintronics. PMID:26067256

  6. Adsorptive removal of heavy metals by magnetic nanoadsorbent: an equilibrium and thermodynamic study

    NASA Astrophysics Data System (ADS)

    Shirsath, D. S.; Shirivastava, V. S.

    2015-11-01

    An efficient and new magnetic nanoadsorbent photocatalyst was fabricated by co-precipitation technique. This research focuses on understanding metal removal process and developing a cost-effective technology for treatment of heavy metal-contaminated industrial wastewater. In this investigation, magnetic nanoadsorbent has been employed for the removal of Zn(II) ions from aqueous solutions by a batch adsorption technique. The adsorption equilibrium data fitted very well to Langmuir and Freundlich adsorption isotherm models. The thermodynamics of Zn(II) ions adsorption onto the magnetic nanoadsorbents indicated that the adsorption was spontaneous, endothermic and physical in nature. Surface morphology of magnetic nanoadsorbent by scanning electron microscopy (SEM) and elemental analysis by EDX technique. The structural and photocatalytic properties of magnetic nanoadsorbent were characterized using X-ray diffraction (XRD) and FTIR techniques. Also, the magnetic properties of synthesized magnetic nanoadsorbent were determined by vibrating spinning magnetometer (VSM).

  7. 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.

  8. Magnetic Properties of CoFe_2O4 and Fe_3O_4

    NASA Astrophysics Data System (ADS)

    Rodriguez, Robert; Chan, T.; Kenning, G. G.; Huang, L.; Yan, Y.

    2002-03-01

    In order to optimize the magnetization of magnetic nanoparticles for use as Magnetic Resonance Imaging contrast agents and other in vivo biological applications, we have synthesized CoFe_2O_4(Liu, C.; Bingsuo, Z.; Rondinone, A.J.; Zhang, Z.J. J. Am. Chem. Soc.) 122, 6263 (2000). and Fe_3O_4(Shen, T.; Weissleder, R.; Papisov, M.; Bogdanov, A.; Brady, T. MRM) 29, 599 (1993). magnetic nanoparticles of sizes 5, 8, and 11nm using water-in-oil reverse micelles. Size was determined using Dynamic Light Scattering (DLS), X-Ray Diffraction (XRD), and High Pressure Liquid Chromatography (HPLC). Magnetic properties were measure from 10K-340K using SQUID magnetometry. Magnetization as a function of magnetic field has been performed at approximately body temperature ( ~310K) in order to help us determine the optimal size and composition for in vivo application.

  9. Biocellulose-based flexible magnetic paper

    NASA Astrophysics Data System (ADS)

    Barud, H. S.; Tercjak, A.; Gutierrez, J.; Viali, W. R.; Nunes, E. S.; Ribeiro, S. J. L.; Jafellici, M.; Nalin, M.; Marques, R. F. C.

    2015-05-01

    Biocellulose or bacterial cellulose (BC) is a biocompatible (nano) material produced with a three-dimensional network structure composed of microfibrils having nanometric diameters obtained by the Gluconacetobacter xylinus bacteria. BC membranes present relatively high porosity, allowing the incorporation or synthesis in situ of inorganic nanoparticles for multifunctional applications and have been used as flexible membranes for incorporation of magnetic nanocomposite. In this work, highly stable superparamagnetic iron oxide nanoparticles (SPION), functionalized with polyethylene glycol (PEG), with an average diameter of 5 nm and a saturation magnetization of 41 emu/g at 300 K were prepared. PEG-Fe2O3 hybrid was dispersed by mixing a pristine BC membrane in a stable aqueous dispersion of PEG-SPION. The PEG chains at PEG-SPION's surface provide a good permeability and strong affinity between the BC chains and SPION through hydrogen-bonding interactions. PEG-SPION also allow the incorporation of higher content of nanoparticles without compromising the mechanical properties of the nanocomposite. Structural and magnetic properties of the composite have been characterized by XRD, SEM, energy-dispersive X-ray spectroscopy (EDX), magnetization, Raman spectroscopy, and magnetic force microscopy.

  10. New iron-based SiC spherical composite magnetic abrasive for magnetic abrasive finishing

    NASA Astrophysics Data System (ADS)

    Zhang, Guixiang; Zhao, Yugang; Zhao, Dongbiao; Zuo, Dunwen; Yin, Fengshi

    2013-03-01

    SiC magnetic abrasive is used to polish surfaces of precise, complex parts which are hard, brittle and highly corrosion-resistant in magnetic abrasive finishing(MAF). Various techniques are employed to produce this magnetic abrasive, but few can meet production demands because they are usually time-consuming, complex with high cost, and the magnetic abrasives made by these techniques have irregular shape and low bonding strength that result in low processing efficiency and shorter service life. Therefore, an attempt is made by combining gas atomization and rapid solidification to fabricate a new iron-based SiC spherical composite magnetic abrasive. The experimental system to prepare this new magnetic abrasive is constructed according to the characteristics of gas atomization and rapid solidification process and the performance requirements of magnetic abrasive. The new iron-based SiC spherical composite magnetic abrasive is prepared successfully when the machining parameters and the composition proportion of the raw materials are controlled properly. Its morphology, microstructure, phase composition are characterized by scanning electron microscope(SEM) and X-ray diffraction(XRD) analysis. The MAF tests on plate of mold steel S136 are carried out without grinding lubricant to assess the finishing performance and service life of this new SiC magnetic abrasive. The surface roughness( R a) of the plate worked is rapidly reduced to 0.051 μm from an initial value of 0.372 μm within 5 min. The MAF test is carried on to find that the service life of this new SiC magnetic abrasive reaches to 155 min. The results indicate that this process presented is feasible to prepare the new SiC magnetic abrasive; and compared with previous magnetic abrasives, the new SiC spherical composite magnetic abrasive has excellent finishing performance, high processing efficiency and longer service life. The presented method to fabricate magnetic abrasive through gas atomization and rapid solidification presented can significantly improve the finishing performance and service life of magnetic abrasive, and provide a more practical approach for large-scale industrial production of magnetic abrasive.

  11. 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.

  12. 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.

  13. Magnetic direction.

    PubMed

    Duchene, Pam; Muhm, John B

    2005-01-01

    In April 2005, the American Nurses Association (ANA) awarded St. Joseph Hospital, Nashua, NH, its highest honor for excellence in nursing: "Magnet Recognition." The Magnet Recognition Program was developed by the ANA's American Nurses Credentialing Center in the early 1980s to recognize health care organizations that provide the best in nursing care and uphold the tradition of excellence in professional nursing practice. St. Joseph began pursuing Magnet status more than three years ago, starting with a number of enhancements to nursing practices. The hospital worked hard to improve nurse-to-patient staffing and included many of its nurses on the nursing quality council, division advisory, and cultural diversity committees. Magnet program appraisers visited the hospital this January to conduct an intensive, on-site three-day examination. They interviewed patients, staff nurses, physicians, hospital employees, administrators, board members, and nursing leadership to evaluate St. Joseph's nursing care, services, and delivery of care to patients and their families. Soon after, Magnet status was bestowed. PMID:16350902

  14. 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

  15. 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 the origin or provenance of a sample. The search for evidence of extant or extinct life on Mars will initially be a search for evidence of present or past conditions supportive of life (e.g., evidence of water), not for life itself.Results of the first 1,000 sols (Mars days) will be discussed, including the discovery of the first habitable environment on Mars.

  16. [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 point). There is a difference each other of the structure and the texture of the four manner annealing aluminum alloy (the innovation point). There is a little difference at the recrystallization processes course reflectived by the observe results of structure transform and by the examination results of texture transmission. PMID:26117903

  17. 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. PMID:23862449

  18. Sterically induced shape control of magnetite nanoparticles

    NASA Astrophysics Data System (ADS)

    Zhang, Ling; Dou, Yong-Hua; Gu, Hong-Chen

    2006-11-01

    Starlike and flowerlike Fe 3O 4 nanoparticles were synthesized by the pyrolysis method using 1- adamantanecarboxylic acid (ACA) and oleylamine (OLA), ACA and 1-adamantaneamine (AA) as the combined surfactants, respectively. XRD, TEM, HRTEM, PPMS are used to characterize the structure and magnetic property of the as-synthesized nanostructures. Control over the morphology of these nanoparticles was realized by using different surfactants under otherwise similar reaction conditions.

  19. 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.

  20. 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.

  1. Functionalization-induced improvement in magnetic properties of Fe3O4 nanoparticles for biomedical applications

    NASA Astrophysics Data System (ADS)

    Nagesha, Dattatri K.; Plouffe, Brian D.; Phan, Minh; Lewis, Laura H.; Sridhar, Srinivas; Murthy, Shashi K.

    2009-04-01

    Fe3O4 were synthesized nanoparticles by thermal decomposition method with oleic acid as the surfactant, and to make them suitable for aqueous environments, dopamine ligand exchange was carried out on the particles. The nanoparticle size and phase was quantified by transmission electron microscopy (TEM) and x-ray diffraction (XRD), respectively. Superconducting quantum interference device magnetometry confirmed superparamagnetic behavior in both nanoparticles. A surprising and significant increase in the remanence MR, saturation magnetization MS, and blocking temperature TB of the particles was found after dopamine functionalization, even though TEM and XRD studies revealed no change in the particles' size and/or structure. The results are consistent with an increase in the magnetic size of the nanoparticle core induced by the dopamine ligand exchange process. These effects are tentatively attributed to surface bonding effects that alter the canted magnetic state of the Fe3O4 nanoparticles.

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

    SciTech Connect

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

    2011-12-15

    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.

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

    NASA Astrophysics Data System (ADS)

    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.

  4. 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. PMID:22225246

  5. AC magnetic susceptibility and influence of heat treatment on obtaining the nanocrystalline structure for the amorphous alloy of Fe37Co35Nb6B11Si10Cu1 composition

    NASA Astrophysics Data System (ADS)

    Orozco, A.; Caamaño, Z.; Rosales, A.

    2016-02-01

    This work presents a study of AC magnetic susceptibility and the influence of heat treatment on obtaining the nanocrystalline structure for the amorphous alloy of Fe37Co35Nb6B11Si10Cu1 composition. AC magnetic susceptibility at different frequencies and sample lengths, using a variable magnetic field was measured. The influence of heat treatment on obtaining the sample nanocrystalline structure was evidenced by means of XRD technique. The crystallite size, the crystalline volume fraction and the distance between grains for each heat treatment temperature were calculated using the XRD peaks refinement software GSAS. Samples were obtained in the amorphous state by melt spinning technique and all measurements by AC magnetic susceptibility and XRD were performed at room temperature.

  6. 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.

  7. Permanent magnet array for the magnetic refrigerator

    NASA Astrophysics Data System (ADS)

    Lee, S. J.; Kenkel, J. M.; Pecharsky, V. K.; Jiles, D. C.

    2002-05-01

    Recent research into the development of magnetic refrigeration (MR) operating at room temperature has shown that it can provide a reliable, energy-efficient cooling system. To enhance the cooling power of the magnetic refrigerator, it is required to use a magnetic refrigerant material with large magnetocaloric effect (MCE) at the appropriate temperature. Most advanced magnetic refrigerant materials show largest MCE at high applied magnetic fields generated by a superconducting magnet. For application of MCE to air conditioners or household refrigerators, it is essential to develop a permanent magnet array to form a compact, strong, and energy-efficient magnetic field generator. Generating a magnetic field well above the remanence of a permanent magnet material is hard to achieve through conventional designs. A permanent magnet array based on a hollow cylindrical flux source is found to provide an appropriate geometry and magnetic field strength for MR applications.

  8. 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...

  9. 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. PMID:26794944

  10. Nano Ag-doped ZnO particles magnetic, optical and structural studies

    NASA Astrophysics Data System (ADS)

    Shah, A. H.; Manikandan, E.; Ahmed, M. Basheer; Irdosh, M.

    2013-02-01

    In this work, we report the influences of annealing effects were explored on the crystallinity, morphology and magnetic properties of Ag doped ZnO nanoparticles. The XRD, SEM and vibrating sample magnetometer (VSM) were used to characterize the crystal structures, surface morphology and magnetic properties of doped and pure ZnO nanoparticles (NPs). As synthesized and annealed ZnO NPs were found hexagonal wurtzite crystal structure and the grain size increases while lattice strain decreases due to annealing. From TEM observation annealed samples were shown nanorod like structure found with Ag NPs embedded on the surface. Due to annealing effect, Ag-ZnO shows higher saturation magnetization at RT.

  11. 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,

  12. Transmission electron microscopy and ferromagnetic resonance investigations of tunnel magnetic junctions using Co2MnGe Heusler alloys as magnetic electrodes

    NASA Astrophysics Data System (ADS)

    Belmeguenai, M.; Genevois, C.; Zighem, F.; Roussigné, Y.; Chérif, S. M.; Westerholt, K.; El Bahoui, A.; Fnidiki, A.; Moch, P.

    2014-01-01

    HRTEM, nano-beam electronic diffraction, energy dispersive X-rays scanning spectroscopy, Vibrating Sample Magnetometry (VSM) and FerroMagnetic Resonance (FMR) techniques are used in view of comparing (static and dynamic) magnetic and structural properties of Co2MnGe (13 nm)/Al2O3 (3 nm)/Co (13 nm) tunnel magnetic junctions (TMJ), deposited on various single crystalline substrates (a-plane sapphire, MgO(100) and Si(111)). They allow for providing a correlation between these magnetic properties and the fine structure investigated at atomic scale. The Al2O3 tunnel barrier is always amorphous and contains a large concentration of Co atoms, which, however, is significantly reduced when using a sapphire substrate. The Co layer is polycrystalline and shows larger grains for films grown on a sapphire substrate. The VSM investigation reveals in-plane anisotropy only for samples grown on a sapphire substrate. The FMR spectra of the TMJs are compared to the obtained ones with a single Co and Co2MnGe films of identical thickness deposited on a sapphire substrate. As expected, two distinct modes are detected in the TMJs while only one mode is observed in each single film. For the TMJ grown on a sapphire substrate the FMR behavior does not significantly differ from the superposition of the individual spectra of the single films, allowing for concluding that the exchange coupling between the two magnetic layers is too small to give rise to observable shifts. For TMJs grown on a Si or on a MgO substrate the resonance spectra reveal one mode which is nearly identical to the obtained one in the single Co film, while the other observed resonance shows a considerably smaller intensity and cannot be described using the magnetic parameters appropriate to the single Co2MnGe film.

  13. Seed-mediated synthesis, properties and application of ?-Fe 2O 3-CdSe magnetic quantum dots

    NASA Astrophysics Data System (ADS)

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

    2011-08-01

    Seed-mediated growth of fluorescent CdSe quantum dots (QDs) around ?-Fe 2O 3 magnetic cores was performed at high temperature (300 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.

  14. Anomalous magnetic behaviour of zinc and chromium ferrites without any hyperfine splitting

    NASA Astrophysics Data System (ADS)

    Pandey, B.; Verma, H. C.

    2008-04-01

    Two groups of ferrite namely zinc ferrite and chromium ferrite were synthesized by citrate precursor route in the size range of 8 to 35 nm. We have studied the structural and magnetic behaviour of these ferrites using X-ray diffraction (XRD), vibrating sample magnetometer (VSM) and Mössbauer spectroscopic techniques. Our studies show that the nanocrystalline ferrites interact with the hand magnet strongly and give large magnetization in the VSM measurement. The maximum magnetization in the samples sensitively depends on the particle size of synthesized ferrites. We observed as large as 28 Am2/kg of magnetization in the zinc ferrite nanoparticles while that in chromium ferrite is around 11 Am2/kg. In spite of the large magnetization in the zinc ferrite nanoparticles we did not observe any hyperfine splitting even down to 12 K of temperature. Similar behaviour is also observed for chromium ferrite down to 16 K.

  15. 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.

  16. (Zn,Co)O alloyed magnetic semiconductor: giant magnetization and experimental determination of band structure

    NASA Astrophysics Data System (ADS)

    Liu, Guolei

    2014-03-01

    Magnetic semiconductor exhibits both ferromagnetism and semiconductor properties. Since the magnetic dopants tend to aggregate in, the thermo-dynamical miscibility of transition metals in semiconductors is in fact extremely low (generally <15%, in diluted region). The miscibility of transition metals exceeding diluted region is challenge for material science and future spintronic applications. In this paper, we have been grown (Zn,Co)O thin films by oxygen plasma-assisted molecular beam epitaxy. The Co context in these films can be up to 45%, which we defined as alloyed magnetic semiconductor (AMS). The measurements of RHEED, XRD and in. situ. XPS indicated that (Zn, Co)O films are spinodal decomposition phase with ZnO wurtzite lattice. The saturated magnetization at room temperature was remarkably enhanced with increasing the Co content. It reach 530emu/cm3 at x = 45% which corresponds to the average magnetic moment 1.6μB per Co. The electronic band structure of (Zn,Co)O films were determined by angle resolved photoemission. the NSF Grant NO. 11374189 and 51231007.

  17. Magnetic liposomes for colorectal cancer cells therapy by high-frequency magnetic field treatment.

    PubMed

    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

    2014-01-01

    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. PMID:25246875

  18. 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.

  19. Magnetic cumulation

    NASA Astrophysics Data System (ADS)

    Pavlovskij, A. I.

    1990-08-01

    The second half of 40-th -finish of 60-th of the XX-th Century were prolific y ears of scientific activity of A.D. Sakharov (1921-1990), when his unique creati ve aptitudes and inventivity has found a wide manifestation. Besides of his decis ive contribution to creation of Soviet thermonuclear weapons, in the area of his interests entered various problems of tehrmonuclaer energetics. In 1950 I.E. Tam m and A.D. Sakharov formulated the principles of magnetic thermoisolation of High temperature Plasmas, which put a beginning to controlled thermonuclear synthesis in the U.S.S.R. In 1951 A.D. Sakharov developed the theory of magnetic stationa ry thermonuclear reactor, which are closed to modern Tokamaks. Approximately in 1960-1961 He examined the possibility of thermonuclear synthesis on the basis of L aser compression of a spherical target. The idea of magnetic cumulation was forwrded by A.D. Sakharov as one of the ways of the obtaining of a controlled impulse thermonuclear reaction.

  20. Structure, magnetic and dielectric properties of BaTiO3-Co multi-layer nano-composite films

    NASA Astrophysics Data System (ADS)

    Zhang, Yiwen; Kobayashi, Nobukiyo; Ohnuma, Shigehiro; Nose, Masateru; Masumoto, Hiroshi

    2016-03-01

    The BTO-Co multi-layer nano-composite films have been deposited successfully, which consist of amorphous BTO layers and Co nano-particles layers. By controlling Co layer thickness from 6.3 to 0.3 nm, the resistivity of BTO-Co films increases from 100 to 106 μΩ m. And the magnetization of films changes from 0.73 to 0.01 T. Noteworthy, when the Co layer thickness is 2.5 nm, the films show superparamagnetic properties. HRTEM observation clearly shows that these films have the nanometer-sized metal Co particles of around 2 nm in diameters and a homogeneous dispersion. With lower Co layer thickness, the BTO-Co films exhibit high electrical resistivity. The dielectric constant tested at 1 kHz of these BTO-Co films increases from about 10-40, by controlling the Co layer thickness.

  1. 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.

  2. Influence of inserted Mo layer on the thermal stability of perpendicularly magnetized Ta/Mo/Co20Fe60B20/MgO/Ta films

    NASA Astrophysics Data System (ADS)

    Li, Minghua; Lu, Jinhui; Yu, Guoqiang; Li, Xiang; Han, Gang; Chen, Xi; Shi, Hui; Yu, Guanghua; Amiri, Pedram Khalili; Wang, Kang L.

    2016-04-01

    We studied the thermal stability of perpendicular magnetic anisotropy (PMA) in Ta/Mo/CoFeB/MgO/Ta films with and without inserted Mo layers. In the absence of a Mo layer, the films show PMA at annealing temperatures below 300 °C. On the other hand, the insertion of a Mo layer preserves PMA at annealing temperatures of up to 500 °C; however, a higher annealing temperature leads to the collapse of PMA. X-ray photoelectron spectroscopy (XPS) and high-resolution transmission electron microscopy (HRTEM) were used to study the microstructure of the films to understand the deterioration of PMA. The XPS results show that the segregation of Ta is partly suppressed by inserting a Mo layer. Once inserted, Mo does not remain at the interface of Ta and CoFeB but migrates to the surface of the films. The HRTEM results show that the crystallization of the MgO (001) texture is improved owing to the higher annealing temperature of the Mo inserted sample. A smooth and clear CoFeB/MgO interface is evident. The inserted Mo layer not only helps to obtain sharper and smoother interfaces but also contributes to the crystallization after the higher annealing temperature of films.

  3. Magnetic properties of hydrogen-included TiZrNiPd quasicrystals.

    PubMed

    Shin, Hongsik; Lee, Sang-Hwa; Jo, Youngsoo; Kim, Jae-Yong

    2012-07-01

    Quasicrystals prepared by rapid quenching of Pd-added TiZrNi ingots were hydrogenated, and effects of hydrogen for magnetic properties were compared with the unhydrogenated ones under magnetic fields from -10000 to 10000 Oe. The magnetization values obtained from vibrating sample magnetometer (VSM) were analyzed with the combination of powder X-ray diffraction (XRD) data. While its contribution is larger than that of Pd, hydrogen decreases the magnetic moments of both Pd-doped and undoped quasicrystals. As increasing the amount of absorbed hydrogen which is represented by H/M (hydrogen to host metal atom ratio) values from 0 to 1.19, the magnetization values of Ti53Zr27Ni20 quasicrystals measured at 10000 Oe significantly decreased from 0.301 to 0.212 emu/g. A careful analysis of XRD data demonstrated that the reduced interactions of magnetic dipole moments between Ni atoms, as the product of the expansion of the quasilattice constants after hydrogenation, are responsible for the decreased magnetization values in hydrogenated TiZrNiPd quasicrystal samples. PMID:22966713

  4. Doxorubicin-loaded magnetic gold nanoshells for a combination therapy of hyperthermia and drug delivery.

    PubMed

    Mohammad, Faruq; Yusof, Nor Azah

    2014-11-15

    In the present work, nanohybrid of an anticancer drug, doxorubicin (Dox) loaded gold-coated superparamagnetic iron oxide nanoparticles (SPIONs@Au) were prepared for a combination therapy of cancer by means of both hyperthermia and drug delivery. The Dox molecules were conjugated to SPIONs@Au nanoparticles with the help of cysteamine (Cyst) as a non-covalent space linker and the Dox loading efficiency was investigated to be as high as 0.32 mg/mg. Thus synthesized particles were characterized by HRTEM, UV-Vis, FT-IR, SQUID magnetic studies and further tested for heat and drug release at low frequency oscillatory magnetic fields. The hyperthermia studies investigated to be strongly influenced by the applied frequency and the solvents used. The Dox delivery studies indicated that the drug release efficacy is strongly improved by maintaining the acidic pH conditions and the oscillatory magnetic fields, i.e. an enhancement in the Dox release was observed from the oscillation of particles due to the applied frequency, and is not effected by heating of the solution. Finally, the in vitro cell viability and proliferation studies were conducted using two different immortalized cell lines containing a cancerous (MCF-7 breast cancer) and non-cancerous H9c2 cardiac cell type. PMID:25170601

  5. Optical measurement of anisotropic magnetic susceptibility for diamagnetic fine particles

    NASA Astrophysics Data System (ADS)

    Kitamura, Naoyuki; Takahashi, Kohki; Mogi, Iwao; Awaji, Satoshi; Watanabe, Kazuo

    2016-01-01

    We have developed an apparatus that allows the observation of the transient rotational motion of fine particles under a high magnetic field in order to determine anisotropic magnetic susceptibility. The anisotropic susceptibilities of spherical nanoparticles of bismuth and commercially available carbon nanofibers were determined. The estimated Δχ = 3.9 × 10-5 of spherical bismuth nanoparticles with a diameter of 370 nm was fairly consistent with the value determined previously by the magnetic field dependence of diffraction peak intensity in the X-ray diffraction (XRD) pattern, but was slightly smaller than the value for the bulk crystal. In contrast, the transient behavior of carbon nanofibers did not obey the theoretical motion of a single crystal. The wide distribution of fiber lengths, the irregularity of the structure in the fiber, and the connections between the fibers are suggested for the anomalous behavior.

  6. Investigations on magnetic particles prepared by cyclic growth

    NASA Astrophysics Data System (ADS)

    Müller, Robert; Dutz, Silvio; Habisreuther, Tobias; Zeisberger, Matthias

    2011-05-01

    Magnetic iron oxide nanoparticles are promising tools for medical applications like hyperthermia or magnetic drug targeting. The relevant properties in these applications strongly depend on particle size and size distribution. In order to investigate the influence of mean size as well as size distribution, iron oxide powders from particles by a cyclic method based on "conventional" precipitation from Fe-salt solution were prepared. Increasing mean particle size with increasing number of cycles is confirmed by XRD. Magnetic parameters of the saturation hysteresis loop, hysteresis losses calculated from minor loops and switching field distributions are shown. A fractionation experiment on a fluid sample of particles prepared by 3 cycles was carried out in order to improve the hysteresis losses.

  7. Magnetic birefringence of iron oxyhydroxide nanoparticles stabilised by sucrose

    NASA Astrophysics Data System (ADS)

    Koralewski, M.; Pochylski, M.; Gierszewski, J.

    2011-05-01

    Magnetically induced optical birefringence is used to investigate pharmaceutically important iron-sucrose aqueous suspensions. XRD and TEM measurements of the system of oxyhydroxide particles stabilised by sucrose have shown that this system contains iron oxyhydroxide in the form of 2-5 nm particles. The mineral form of the iron-core is suggested to be akaganeite. Anisotropy of the optical polarizability and magnetic susceptibility of akaganeite nanoparticles are calculated. The permanent dipole moment obtained for the nanoparticles studied was found to be negligible, in agreement with the characteristic superparamagnetic behaviour of the magnetic nanoparticles observed at room temperature. The Neel temperature of these nanoparticles is estimated as below 276 K. The results obtained are discussed against a background of the earlier studies of similar nanoscale systems.

  8. Diameter Dependence of Magnetic Properties in Nanoparticle-Filled CNTs

    NASA Astrophysics Data System (ADS)

    Stojak, Kristen; Chandra, Sayan; Khurshid, Hafsa; Phan, Manh-Huong; Srikanth, Hariharan; Palmero, Ester; Vázquez, Manuel

    2014-03-01

    In past studies we showed magnetic polymer nanocomposites (MPNCs) with ferrite nanoparticle (NP) fillers to be magnetically tunable when passing microwave signals through films under the influence of an external magnetic field. We extend this study to include NP-filled multi-walled carbon nanotubes (CNTs) of various diameter (~300nm, ~100nm, ~40nm) synthesized by a catalyst-free CVD method, where the outer diameter of the CNTs is determined by a porous alumina template. These high-aspect ratio magnetic nanostructures, with tunable anisotropy and tunable saturation magnetization, are of particular interest in enhancing magnetic and microwave response in existing MPNCs. CNTs with ~ 300nm diameter have been uniformly filled with cobalt ferrite and nickel ferrite NPs (~7nm). NP-filled CNTs show an increase in blocking temperature of ~40K, as well as an increase in relaxation time, τ0. The enhancement of these properties indicates that enclosing NPs in CNTs increases interparticle interactions. The magnetic properties are also tunable by varying the diameter of CNTs. Characterization was completed with XRD, TEM and Quantum Design PPMS, with VSM and ACMS options.

  9. Preparation and characterization of biocompatible magnetic carbon nanotubes

    NASA Astrophysics Data System (ADS)

    Shan, Yan; Chen, Kezheng; Yu, Xuegang; Gao, Lian

    2010-11-01

    Magnetic carbon nanotubes consisting of multi-wall carbon nanotubes (MWNTs) core and Fe3O4 shell were successfully prepared by in situ thermal decomposition of Fe(acac)3 or FeCl3 or Fe(CO)5 in 2-pyrrolidone containing acid treated MWNTs at 240 °C with the protection of nitrogen gas. The samples were characterized by TEM, XRD, SEAD, XPS and superconducting quantum interference device. Also, their biocompatibility was compared with naked carbon nanotubes. The results showed that after coated with Fe3O4 nanoparticles, the obtained magnetic carbon nanotubes show superparamagnetic characteristic at room temperature, and their blocking temperature is about 80 K. The magnetic properties of the nanotubes are relevant to the content of magnetic particles, increasing content of magnetic nanoparticles leads to higher blocking temperature and saturation magnetization. The results of antimicrobial activities to bacterial cells (Escherichia coli) showed that the MWNTs have antimicrobial activity, while the magnetic nanotubes are biocompatible even with a higher concentration than that of MWNTs.

  10. Studies on the self-catalyzed Knoevenagel condensation, characterization, DPPH radical scavenging activity, cytotoxicity, and molecular properties of 5-arylidene-2,2-dimethyl-1,3-dioxane-4,6-diones using single crystal XRD and DFT techniques

    NASA Astrophysics Data System (ADS)

    Suresh Kumar, G. S.; Antony Muthu Prabhu, A.; Bhuvanesh, N.

    2014-10-01

    We have studied the self-catalyzed Knoevenagel condensation, spectral characterization, DPPH radical scavenging activity, cytotoxicity, and molecular properties of 5-arylidene-2,2-dimethyl-1,3-dioxane-4,6-diones using single crystal XRD and DFT techniques. In the absence of any catalyst, a series of novel 5-arylidene-2,2-dimethyl-1,3-dioxane-4,6-diones were synthesized using Meldrum’s acid and formylphenoxyaliphatic acid(s) in water. These molecules are arranged in the dimer form through intermolecular H-bonding in the single crystal XRD structure. Compounds have better DPPH radical scavenging activity and cytotoxicity against A431 cancer cell line. The optimized molecular structure, natural bond orbital analysis, electrostatic potential map, HOMO-LUMO energies, molecular properties, and atomic charges of these molecules have been studied by performing DFT/B3LYP/3-21G(*) level of theory in gas phase.

  11. XRD study of yttria stabilized zirconia irradiated with 7.3 MeV Fe, 10 MeV I, 16 MeV Au, 200 MeV Xe and 2.2 GeV Au ions

    NASA Astrophysics Data System (ADS)

    Nakano, K.; Yoshizaki, H.; Saitoh, Y.; Ishikawa, N.; Iwase, A.

    2016-03-01

    To simulate energetic neutron irradiation effects, yttria-stabilized zirconia (YSZ) which is one of the major materials for electrical corrosion potential sensors (ECP sensors) was irradiated with heavy ions at energies ranging from 7.3 MeV to 2.2 GeV. Ion irradiation effects on the lattice structure were analyzed using the X-ray diffraction (XRD). The increase in lattice constant was induced by the ion irradiation. It was dominated by the elastic collision process and not by the electronic excitation process. The lattice disordering which was observed as a broadening of XRD peaks was also induced by the irradiation especially for 200 MeV Xe ion irradiation. The present result suggests that the expansion and/or the disordering of YSZ lattice induced by energetic neutrons may affect the durability of a joint interface between a metal housing and YSZ membrane for the usage of ECP sensors in nuclear power reactors.

  12. SmCo5/Fe nanocomposite magnetic powders processed by magnetic field-assisted ball milling with and without surfactant

    NASA Astrophysics Data System (ADS)

    Saravanan, P.; Gopalan, R.; Rama Rao, N. V.; Manivel Raja, M.; Chandrasekaran, V.

    2007-09-01

    A magnetic field-assisted ball milling has been employed for the preparation of SmCo5 + 10 wt% Fe nanocomposite powders in the presence of oleic acid as surfactant. Milling experiments were also carried out without using surfactant and the nanocomposite powders so obtained, with and without surfactant, were investigated for their structural and magnetic properties using SEM, XRD, VSM and Mössbauer spectrometry. The field-milled SmCo5/Fe nanopowders in the presence of surfactant display a possible grain orientation and possess relatively high coercivity as compared with that of SmCo5/Fe powders obtained with field-milling or conventional milling. Mössbauer studies revealed that the formation of α-Fe(Co) (soft magnetic phase) is more pronounced for the powders milled without surfactant.

  13. 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.

  14. 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.

  15. 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.

  16. 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.

  17. 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.

  18. 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

  19. 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. PMID:25734962

  20. 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.

  1. 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.

  2. Development of Magnetic Refrigerator

    NASA Astrophysics Data System (ADS)

    Ogiwara, Hiroyasu; Nakagome, Hideki; Kuriyama, Tohru

    A series of R & D of magnetic refrigerators has been done in order to realize an advanced type cryocooler for superconducting magnets of maglev trains and MRI medical system. As a result of efforts on both the magnetic refrigerator and superconducting magnets, a parasitic type magnetic refrigeration system was proposed.

  3. Polyvinyl Pyrrolidone-Assisted Solvothermal Synthesis of Fe3O4 Vesicular Nanospheres.

    PubMed

    Song, Hongfei; Liu, Meiying; Li, Sainan; Chen, Linlin; Lin, Chunming; Zhang, Liqing

    2015-05-01

    Monodispersed Fe3O4 vesicular nanospheres with a diameter of 160 nm have been fabricated solvothermally in the mixed solution of ethylene glycol (EG) and ethylenediamine (en) with the surfactant polyvinyl pyrrolidone (PVP). The microstructure and magnetic properties of the products were characterized by XRD, Raman, SEM, TEM, HRTEM, N2 adsorption-desorption and SQUID techniques. The HRTEM result shows that spherical Fe3O4 nanoparticles are structurally uniform with a distinct lattice spacing of 2.6 Å, which can be assigned to the (311) crystal facet of cubic Fe3O4. Besides, the as-obtained Fe3O4 vesicular nanospheres are ferromagnetic with a saturation magnetization of 86.9 emu/g as high as its bulk counterpart, demonstrating its promising applications in advanced magnetic materials and biomedicine. PMID:26505038

  4. Effect of Pt layer thickness on perpendicular magnetic anisotropy in ultrathin Co/Pt multilayers

    NASA Astrophysics Data System (ADS)

    Kulkarni, P. D.; Krishnan, M.; Barshilia, H. C.; Chowdhury, P.

    2013-02-01

    Co/Pt multilayer structures with varying Pt layer thicknesses from 1.5 to 12 Å were deposited on Ta buffer layer by DC magnetron sputtering technique and both of their magnetic and structural properties were investigated. All the multilayers showed perpendicular magnetic anisotropy (PMA) and the enhancement in PMA is observed with increase in the Pt layer thickness. The structural investigation using XRD reveals the presence of single peak in all these multilayers, which indicate the formation of coherent Co/Pt (111) structure. The origin of PMA in these multilayer structure is due to the strain induced in the Co layer. From the full-width-half-maximum (FWHM) of the XRD patterns it is observed that the grain size is increasing with increasing the Pt layer thickness. The influence of the enhancement of the grain size is then correlated with the measured M-H hysteresis behavior and subsequently the anisotropy energy.

  5. Magnetic guns with cylindrical permanent magnets

    NASA Astrophysics Data System (ADS)

    Vokoun, David; Beleggia, Marco; Heller, Lud?k

    2012-05-01

    The motion of a cylindrical permanent magnet (projectile) inside a tubular permanent magnet, with both magnets magnetized axially, illustrates nicely the physical principles behind the operation of magnetic guns. The force acting upon the projectile is expressed semi-analytically as derivative of the magnetostatic interaction energy. For comparison, the forces involved are also calculated numerically using finite elements methods. Based on the conservation of the magnetostatic and kinetic energies, the exit and asymptotic velocities are determined. The derived formulas can be used to optimize the generated forces and motion of the inner cylindrical magnet.

  6. Magnet system for a superconducting magnetic separator

    NASA Astrophysics Data System (ADS)

    Jüngst, K. P.; Ries, G.; Förster, S.; Graf, F.; Obermaier, G.; Lehmann, W.

    A magnetic separator with superconducting magnets has been designed, constructed and successfully tested. Its application is sorting finely ground ores or minerals with low susceptibility. The system can be described as a superconducting drum separator combining the advantages of the well known reliable conventional drum separators with the advantage of high magnetic field economically produced by superconducting magnets. This laboratory magnetic separator with a relevant drum diameter of 1 m served as a first step on the way to an industrial pilot plant. This paper reports on design, construction, and test of the sc magnet system and its supply.

  7. Magnetic nanowires as permanent magnet materials

    NASA Astrophysics Data System (ADS)

    Maurer, T.; Ott, F.; Chaboussant, G.; Soumare, Y.; Piquemal, J.-Y.; Viau, G.

    2007-10-01

    We present the fabrication of metallic magnetic nanowires using a low temperature chemical process. We show that pressed powders and magnetically oriented samples exhibit a very high coercivity (6.5kOe at 140K and 4.8kOe at 300K). We discuss the magnetic properties of these metamaterials and show that they have the suitable properties to realize "high temperature magnets" competitive with AlNiCo or SmCo permanent magnets. They could also be used as recording media for high density magnetic recording.

  8. Magnetic cluster developement in In1- x Mn x Sb semiconductor alloys

    NASA Astrophysics Data System (ADS)

    Rednic, Lidia; Deac, Iosif G.; Dorolti, Eugen; Coldea, Marin; Rednic, Vasile; Neumann, Manfred

    2010-08-01

    X-ray Diffraction (XRD), X-ray Photoelectron Spectroscopy (XPS), Transmission Electron Microscopy (TEM) and magnetic measurements as a function of applied magnetic field and temperature for In1- x Mn x Sb (0.05≤ x≤0.2) system are reported. Magnetic measurements performed at high and small magnetic field in ZFC and FC indicate the coexistence of ferromagnetic In1- x Mn x Sb solid solution and two types of magnetic cluster: ferromagnetic MnSb and ferrimagnetic Mn2Sb. XPS valence band and Mn 2p core level spectra have confirmed the presence of MnSb and Mn2Sb phases. TEM images show some manganese antimonide phase microinclusions with dimension between (30-40) nm.

  9. Magnetic cluster developement in In1-x MnxSb semiconductor alloys

    NASA Astrophysics Data System (ADS)

    Rednic, Lidia; Deac, Iosif; Dorolti, Eugen; Coldea, Marin; Rednic, Vasile; Neumann, Manfred

    2010-08-01

    X-ray Diffraction (XRD), X-ray Photoelectron Spectroscopy (XPS), Transmission Electron Microscopy (TEM) and magnetic measurements as a function of applied magnetic field and temperature for In1-x MnxSb (0.05≤x≤0.2) system are reported. Magnetic measurements performed at high and small magnetic field in ZFC and FC indicate the coexistence of ferromagnetic In1-x MnxSb solid solution and two types of magnetic cluster: ferromagnetic MnSb and ferrimagnetic Mn2Sb. XPS valence band and Mn 2p core level spectra have confirmed the presence of MnSb and Mn2Sb phases. TEM images show some manganese antimonide phase microinclusions with dimension between (30-40) nm.

  10. Enhanced magnetization by doping aluminum in laser ablated copper ferrite thin films

    NASA Astrophysics Data System (ADS)

    Raghavender, A. T.; Hong, Nguyen Hoa; Kurisu, M.

    2016-03-01

    Highly crystalline oriented CuFe2-xAlxO4 (0.0≤x≤0.8) thin films with thickness as of about 130 nm were grown on MgO (100) substrates using pulsed laser deposition technique. The lattice parameters were not affected by the Al3+ doping into CuFe2O4 thin films. The magnetization of Al-Cu-ferrite films was gradually increased when Al3+ content increases. The enhancement in magnetization with the higher doping of Al3+ content might cause the overall better magnetic domain alignment during the magnetization measurements and thus a stronger magnetization is observed as evidenced from the film crystalline quality by the stronger (222) peak in XRD. Additionally, other factors such as defects, strains etc. might also play some role.

  11. Preparation of novel magnetic chitosan/graphene oxide composite as effective adsorbents toward methylene blue.

    PubMed

    Fan, Lulu; Luo, Chuannan; Sun, Min; Li, Xiangjun; Lu, Fuguang; Qiu, Huamin

    2012-06-01

    A novel magnetic composite bioadsorbent composed of magnetic chitosan and graphene oxide (MCGO) was prepared as the magnetic adsorbent toward methylene blue. The magnetic composite bioadsorbent was characterized by SEM, FTIR and XRD measurements. The effect factors including pH, contact time and temperature on the adsorption properties of methylene blue onto MCGO were investigated. The resulting shows extraordinary adsorption capacity and fast adsorption rates for removal of methylene blue. The kinetics are well-described by pseudo-second-order kinetic. The experimental data of isotherm followed the Langmuir isotherm model and the Freundlich model, respectively. This work shows that the MCGO could be utilized as an efficient, magnetically separable adsorbent for the environmental cleanup. PMID:22464421

  12. 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.

  13. 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.

  14. 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.

  15. Magnetic storms

    NASA Astrophysics Data System (ADS)

    Tsurutani, Bruce T.; Gonzalez, Walter D.; Kamide, Yohsuke

    This talk provides a brief summary of the first conference devoted entirely to magnetic storms. The conference was held in Pasadena, California, at the Jet Propulsion Laboratory, 12-16 February 1996. Topics covered the relevant time-varying phenomena at the sun/corona, propagation of these structures through interplanetary space, the response of the magnetosphere from its interaction with these interplanetary structures, the formation of the storm- time ring-current (in particular the oxygen content of the ring-current), and storm ionospheric effects and ground based effects. A complementary summary is provided by Gonzalez et al. in EOS, 1996. The full set of review articles will be published in an AGU monograph and many of the contributed articles will appear in a special section of the Journal of Geophysical Research, Space Physics.

  16. 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.

  17. Magnetization dynamics using ultrashort magnetic field pulses

    NASA Astrophysics Data System (ADS)

    Tudosa, Ioan

    Very short and well shaped magnetic field pulses can be generated using ultra-relativistic electron bunches at Stanford Linear Accelerator. These fields of several Tesla with duration of several picoseconds are used to study the response of magnetic materials to a very short excitation. Precession of a magnetic moment by 90 degrees in a field of 1 Tesla takes about 10 picoseconds, so we explore the range of fast switching of the magnetization by precession. Our experiments are in a region of magnetic excitation that is not yet accessible by other methods. The current table top experiments can generate fields longer than 100 ps and with strength of 0.1 Tesla only. Two types of magnetic were used, magnetic recording media and model magnetic thin films. Information about the magnetization dynamics is extracted from the magnetic patterns generated by the magnetic field. The shape and size of these patterns are influenced by the dissipation of angular momentum involved in the switching process. The high-density recording media, both in-plane and perpendicular type, shows a pattern which indicates a high spin momentum dissipation. The perpendicular magnetic recording media was exposed to multiple magnetic field pulses. We observed an extended transition region between switched and non-switched areas indicating a stochastic switching behavior that cannot be explained by thermal fluctuations. The model films consist of very thin crystalline Fe films on GaAs. Even with these model films we see an enhanced dissipation compared to ferromagnetic resonance studies. The magnetic patterns show that damping increases with time and it is not a constant as usually assumed in the equation describing the magnetization dynamics. The simulation using the theory of spin-wave scattering explains only half of the observed damping. An important feature of this theory is that the spin dissipation is time dependent and depends on the large angle between the magnetization and the magnetic field.

  18. 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.

  19. Magnetic Resonance Imaging (MRI)

    MedlinePlus

    ... How Can I Help a Friend Who Cuts? Magnetic Resonance Imaging (MRI) KidsHealth > For Teens > Magnetic Resonance Imaging (MRI) Print ... MRI Exam Safety Getting Your Results What Is MRI? Magnetic resonance imaging (MRI) is a type of ...

  20. 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.

  1. 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.

  2. Laced permanent magnet quadrupole drift tube magnets

    SciTech Connect

    Feinberg, B.; Behrsing, G.U.; Halbach, K.; Marks, J.S.; Morrison, M.E.; Nelson, D.H.

    1989-03-01

    Twenty-three laced permanent magnet quadrupole drift tube magnets have been constructed, tested, and installed in the SuperHILAC heavy ion linear accelerator at LBL, marking the first accelerator use of this new type of quadrupole. The magnets consist of conventional tape-wound quadrupole electromagnets, using iron pole-pieces, with permanent magnet material (samarium cobalt) inserted between the poles to reduce the effects of saturation. The iron is preloaded with magnetic flux generated by the permanent magnet material, resulting in an asymmetrical saturation curve. Since the polarity of the individual quadrupole magnets in a drift tube linac is never reversed, we can take advantage of this asymmetrical saturation to provide about 20% greater focusing strength than is available with conventional quadrupoles, while replacing the vanadium permendur poletips with iron poletips. Comparisons between these magnets and conventional tape-wound quadrupoles will be presented. 3 refs., 5 figs.

  3. Scanning nonlinear magnetic microscopy.

    PubMed

    Endo, Makoto; Ohara, Koya; Cho, Yasuo

    2007-07-01

    Scanning nonlinear magnetic microscopy (SNMM) is introduced as a new microscopic technique for measurement of the distribution of magnetization. The technique is based on the detection of inductance variation in a magnetic material under application of an external alternating magnetic field. The measured inductance thus reflects the nonlinear magnetic response of the material, giving the nonlinear magnetic permeability (mu(333)) and the direction and magnitude of magnetization. SNMM is demonstrated in application to measurement of the magnetization distribution of a floppy disk. PMID:17672763

  4. 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.

  5. 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.

  6. Structural and magnetic characterization of electrodeposited Ni-Cu/Cu and Fe-Ni-Cu/Cu multilayer

    NASA Astrophysics Data System (ADS)

    Hedayati, Kambiz

    2015-03-01

    In this research, Ni-Cu/Cu and Fe-Ni-Cu/Cu multilayers were electrodeposited on Au/Cr/glass substrate. The XRD pattern of Ni-Cu/Cu multilayer indicates satellite peaks of Ni-Cu and Cu bilayers. The EDX results had shown that the Ni content increased with increasing magnetic layers in both Ni-Cu/Cu and Fe-Ni-Cu/Cu multilayers. The AFM images had shown that increasing the magnetic and nonmagnetic layers leads to increasing surface roughness. The VSM of samples obtained the coercivity by increasing magnetic layer thickness and by decreasing the addition of Fe to Ni-Cu/Cu multilayers.

  7. 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.

  8. 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.

  9. 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.

  10. 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)

  11. 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 achieved after annealing at temperature of 700 °C. The contribution of the changes in the crystalline structure, induced by the heat treatment, to the magnetic hardening of the FeCoCu nanowires is discussed.

  12. Structural and magnetic characterization of as-prepared and annealed FeCoCu nanowire arrays in ordered anodic aluminum oxide templates

    NASA Astrophysics Data System (ADS)

    Rodríguez-González, B.; Bran, C.; Warnatz, T.; Rivas, J.; Vazquez, M.

    2014-04-01

    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 Fe0.28Co0.67Cu0.05 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 achieved after annealing at temperature of 700 °C. The contribution of the changes in the crystalline structure, induced by the heat treatment, to the magnetic hardening of the FeCoCu nanowires is discussed.

  13. Direct binding and characterization of lipase onto magnetic nanoparticles.

    PubMed

    Huang, Shih-Hung; Liao, Min-Hung; Chen, Dong-Hwang

    2003-01-01

    Lipase was covalently bound onto Fe(3)O(4) magnetic nanoparticles (12.7 nm) via carbodiimide activation. The Fe(3)O(4) magnetic nanoparticles were prepared by coprecipitating Fe(2+) and Fe(3+) ions in an ammonia solution and treating under hydrothermal conditions. The analyses of transmission electron microscopy (TEM) and X-ray diffraction (XRD) showed that the size and structure of magnetic nanoparticles had no significant changes after enzyme binding. Magnetic measurement revealed the resultant lipase-bound magnetic nanoparticles were superparamagnetic with a saturation magnetization of 61 emu/g (only slightly lower than that of the naked ones (64 emu/g)), a remanent magnetization of 1.0 emu/g, and a coercivity of 7.5 Oe. The analysis of Fourier transform infrared (FTIR) spectroscopy confirmed the binding of lipase onto magnetic nanoparticles. The binding efficiency of lipase was 100% when the weight ratio of lipase bound to Fe(3)O(4) nanoparticles was below 0.033. Compared to the free enzyme, the bound lipase exhibited a 1.41-fold enhanced activity, a 31-fold improved stability, and better tolerance to the variation of solution pH. For the hydrolysis of pNPP by bound lipase at pH 8, the activation energy within 20-35 degrees C was 6.4 kJ/mol, and the maximum specific activity and Michaelis constant at 25 degrees C were 1.07 micromol/min mg and 0.4 mM, respectively. It revealed that the available active sites of lipase and their affinity to substrate increased after being bound onto magnetic nanoparticles. PMID:12790688

  14. 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 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. Electronic supplementary information (ESI) available. See DOI: 10.1039/c5nr06509g

  15. Exchange coupled L10-FePt/fcc-FePt nanomagnets: Synthesis, characterization and magnetic properties

    NASA Astrophysics Data System (ADS)

    Srivastava, Sachchidanand; Gajbhiye, Namdeo S.

    2016-03-01

    We report synthesis, characterization and magnetic properties of exchange-coupled L10-FePt/fcc-FePt nanomagnets. Structural and morphological characterization of exchange-coupled L10-FePt/fcc-FePt was carried out by powder X-ray diffraction, Mössbauer spectroscopy and transmission electron microscopy. Rietveld refinement of powder X-ray diffraction pattern has been used to quantify L10-FePt and fcc-FePt phases present in samples. Room temperature Mössbauer spectroscopy showed sextets of both L10-FePt and fcc-FePt phases with their respective hyperfine interaction parameters. Transmission electron microscopic (TEM and HRTEM) images confirmed nanocrystalline nature of exchange-coupled nanomagnets with particle size ranges from 15 nm to 50 nm after annealing for different time at 700 °C. Room temperature magnetic studies showed ferromagnetic nature of nanomagnets and maximum energy product (BH)max~10.92 MGOe was obtained for sample containing 89.0% volume fraction of L10-FePt phase.

  16. Mixed-valence magnetism in TiO2/TiOx superlattices

    NASA Astrophysics Data System (ADS)

    Hsieh, W. C.; Wadekar, P. V.; Huang, H. C.; Chang, C. F.; Wong, M. S.; Seo, H. W.; Chuang, F. C.; Chen, Q. Y.

    2015-03-01

    Epitaxial TiO2 and TiOx superlattices, ~ 1-nm thick per layer by sputtering at 570°C using pure argon on sapphire substrates. From HR-TEM, the periodically alternating layers are well-defined. XPS analyses based on the binding energy of Ti 2p3/2 peaks suggest the co-existence of Ti+3 and Ti+4, thus verifying the mixed-valence nature. The M(H) curves measured at room temperature using SQUID showed hysteretic loops typical of ferromagnetism. Electrical transport measurements were done at zero field demonstrate transition of charge ordering at low temperatures, reminiscent of what was found in Ti-rich Ti1+xO2 single-layer thin films, made by Ti ion implantation into TiO2 crystals, in which randomly distributed TiO2, Ti2O3 and TiO were found to coexist. Preliminary First-principle (ab initio) calculations to understand the roles of oxygen vacancies in various TiO2 super-cells could indeed lead to spontaneous magnetizations. We thus argue that mixed-valence titanium ions are responsible for the magnetism

  17. 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. PMID:26666195

  18. Magnetic properties of nanoscale crystalline maghemite obtained by a new synthetic route

    NASA Astrophysics Data System (ADS)

    Mercante, L. A.; Melo, W. W. M.; Granada, M.; Troiani, H. E.; Macedo, W. A. A.; Ardison, J. D.; Vaz, M. G. F.; Novak, M. A.

    2012-09-01

    In this work we describe the synthesis and characterization of maghemite nanoparticles obtained by a new synthetic route. The material was synthesized using triethylamine as a coprecipitation agent in the presence of the organic ligand N,N‧-bis(3,5-di-tert-butyl-catechol)-2,4-diaminotoluene (LCH3). Mössbauer spectrum at 4 K shows typical hyperfine parameters of maghemite and Transmission Electron Microscopy images reveal that the nanoparticles have a mean diameter of 3.9 nm and a narrow size distribution. AC magnetic susceptibility in zero field presents an Arrhenius behavior with unreasonable relaxation parameters due to the strong influence of dipolar interaction. In contrast when the measurements are performed in a 1 kOe field, the effect of dipolar interactions becomes negligible and the obtained parameters are in good agreement with the static magnetic properties. The dynamic energy barrier obtained from the AC susceptibility results is larger than the expected from the average size observed by HRTEM results, evidencing the strong influence of the surface contribution to the anisotropy.

  19. Folate-conjugated luminescent Fe3O4 nanoparticles for magnetic hyperthermia

    NASA Astrophysics Data System (ADS)

    Barick, K. C.; Rana, Suman; Hassan, P. A.

    2014-04-01

    We demonstrate a facile approach for the synthesis of folate-conjugated luminescent iron oxide nanoparticles (FLIONs). XRD and TEM analyses reveal the formation of highly crystalline single-phase Fe3O4 nanoparticles of size about 10 nm. The conjugation of folate receptor (folic acid, FA) and luminescent molecule (fluorescein isothiocyanate, FITC) onto the surface of nanoparticles was evident from FTIR and UV-visible spectroscopy. These FLIONs show good colloidal stability, high magnetic field responsivity and excellent self-heating efficacy. Specifically, a new class of magnetic nanoparticles has been fabricated, which can be used as an effective heating source for hyperthermia.

  20. Magnetic and optical properties of monosized Eu-doped ZnO nanocrystals from nanoemulsion

    NASA Astrophysics Data System (ADS)

    Yoon, Hayoung; Hua Wu, Jun; Hyun Min, Ji; Sung Lee, Ji; Ju, Jae-Seon; Keun Kim, Young

    2012-04-01

    We report the synthesis and characterization of monosized Eu-doped ZnO nanocrystals via a nanoemulsion process as a function of the doping ratio. The structure, optical, and magnetic properties of the nanocrystals are investigated by XRD, TEM, PL spectrometry, and physical property measurement system. The nanocrystals as prepared show high crystallinity and tight particle size distributions with the diameters of ˜ 10 nm. The doped samples clearly exhibit the 5D0→7FJ transition emission due to the presence of the Eu3+ ions. Meanwhile, the magnetic responses demonstrate the temperature dependence and change with dopant concentration.

  1. Effects of boron composition on tunneling magnetoresistance ratio and microstructure of CoFeB/MgO/CoFeB pseudo-spin-valve magnetic tunnel junctions

    SciTech Connect

    Kodzuka, M.; Ohkubo, T.; Hono, K.; Ikeda, S.; Ohno, H.; Gan, H. D.

    2012-02-15

    The effect of B concentration on the tunneling magnetoresistance (TMR) of (Co{sub 25}Fe{sub 75}){sub 100-x}B{sub x}/MgO/(Co{sub 25}Fe{sub 75}){sub 100-x}B{sub x} (x = 22 and 33) pseudo-spin-valve (P-SV) magnetic tunnel junctions (MTJs) was investigated. The TMR ratios for optimally annealed MTJs with x = 22 and 33 were 340% and 170%, respectively, at room temperature. High resolution transmission electron microscopy (HRTEM) observation showed a weaker (001) texture in the MgO barrier in the MTJ with x = 33. The bottom electrode was not fully crystallized even with a considerable amount of B in the (Co{sub 25}Fe{sub 75}){sub 67}B{sub 33}, while good epitaxy was observed between (001) textured MgO and (Co{sub 25}Fe{sub 75}){sub 78}B{sub 22} electrodes.

  2. Highly c-axis oriented ZnO:Ni thin film nanostructure by RF magnetron sputtering: Structural, morphological and magnetic studies

    NASA Astrophysics Data System (ADS)

    Siddheswaran, R.; Savková, Jarmila; Medlín, Rostislav; Očenášek, Jan; Životský, Ondřej; Novák, Petr; Šutta, Pavol

    2014-10-01

    Nickel doped zinc oxide (ZnO:Ni) thin films with different Ni concentrations were deposited on silicon substrates at 400 °C by reactive magnetron sputtering using a mixture of Ar and O2 gases. The X-ray diffraction and azimuthal patterns of the ZnO:Ni were carried out, and the quality of the strong preferred orientation of crystalline columns in the direction [0 0 1] perpendicular to the substrate surface were analysed. The grain size, distribution, and homogeneity of the thin film surfaces were studied by FE-SEM. The EDX and mapping confirmed that the Ni is incorporated into ZnO uniformly. The microstructure of the textured columns was analysed by TEM and HRTEM analyses. The average thickness and length of the columns were found to be about 50 nm and 600 nm, respectively. The rise of ferromagnetism by the influence of Ni content was studied by VSM magnetic studies at room temperature.

  3. Superconducting magnets 1992

    SciTech Connect

    Not Available

    1993-06-01

    This report discusses the following topics on Superconducting Magnets; SSC Magnet Industrialization; Collider Quadrupole Development; A Record-Setting Magnet; D20: The Push Beyond 10T; Nonaccelerator Applications; APC Materials Development; High-T{sub c} at Low Temperature; Cable and Cabling-Machine Development; and Analytical Magnet Design.

  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. Quadrupole magnets measurement

    SciTech Connect

    Wang, Xijie . Center for Advanced Accelerators Physics); Sylvester, C. )

    1991-01-01

    A rotating coil setup is designed for quadrupole magnet measurement at the Accelerator Test Facility (ATF); Hall probe measurement was also performed for one of each type of quadrupole magnet. Both mechanical and magnetic properties of the quadrupole magnets were measured, the results are reported here. 5 refs., 12 figs., 12 tabs.

  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. Tunable magnetic and magnetocaloric properties of La0.6Sr0.4MnO3 nanoparticles

    NASA Astrophysics Data System (ADS)

    Ehsani, M. H.; Kameli, P.; Ghazi, M. E.; Razavi, F. S.; Taheri, M.

    2013-12-01

    Nanoparticles of La0.6Sr0.4MnO3 with different particle sizes are synthesized by the nitrate-complex auto-ignition method. The structural and magnetic properties of the samples are investigated by X-Ray diffraction (XRD), Fourier transform infra-red (FT-IR) spectroscopy, transmission electron microscopy (TEM), and DC magnetization measurements. The XRD study coupled with the Rietveld refinement shows that all samples crystallize in a rhombohedral structure with the space group of R-3 C. The FT-IR spectroscopy and TEM images indicate formation of the perovskite structure with the average sizes of 20, 40, and 100 nm for the samples sintered at 700, 800, and 1100 C, respectively. The DC magnetization measurements confirm tuning of the magnetic properties due to the particle size effects, e.g., reduction in the ferromagnetic moment and increase in the surface spin disorder by decreasing the particle size. The magnetocaloric effect (MCE) study based on isothermal magnetization vs. filed measurements in all samples reveals a relatively large MCE around the Curie temperature of the samples. The peak around the Curie temperature gradually broadens with reduction of the particle size. The data obtained show that although variations in the magnetic entropy and adiabatic temperature decrease by lowering the particle size, variation in the relative cooling power values are the same for all samples. These results make this material a proper candidate in the magnetic refrigerator application above room temperature at moderate fields.

  8. 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.

  9. Structural and magnetic effects of Cd1-xInxCr2Se4

    NASA Astrophysics Data System (ADS)

    Behera, P. Suchismita; Bhobe, P. A.; Nigam, A. K.

    2015-06-01

    Polycrystalline CdCr2Se4 spinels with non-magnetic indium substitution were investigated with an aim to study the influence of non-magnetic substitution at the Cd site on its structural and magnetic properties. We carried out powder XRD and magnetic measurements on three compositions: Cd1-xInxCr2Se4 (x=0, 0.05, 0.1). The XRD patterns were analyzed by carrying out Rietveld analysis and structural parameters were estimated. Phase purity of the compounds using reitveld refinement technique where confirming the indium distribution at tetrahedral site of the cubic close-packed sublattice formed by the selenium ions. The chemical compositions of these compounds were determined by energy dispersive x-ray analysis. Compared to parent compound, CdCr2Se4, the ferromagnetic Curie temperature TC was found to decrease from 130K to 123K and 114K as x varied from 0 to 0.05 and 0.1 respectively, whereas the saturation magnetization increases in Cd0.95In0.05Cr2Se4 and again decreases in Cd0.9In0.1Cr2Se4.

  10. Properties of Gd2O3 nanoparticles studied by hyperfine interactions and magnetization measurements

    NASA Astrophysics Data System (ADS)

    Correa, E. L.; Bosch-Santos, B.; Cavalcante, F. H. M.; Correa, B. S.; Freitas, R. S.; Carbonari, A. W.; Potiens, M. P. A.

    2016-05-01

    The magnetic behavior of Gd2O3 nanoparticles, produced by thermal decomposition method and subsequently annealed at different temperatures, was investigated by magnetization measurements and, at an atomic level, by perturbed γ - γ angular correlation (PAC) spectroscopy measuring hyperfine interactions at 111In(111Cd) probe nuclei. Nanoparticle structure, size and shape were characterized by X-ray diffraction (XRD) and Transmission Electron Microscopy (TEM). Magnetization measurements were carried out to characterize the paramagnetic behavior of the samples. XRD results show that all samples crystallize in the cubic-C form of the bixbyite structure with space group Ia3. TEM images showed that particles annealed at 873 K present particles with highly homogeneous sizes in the range from 5 nm to 10 nm and those annealed at 1273 K show particles with quite different sizes from 5 nm to 100 nm, with a wide size distribution. PAC and magnetization results show that samples annealed at 873 and 1273 K are paramagnetic. Magnetization measurements show no indication of blocking temperatures for all samples down to 2 K and the presence of antiferromagnetic correlations.

  11. Flexible magnetic membranes based on bacterial cellulose and its evaluation as electromagnetic interference shielding material.

    PubMed

    Marins, Jéssica A; Soares, Bluma G; Barud, Hernane S; Ribeiro, Sidney J L

    2013-10-01

    Flexible magnetic membranes with high proportion of magnetite were successfully prepared by previous impregnation of the never dried bacterial cellulose pellicles with ferric chloride followed by reduction with sodium bisulfite and alkaline treatment for magnetite precipitation. Membranes were characterized by Raman spectroscopy, Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), vibrating magnetometer, field emission scanning electron microscopy (FEG-SEM) and impedance spectroscopy. Microwave properties of these membranes were investigated in the X-band (8.2 to 12.4 GHz). FEG-SEM micrographs show an effective coverage of the BC nanofibers by Fe3O4 nanoparticles. Membranes with up to 75% in weight of particles have been prepared after 60 min of reaction. Magnetite nanoparticles in the form of aggregates well adhered to the BC fibers were observed by SEM. The average crystal sizes of the magnetic particles were in the range of 10±1 to 13±1 nm (estimated by XRD). The magnetic particles in the BC pellicles presented superparamagnetic behavior with a saturation magnetization in the range of 60 emu g(-1) and coercive force around 15 Oe. These magnetic pellicles also displayed high electrical permittivity and a potential application as microwave absorber materials. PMID:23910306

  12. Magnetic properties of nanocrystalline Ni-Zn, Zn-Mn, and Ni-Mn ferrites synthesized by reverse micelle technique

    NASA Astrophysics Data System (ADS)

    Gubbala, S.; Nathani, H.; Koizol, K.; Misra, R. D. K.

    2004-05-01

    Nanocrystalline nickel-zinc, zinc-manganese, and nickel-manganese ferrites synthesized by reverse micelle synthesis technique were characterized by high-resolution transmission electron microscopy (HRTEM) and X-ray diffraction, and the magnetic behavior studied by Superconducting Quantum Interference Device. The mixed (Ni-Zn, Zn-Mn, and Ni-Mn) ferrites exhibit blocking temperatures of 11, 20, and 15 K, respectively. The small differences in the blocking temperatures are attributed to the magnetocrystalline anisotropy and L-S coupling. The saturation magnetization of nanocrystalline Ni-Zn, Zn-Mn, and Ni-Mn at 300 K was 4.5, 9, and 7 emu/g, respectively, and at 2 K was 15, 19, and 14 emu/g, respectively. The lower saturation magnetization of the nanocrystalline ferrites compared to their bulk counterparts is attributed to the core-shell morphology of the particles consisting of ferromagnetically aligned core spins and a spin-glass-like surface layer.

  13. Magnetic Flux and Helicity of Magnetic Clouds

    NASA Astrophysics Data System (ADS)

    Démoulin, P.; Janvier, M.; Dasso, S.

    2016-02-01

    Magnetic clouds (MCs) are formed by flux ropes (FRs) launched from the Sun as part of coronal mass ejections (CMEs). They carry away a large amount of magnetic flux and helicity. The main aim of this study is to quantify these amounts from in situ measurements of MCs at 1 AU. The fit of these data by a local FR model provides the axial magnetic field strength, the radius, the magnetic flux, and the helicity per unit length along the FR axis. We show that these quantities are statistically independent of the position along the FR axis. We then derive the generic shape and length of the FR axis from two sets of MCs. These results improve the estimation of magnetic helicity. Next, we evaluate the total magnetic flux and helicity that cross the sphere of radius of 1 AU, centred at the Sun, per year and during a solar cycle. We also include in the study two sets of small FRs that do not have all the typical characteristics of MCs. While small FRs are at least ten times more numerous than MCs, the magnetic flux and helicity are dominated by the contribution from the larger MCs. In one year they carry away the magnetic flux of about 25 large active regions and the magnetic helicity of 200 of them. MCs carry away an amount of unsigned magnetic helicity similar to the amount estimated for the solar dynamo and that measured in emerging active regions.

  14. Magnetic Flux and Helicity of Magnetic Clouds

    NASA Astrophysics Data System (ADS)

    Démoulin, P.; Janvier, M.; Dasso, S.

    2015-12-01

    Magnetic clouds (MCs) are formed by flux ropes (FRs) launched from the Sun as part of coronal mass ejections (CMEs). They carry away a large amount of magnetic flux and helicity. The main aim of this study is to quantify these amounts from in situ measurements of MCs at 1 AU. The fit of these data by a local FR model provides the axial magnetic field strength, the radius, the magnetic flux, and the helicity per unit length along the FR axis. We show that these quantities are statistically independent of the position along the FR axis. We then derive the generic shape and length of the FR axis from two sets of MCs. These results improve the estimation of magnetic helicity. Next, we evaluate the total magnetic flux and helicity that cross the sphere of radius of 1 AU, centred at the Sun, per year and during a solar cycle. We also include in the study two sets of small FRs that do not have all the typical characteristics of MCs. While small FRs are at least ten times more numerous than MCs, the magnetic flux and helicity are dominated by the contribution from the larger MCs. In one year they carry away the magnetic flux of about 25 large active regions and the magnetic helicity of 200 of them. MCs carry away an amount of unsigned magnetic helicity similar to the amount estimated for the solar dynamo and that measured in emerging active regions.

  15. Magnetic Damping For Maglev

    DOE PAGESBeta

    Zhu, S.; Cai, Y.; Rote, D. M.; Chen, S. S.

    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.

  16. High efficiency magnetic bearings

    NASA Technical Reports Server (NTRS)

    Studer, Philip A.; Jayaraman, Chaitanya P.; Anand, Davinder K.; Kirk, James A.

    1993-01-01

    Research activities concerning high efficiency permanent magnet plus electromagnet (PM/EM) pancake magnetic bearings at the University of Maryland are reported. A description of the construction and working of the magnetic bearing is provided. Next, parameters needed to describe the bearing are explained. Then, methods developed for the design and testing of magnetic bearings are summarized. Finally, a new magnetic bearing which allows active torque control in the off axes directions is discussed.

  17. 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.

  18. Ionic, XRD, dielectric and cyclic voltammetry studies on PVdF-co-HFP / MMT clay intercalated LiN(C2F5SO2)2 based composite electrolyte for Li-ion batteries

    NASA Astrophysics Data System (ADS)

    Vickraman, P.; Purushothaman, K.; SankaraSubramanian, N.

    2014-04-01

    The composition dependence of plasticizer, (EC/DMC)(70-x(wt%)) and LiBETIx(wt%) salt for fixed contents on PVdF-co-HFP(25wt%)/surface modified(SM)-octadecylamine MMT(ODA-MMT) nanoclay(5wt%) host matrix by varying its compositions x=1.5, 3.0, 4.5, 6.0 wt% prepared via solution casting technique has been investigated by A.C. Impedance, Dielectric, XRD, and cyclic voltammetry(CV) studies. The enhanced conductivity 2.1×10-5 S/cm at 300C is observed for (EC/DMC)(70-6)wt%/LiBETI(x=6)wt%. The XRD at 2θ=20.9° confirms β-phase formation, and CV studies on membranes show cyclability and reversibility. The dielectric studies show increase in dielectric constant and dielectric loss with decrease in frequency is attributed to high contribution of charge accumulation at the electrode-electrolyte interface.

  19. Cobalt ferrite nano-composite coated on glass by Doctor Blade method for photo-catalytic degradation of an azo textile dye Reactive Red 4: XRD, FESEM and DRS investigations.

    PubMed

    Habibi, Mohammad Hossein; Parhizkar, Janan

    2015-11-01

    Cobalt ferrite nano-composite was prepared by hydrothermal route using cobalt nitrate, iron nitrate and ethylene glycol as chelating agent. The nano-composite was coated on glass by Doctor Blade method and annealed at 300 °C. The structural, optical, and photocatalytic properties have been studied by powder X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM) and UV-visible spectroscopy (UV-Vis DRS). Powder XRD analysis confirmed formation of CoFe2O4 spinel phase. The estimated particle size from FESEM data was 50 nm. The calculated energy band gaps, obtained by Tauc relation from UV-Vis absorption spectra was 1.3 eV. Photocatalytic degradation of Reactive Red 4 as an azo textile was investigated in aqueous solution under irradiation showed 68.0% degradation of the dye within 100 min. The experimental enhanced activity compare to pure Fe2O3 can be ascribed to the formation of composite, which was mainly attributable to the transfer of electron and hole to the surface of composite and hinder the electron hole recombination. PMID:26116997

  20. Effect of annealing temperature on optical properties of binary zinc tin oxide nano-composite prepared by sol-gel route using simple precursors: Structural and optical studies by DRS, FT-IR, XRD, FESEM investigations

    NASA Astrophysics Data System (ADS)

    Habibi, Mohammad Hossein; Mardani, Maryam

    2015-02-01

    Binary zinc tin oxide nano-composite was synthesized by a facile sol-gel method using simple precursors from the solutions consisting of zinc acetate, tin(IV) chloride and ethanol. Effect of annealing temperature on optical and structural properties was investigated using X-ray diffraction (XRD), diffuse reflectance spectra (DRS), field emission scanning electron microscopy (FESEM) and Fourier transform infrared spectroscopy (FTIR). XRD results revealed the existence of the ZnO and SnO2 phases. FESEM results showed that binary zinc tin oxide nano-composites ranges from 56 to 60 nm in diameter at 400 °C and 500 °C annealing temperatures respectively. The optical band gap was increased from 2.72 eV to 3.11 eV with the increasing of the annealing temperature. FTIR results confirmed the presence of zinc oxide and tin oxide and the broad absorption peaks at 3426 and 1602 cm-1 can be ascribed to the vibration of absorptive water, and the absorption peaks at 546, 1038 and 1410 cm-1 are due to the vibration of Zn-O or Sn-O groups in binary zinc tin oxide.

  1. Structural and magnetic characterization of La0.8Sr0.2MnO3 nanoparticles prepared via a facile microwave-assisted method

    NASA Astrophysics Data System (ADS)

    Moradi, J.; Ghazi, M. E.; Ehsani, M. H.; Kameli, P.

    2014-07-01

    Nanoparticles of La0.8Sr0.2MnO3 (LSMO) with different particle sizes are synthesized by a very fast, inexpensive, reproducible, and environmentally friendly method: the microwave irradiation of the corresponding mixture of nitrates. The structural and magnetic properties of the samples are investigated by the X-Ray diffraction (XRD), Fourier transform infra-red (FT-IR) spectroscopy, field-emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), and magnetic (DC magnetization and AC susceptibility) measurements. The XRD study coupled with the Rietveld refinement show that all samples crystallize in a rhombohedral structure with the space group of R-3C. The FT-IR spectroscopy and FE-SEM images indicate formation of the perovskite structure of LSMO. The DC magnetization measurements confirm the decrease in the particle size effects on the magnetic properties, e.g. reduction in the ferromagnetic (FM) moment and increase in the surface spin disorder. Magnetic dynamics of the samples studied by AC magnetic susceptibility shows that the magnetic behavior of the nanometer-sized samples is well-described by the Vogel-Fulcher and critical slowing down laws. Strong interaction between magnetic nanoparticles of LSMO was detected by fitting the experimental data with the mentioned models.

  2. Ferro- and antiferro-magnetism in (Np, Pu)BC

    SciTech Connect

    Klimczuk, T.; Kozub, A. L.; Griveau, J.-C.; Colineau, E.; Wastin, F.; Falmbigl, M.; Rogl, P.

    2015-04-01

    Two new transuranium metal boron carbides, NpBC and PuBC, have been synthesized. Rietveld refinements of powder XRD patterns of (Np,Pu)BC confirmed in both cases isotypism with the structure type of UBC. Temperature dependent magnetic susceptibility data reveal antiferromagnetic ordering for PuBC below T{sub N} = 44 K, whereas ferromagnetic ordering was found for NpBC below T{sub C} = 61 K. Heat capacity measurements prove the bulk character of the observed magnetic transition for both compounds. The total energy electronic band structure calculations support formation of the ferromagnetic ground state for NpBC and the antiferromagnetic ground state for PuBC.

  3. Magnetic attachment mechanism

    NASA Technical Reports Server (NTRS)

    Wu, Mitchell B. (inventor); Harwell, William D. (inventor)

    1988-01-01

    A magnetic attachment mechanism adapted for interfacing with the manipulator arm of a remote manipulator system and comprising a pair of permanent magnets of rare earth material are arranged in a stator-rotor relationship. The rotor magnet is journalled for rotation about its longitudinal axis between pole plates of the stator magnet, each of which includes an adhering surface. In a first rotary position corresponding to the ON condition, each of the poles of the rotor magnet is closely adjacent to a stator magnet pole plate of like polarity whereby the respective magnet fields are additive for producing a strong magnetic field emanating from the adhering surfaces for attracting a ferrous magnetic plate, or the like, affixed to the payload. When the rotor magnet is rotated to a second position corresponding to the OFF condition, each of the poles of the rotor magnet is disposed closely adjacent to a pole plate of unlike polarity whereby the magnetic fields of the magnets are in cancelling relationship at the adhering surfaces, which permits the release of a payload. An actuator for selectively rotating the rotor magnet between the ON and OFF positions is provided for interfacing and connecting the magnetic attachment mechanism with a manipulator arm. For affecting an optimal rigidized attachment the payload is provided with guide means cooperable with guide means on the housing of the mechanism for directing adhering surfaces of the polar plates to the ferrous plate.

  4. Single-molecule magnets

    NASA Astrophysics Data System (ADS)

    Aubin, Sheila Marie Josee

    This thesis discusses the syntheses and magnetization studies of several single-molecule magnets. These single- molecule magnets are also shown to display resonant magnetization tunneling. In chapter 1 an introduction into this area of research and similar areas of research are presented. In chapter 2 several complexes from a family of molecules with [ Mn4O3X]6+ cores are shown to behave as single-molecule magnets based on AC magnetic susceptibility measurements on microcrystalline and dilute frozen solution samples. In chapter 3 more detailed magnetic studies are reported for one complex from the Mn4 family of molecules-[ Mn4O3Cl(O2CCH3)3(dbm)3], where dbm is dibenzoylmethane. It is shown that this Mn4 complex exhibits resonant magnetization tunneling based on the observation of steps on magnetic hysteresis loops, ac magnetic susceptibility studies and the observation of a temperature-independent rate of magnetization relaxation below 0.6 K. In chapters 4 through 6 the syntheses and magnetization studies of several new Mn12 molecules with general composition [ Mn12O12(O2CR)16(H2O)4] are reported. From ac susceptibility measurements it is shown that some of these complexes exhibit much faster magnetic relaxation than others. Also, steps are observed at constant intervals of field on the magnetization hysteresis loops collected on some of these Mn12 complexes. This is evidence of field-tuned resonant magnetization tunneling.

  5. Structural and magnetic properties of chromium doped zinc ferrite

    SciTech Connect

    Sebastian, Rintu Mary; Thankachan, Smitha; Xavier, Sheena; Mohammed, E. M.; Joseph, Shaji

    2014-01-28

    Zinc chromium ferrites with chemical formula ZnCr{sub x}Fe{sub 2−x}O{sub 4} (x = 0.0, 0.2, 0.4, 0.6, 0.8, 1.0) were prepared by Sol - Gel technique. The structural as well as magnetic properties of the synthesized samples have been studied and reported here. The structural characterizations of the samples were analyzed by using X – Ray Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR), Scanning Electron Microscope (SEM), and Transmission Electron Microscope (TEM). The single phase spinel cubic structure of all the prepared samples was tested by XRD and FTIR. The particle size was observed to decrease from 18.636 nm to 6.125 nm by chromium doping and induced a tensile strain in all the zinc chromium mixed ferrites. The magnetic properties of few samples (x = 0.0, 0.4, 1.0) were investigated using Vibrating Sample Magnetometer (VSM)

  6. Photodegradation of Eosin Y Using Silver-Doped Magnetic Nanoparticles

    PubMed Central

    Alzahrani, Eman

    2015-01-01

    The purification of industrial wastewater from dyes is becoming increasingly important since they are toxic or carcinogenic to human beings. Nanomaterials have been receiving significant attention due to their unique physical and chemical properties compared with their larger-size counterparts. The aim of the present investigation was to fabricate magnetic nanoparticles (MNPs) using a coprecipitation method, followed by coating with silver (Ag) in order to enhance the photocatalytic activity of the MNPs by loading metal onto them. The fabricated magnetic nanoparticles coated with Ag were characterised using different instruments such as a scanning electron microscope (SEM), transmission electron microscopy (TEM), energy-dispersive X-ray (EDAX) spectroscopy, and X-ray diffraction (XRD) analysis. The average size of the magnetic nanoparticles had a mean diameter of about 48 nm, and the average particle size changed to 55 nm after doping. The fabricated Ag-doped magnetic nanoparticles were used for the degradation of eosin Y under UV-lamp irradiation. The experimental results revealed that the use of fabricated magnetic nanoparticles coated with Ag can be considered as reliable methods for the removal of eosin Y since the slope of evaluation of pseudo-first-order rate constant from the slope of the plot between ln⁡(Co/C) and the irradiation time was found to be linear. Ag-Fe3O4 nanoparticles would be considered an efficient photocatalyst to degrade textile dyes avoiding the tedious filtration step. PMID:26617638

  7. 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.

  8. 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.

  9. Radial magnetic field in magnetic confinement device

    NASA Astrophysics Data System (ADS)

    Xiong, Hao; Liu, Ming-Hai; Chen, Ming; Rao, Bo; Chen, Jie; Chen, Zhao-Quan; Xiao, Jin-Shui; Hu, Xi-Wei

    2015-09-01

    The intrinsic radial magnetic field (Br) in a tokamak is explored by the solution of the Grad-Shafranov equation in axisymmetric configurations through an expansion of the four terms of the magnetic surfaces. It can be inferred from the simulation results that at the core of the device, the tokamak should possess a three-dimensional magnetic field configuration, which could be reduced to a two-dimensional one when the radial position is greater than 0.6a. The radial magnetic field and the amzimuthal magnetic field have the same order of magnitude at the core of the device. These results can offer a reference for the analysis of the plasma instability, the property of the core plasma, and the magnetic field measurement. Project supported by the Special Domestic Program of ITER, China (Grant No. 2009GB105003).

  10. 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.

  11. Effect of quenching on the magnetic properties of Mg-ferrite thin films

    NASA Astrophysics Data System (ADS)

    Roy Dakua, Himadri; Venkataramani, N.; Prasad, Shiva

    2016-05-01

    We have investigated the microstructural and magnetic properties of the post annealed slow cooled and quenched Mg-ferrite thin films. The microstructural properties of these films were studied through XRD, TEM and SEM. The magnetic properties were studied using VSM at 300K and 10K. The quenched film showed ˜1.66 times higher magnetization at room temperature (RT) compared to the bulk and the slow cooled film (4πMS of bulk˜1880 Gauss at RT) though the crystal phase, grain size and thickness of both the films were similar. The change in the cation distribution is the plausible origin of large magnetization observed in the quenched (rapid cooled) film.

  12. Investigation of structural, thermal and magnetic properties of cadmium substituted cobalt ferrite nanoparticles

    NASA Astrophysics Data System (ADS)

    Venkata Reddy, Ch.; Byon, Chan; Narendra, B.; Baskar, D.; Srinivas, G.; Shim, Jaesool; Prabhakar Vattikuti, S. V.

    2015-06-01

    Cd substituted Cobalt ferrite nano particles are synthesis using co-precipitation method. The as prepared samples are calcinated at 300 and 600 °C respectively. The existence of single phase spinal cubic structure of the prepared ferrite material is confirmed by the powder XRD measurement. The surface morphology images, compositional features are studied by SEM with EDX, and TEM. From the FT-IR spectra the absorption bands observed at 595 and 402 cm-1 are attributed to vibrations of tetrahedral and octahedral complexes respectively. From the VSM data, parameters like magnetization, coercivity, remanent magnetization and remanent squareness are measured. The saturation magnetization value is increases with increasing calcination temperature. The DSC and TG-DTA curves reveal that the thermal stability of the prepared ferrite nanoparticles. The calcination temperature affects the crystallite size, morphology and magnetic properties of the samples.

  13. τ-MnAl with high coercivity and saturation magnetization

    SciTech Connect

    Wei, J. Z.; Song, Z. G.; Yang, Y. B.; Liu, S. Q.; Du, H. L.; Han, J. Z.; Zhou, D.; Wang, C. S.; Yang, Y. C.; Franz, A.; Többens, D.; Yang, J. B.

    2014-12-15

    In this paper, high purity τ-Mn{sub 54}Al{sub 46} and Mn{sub 54−x}Al{sub 46}C{sub x}alloys were successfully prepared using conventional arc-melting, melt-spinning, and heat treatment process. The magnetic and the structural properties were examined using x-ray diffraction (XRD), powder neutron diffraction and magnetic measurements. A room temperature saturation magnetization of 650.5 kAm{sup -1}, coercivity of 0.5 T, and a maximum energy product of (BH){sub max} = 24.7 kJm{sup -3} were achieved for the pure Mn{sub 54}Al{sub 46} powders without carbon doping. The carbon substituted Mn{sub 54−x}Al{sub 46}C{sub x}, however, reveals a lower Curie temperature but similar saturation magnetization as compared to the carbon-free sample. The electronic structure of MnAl shows that the Mn atom possesses a magnetic moment of 2.454 μ{sub B} which results from strong hybridization between Mn-Al and Mn-Mn. We also investigated the volume and c/a ratio dependence of the magnetic moments of Mn and Al. The results indicate that an increase in the intra-atomic exchange splitting due to the cell volume expansion, leads to a large magnetic moment for the Mn atom. The Mn magnetic moment can reach a value of 2.9 μ{sub B} at a volume expansion rate of ΔV/V ≈ 20%.

  14. Synthesis and characterization of magnetic palygorskite nanoparticles and their application on methylene blue remotion from water

    NASA Astrophysics Data System (ADS)

    Middea, Antonieta; Spinelli, Luciana S.; Souza, Fernando G.; Neumann, Reiner; Gomes, Otavio da F. M.; Fernandes, Thais L. A. P.; de Lima, Luiz C.; Barthem, Vitoria M. T. S.; de Carvalho, Fernanda V.

    2015-08-01

    Recently there has been considerable interest in magnetic sorbents materials, which is added excellent capabilities such as sorption and magnetic response to an applied field. Accordingly, palygorskite nanoparticles were covered by magnetite using a co-precipitation technique and characterized by: X-ray fluorescence (XRF), X-ray diffraction (XRD), surface analysing and scanning electron microscopy (SEM) with element analysis and mapping, particle size, pore surface area (BET), density, Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA) and zeta potential. Additionally, magnetic properties were studied by SQUID magnetometer, magnetic force microscopy (MFM) and also using a simple experimental setup. Magnetic nanoparticles produced had average diameters in a nanometric range. The amount of iron present in the nanoparticles increased by six times after the magnetization and a superparamagnetic behavior was exhibited with high saturation magnetization, from 4.0 × 10-4 Am2/kg to about 20 Am2/kg. A weight loss was also observed around 277 °C-339 °C by TGA, indicating a structural change from magnetite to maghemite, which confirms the magnetization of palygorskite. Batch adsorption experiments were carried out for the removal of methylene blue cationic dye from aqueous solution using pure and covered by magnetite palygorskite nanoparticles as adsorbents. Furthermore, about 90% of methylene blue was removed within 3 min using magnetized palygorskite.

  15. Synthesis and characterization of montmorillonite clay intercalated with molecular magnetic compounds

    SciTech Connect

    Martins, Marcel G.; Martins, Daniel O.T.A.; Carvalho, Beatriz L.C. de; Mercante, Luiza A.; Soriano, Stéphane; Andruh, Marius; Vieira, Méri D.; Vaz, Maria G.F.

    2015-08-15

    In this work montmorillonite (MMT) clay, whose matrix was modified with an ammonium salt (hexadecyltrimethylammonium bromide – CTAB), was employed as an inorganic host for the intercalation of three different molecular magnetic compounds through ion exchange: a nitronyl nitroxide derivative 2-[4-(N-ethyl)-pyridinium]-4,4,5,5-tetramethylimidazoline-1-oxyl-3-oxide (p-EtRad{sup +}) and two binuclear coordination compounds, [Ni(valpn)Ln]{sup 3+}, where H{sub 2}valpn stands for 1,3-propanediyl-bis(2-iminomethylene-6-methoxy-phenol), and Ln=Gd{sup III}; Dy{sup III}. The pristine MMT and the intercalated materials were characterized by X-ray powder diffraction (XRD), infrared spectroscopy (IR), scanning electron microscopy (SEM), thermogravimetric analysis (TGA) and magnetic measurements. The X-ray diffraction data analysis showed an increase of the interlamellar space of the intercalated MMT, indicating the intercalation of the magnetic compounds. Furthermore, the magnetic properties of the hybrid compounds were investigated, showing similar behavior as the pure magnetic guest species. - Graphical abstract: Montmorillonite clay was employed as inorganic host for the intercalation of three different molecular magnetic compounds through ion exchange - Highlights: • Montmorillonite was employed as a host material. • Three molecular magnetic compounds were intercalated through ion exchange. • The compounds were successful intercalated maintaining the layered structure. • The hybrid materials exhibited similar magnetic behavior as the pure magnetic guest.

  16. The cation inversion and magnetization in nanopowder zinc ferrite obtained by soft mechanochemical processing

    SciTech Connect

    Milutinović, A.; Lazarević, Z.; Jovalekić, Č.; Kuryliszyn-Kudelska, I.

    2013-11-15

    Graphical abstract: - Highlights: • Nano powder of ZnFe{sub 2}O{sub 4} prepared by a soft mechanochemical route after 18 h milling. • Phase formation controlled by XRD, Raman spectroscopy and magnetic measurements. • Size, strain and cation inversion degree determined by Rietveld refinement. • We were able to estimate the degree of inversion at most 0.348 and 0.4. • Obtained extremely high values of saturation magnetizations at T = 4.5 K. - Abstract: Two zinc ferrite nanoparticle materials were prepared by the same method – soft mechanochemical synthesis, but starting from different powder mixtures: (1) Zn(OH){sub 2}/α-Fe{sub 2}O{sub 3} and (2) Zn(OH){sub 2}/Fe(OH){sub 3}. In both cases a single phase system was obtained after 18 h of milling. The progress of the synthesis was controlled by X-ray diffractometry (XRD), Raman spectroscopy, TEM and magnetic measurements. Analysis of the XRD patterns by Rietveld refinement allowed determination of the cation inversion degree for both obtained single phase ZnFe{sub 2}O{sub 4} samples. The sample obtained from mixture (1) has the cation inversion degree 0.3482 and the sample obtained from mixture (2) 0.400. Magnetization measurements were confirmed that the degrees of the inversion were well estimated. Comparison with published data shows that used method of synthesis gives nano powder samples with extremely high values of saturation magnetizations: sample (1) 78.3 emu g{sup −1} and sample (2) 91.5 emu g{sup −1} at T = 4.5 K.

  17. Influence of spherical assembly of copper ferrite nanoparticles on magnetic properties: orientation of magnetic easy axis.

    PubMed

    Chatterjee, Biplab K; Bhattacharjee, Kaustav; Dey, Abhishek; Ghosh, Chandan K; Chattopadhyay, Kalyan K

    2014-06-01

    The magnetic properties of copper ferrite (CuFe2O4) nanoparticles prepared via sol-gel auto combustion and facile solvothermal method are studied focusing on the effect of nanoparticle arrangement. Randomly oriented CuFe2O4 nanoparticles (NP) are obtained from the sol-gel auto combustion method, while the solvothermal method allows us to prepare iso-oriented uniform spherical ensembles of CuFe2O4 nanoparticles (NS). X-ray diffractometry (XRD), atomic absorption spectroscopy (AAS), infra-red (IR) spectroscopy, Raman spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), (57)Fe Mössbauer spectroscopy and vibrating sample magnetometer (VSM) are used to investigate the composition, microstructure and magnetic properties of as-prepared ferrite nanoparticles. The field-dependent magnetization measurement for the NS sample at low temperature exhibits a step-like rectangular hysteresis loop (M(R)/M(S) ~ 1), suggesting cubic anisotropy in the system, whereas for the NP sample, typical features of uniaxial anisotropy (M(R)/M(S) ~ 0.5) are observed. The coercive field (HC) for the NS sample shows anomalous temperature dependence, which is correlated with the variation of effective anisotropy (K(E)) of the system. A high-temperature enhancement of H(C) and K(E) for the NS sample coincides with a strong spin-orbit coupling in the sample as evidenced by significant modification of Cu/Fe-O bond distances. The spherical arrangement of nanocrystals at mesoscopic scale provokes a high degree of alignment of the magnetic easy axis along the applied field leading to a step-like rectangular hysteresis loop. A detailed study on the temperature dependence of magnetic anisotropy of the system is carried out, emphasizing the influence of the formation of spherical iso-oriented assemblies. PMID:24714977

  18. Magnetic field modification of optical magnetic dipoles.

    PubMed

    Armelles, Gaspar; Caballero, Blanca; Cebollada, Alfonso; Garcia-Martin, Antonio; Meneses-Rodríguez, David

    2015-03-11

    Acting on optical magnetic dipoles opens novel routes to govern light-matter interaction. We demonstrate magnetic field modification of the magnetic dipolar moment characteristic of resonant nanoholes in thin magnetoplasmonic films. This is experimentally shown through the demonstration of the magneto-optical analogue of Babinet's principle, where mirror imaged MO spectral dependencies are obtained for two complementary magnetoplasmonic systems: holes in a perforated metallic layer and a layer of disks on a substrate. PMID:25646869

  19. Magnetic switch coupling to synchronize magnetic modulators

    DOEpatents

    Reed, K.W.; Kiekel, P.

    1999-04-27

    Apparatus for synchronizing the output pulses from a pair of magnetic switches is disclosed. An electrically conductive loop is provided between the pair of switches with the loop having windings about the core of each of the magnetic switches. The magnetic coupling created by the loop removes voltage and timing variations between the outputs of the two magnetic switches caused by any of a variety of factors. The only remaining variation is a very small fixed timing offset caused by the geometry and length of the loop itself. 13 figs.

  20. Magnetic switch coupling to synchronize magnetic modulators

    DOEpatents

    Reed, Kim W.; Kiekel, Paul

    1999-01-01

    Apparatus for synchronizing the output pulses from a pair of magnetic switches. An electrically conductive loop is provided between the pair of switches with the loop having windlings about the core of each of the magnetic switches. The magnetic coupling created by the loop removes voltage and timing variations between the outputs of the two magnetic switches caused by any of a variety of factors. The only remaining variation is a very small fixed timing offset caused by the geometry and length of the loop itself.