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Sample records for xrd hrtem magnetic

  1. Substructural Properties and Anisotropic Peak Broadening in Zn1-x Mn x Te Films Determined by a Combined Methodology Based on SEM, HRTEM, XRD, and HRXRD

    NASA Astrophysics Data System (ADS)

    Martinez-Tomas, C.; Klymov, O.; Agouram, S.; Kurbatov, D.; Opanasyuk, A.; Muñoz-Sanjosé, V.

    2016-09-01

    Lattice deformation and extended defects such as grain boundaries and dislocations affect the crystalline quality of films and can dramatically change material's properties. In particular, magnetic and optoelectronic properties depend strongly on these structural and substructural characteristics. In this paper, a combined methodology based on SEM, HRTEM, XRD, and HRXRD measurements is used to determine and assess the structural and substructural characteristics of films. This combined methodology has been applied to Zn1-x Mn x Te films grown on glass substrates by close-spaced vacuum sublimation. Nevertheless the methodology can be applied to a wide variety of materials and could become a useful characterization method which would be particularly valuable in semiconductor growth field. The knowledge of the structural and substructural characteristics can allow not only the optimization of growth parameters, but also the selection of specific samples having the desired characteristics (crystallite size, minimum dislocation content, etc.) for high-quality technological devices.

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

    PubMed

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

    2008-08-01

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

  3. 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.

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

    NASA Technical Reports Server (NTRS)

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

    1994-01-01

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

  5. Magnetic composites from minerals: study of the iron phases in clay and diatomite using Mössbauer spectroscopy, magnetic measurements and XRD

    NASA Astrophysics Data System (ADS)

    Cabrera, M.; Maciel, J. C.; Quispe-Marcatoma, J.; Pandey, B.; Neri, D. F. M.; Soria, F.; Baggio-Saitovitch, E.; de Carvalho, L. B.

    2014-01-01

    Magnetic particles as matrix for enzyme immobilization have been used and due to the enzymatic derivative can be easily removed from the reaction mixture by a magnetic field. This work presents a study about the synthesis and characterization of iron phases into magnetic montmorillonite clay (mMMT) and magnetic diatomaceous earth (mDE) by 57Fe Mössbauer spectroscopy (MS), magnetic measurements and X-ray diffraction (XRD). Also these magnetic materials were assessed as matrices for the immobilization of invertase via covalent binding. Mössbauer spectra of the magnetic composites performed at 4.2 K showed a mixture of magnetite and maghemite about equal proportion in the mMMT, and a pure magnetite phase in the sample mDE. These results were verified using XRD. The residual specific activity of the immobilized invertase on mMMT and mDE were 83 % and 92.5 %, respectively. Thus, both magnetic composites showed to be promising matrices for covalent immobilization of invertase.

  6. Structure and magnetic properties of Ge99.04Mn0.96 thin film prepared by thermal evaporation of Mn doped GeO2 ceramic film under hydrogen atmosphere

    NASA Astrophysics Data System (ADS)

    Jing, Chengbin; Guo, Hong; Bai, Wei; Hu, Zhigao; Yang, Jing; Yang, Pingxiong; Chu, Junhao; Liu, Aiyun; Lin, Fangting

    2013-12-01

    Ge99.04Mn0.96 thin film was fabricated by thermal evaporation of Mn doped GeO2 ceramic film under hydrogen atmosphere. Secondary phases were not detected by X-ray diffraction (XRD) and high resolution transmission electron microscopy (HRTEM) analyses. The film is p type. Room-temperature ferromagnetism was detected in the film. The ferromagnetic behavior may arise from alignment of the bound magnetic polarons (BMP) mediated by the localized holes in the system as well as ultra small secondary phases unable to be detected by XRD and HRTEM analyses.

  7. 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.

  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. Effect of Gd doping on the structural, luminescence and magnetic properties of ZnS nanoparticles synthesized by the hydrothermal method

    NASA Astrophysics Data System (ADS)

    Poornaprakash, B.; Chalapathi, U.; Reddeppa, Maddaka; Park, Si-Hyun

    2016-09-01

    This paper reports the synthesis and characterization of ZnS:Gd nanoparticles prepared by a hydrothermal process using different doping concentrations. The chemical, structural, luminescence and magnetic properties of these nanoparticles were investigated by X-ray diffraction (XRD), high resolution transmission electron microscopy (HRTEM), X-ray photoelectron spectroscopy (XPS), photoluminescence (PL) spectroscopy, and vibrating sample magnetometer (VSM) measurements. XRD confirmed that all the samples had a cubic structure with good crystallinity. HRTEM showed that the particles were polycrystalline with a mean size of 4-6 nm. XPS revealed the oxidation state of Gd in the ZnS lattice to be +3. The PL spectra of all the nanoparticles exhibited broad emission peaks in the visible region. All the Gd doped nanoparticles exhibited well-defined ferromagnetic behavior at room temperature. The saturation magnetization increased significantly with increasing Gd concentration, reaching a maximum for 3 at.% Gd and decreasing for the 5 at.% Gd doped ZnS nanoparticles.

  10. Fabrication and magnetism of α-Fe2O3 nanotubes via a multistep ac electrodeposition

    NASA Astrophysics Data System (ADS)

    Han, C.; Wang, Y.; Lu, T.; Yang, S.; Wang, L. Q.; Song, X. P.

    2015-07-01

    Hematite Fe2O3 nanotubes were successfully synthesized by a multistep ac electro-deposition on anodic aluminum oxide templates remaining the barrier layers. X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), high-resolution transmission electron microscopy (HRTEM), and magnetic measurements were used to characterize the morphology, structure, and magnetic properties of α-Fe2O3 nanotubes. Based on the characterization results, a self-assemble mechanism for electro-deposition α-Fe2O3 nanotubes was proposed. The magnetic property investigation showed that hematite Fe2O3 nanotubes exhibit ferromagnetic behavior with the Morin transition.

  11. 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.

  12. HRTEM at half-Angstrom resolution: From OAM to TEAM

    SciTech Connect

    O'Keefe, Michael A.

    2003-02-17

    Transmission electron microscopy (TEM) at sub-Angstrom resolution is important for nanotechnology. Identifying atom positions requires appropriate resolution, the ability to separate distinct objects in images. With Cs corrected, the information limit of the TEM controls resolution. The OAM has demonstrated that a resolution of 0.78A is possible. The TEAM (transmission electron achromatic microscope) will be a TEM using hardware correction of Cs with a monochromator to improve its information limit beyond that of the OAM by improvement of the electron-beam energy spread. It is shown that A 300keV HRTEM TEAM does not require a Cc corrector to reach 0.5A as long as beam energy spread and objective-lens current ripple are lowered sufficiently. A lower-voltage TEAM will require stricter limits on objective-lens current ripple to reach the targeted 0.5A resolution. No improvement in HT ripple or noise is required to improve the information limit per se since the monochromator determines the energy spread in the beam. However, improved HT ripple and noise will improve the beam current statistics (number of electrons passing through the monochromator) by placing more of the electrons closer to the center of the energy-spread distribution

  13. HRTEM analysis of solid precipitates in Xe-implanted aluminum

    SciTech Connect

    Allen, C.W.; Birtcher, R.; Ishikawa, N.; Furuya, K.; Awaji, M.

    1996-09-01

    High-resolution TEM was carried out to determine shape and atomic arrangement of solid Xe precipitates in Al. Polycrystalline Al TEM specimens were implanted with 30 keV Xe{sup +} at RT to a dose of 3x10{sup 20} ions/m{sup 2} and then annealed at 523 K. Below a size 4 nm dia, the Xe precipitates are solid with an fcc crystal structure mesotacticly aligned with the Al lattice. In HRTEM along [011] projection, the difference in the lattice parameters of solid Xe and Al produces a precipitate image dominated by a 2-D Moire pattern that repeats in both the <001> and <111> directions every 3 Al (or 2 Xe) lattice spacings. Multi-slice image simulations, using a 3-D atomic model, demonstrates that the precipitates are tetradecahedra with faces parallel to the dense {l_brace}111{r_brace} planes and the {l_brace}100{r_brace} planes. Off-Bragg illumination of the precipitates minimizes Al lattice fringes and generates precipitate images which are in good agreement with the model.

  14. 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.

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

    SciTech Connect

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

    2015-06-15

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

  16. In-situ synthesis of magnetic (NiFe 2O 4/CuO/FeO) nanocomposites

    NASA Astrophysics Data System (ADS)

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

    2010-11-01

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

  17. 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).

  18. Vanga Bhasma and its XRD analysis

    PubMed Central

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

    2010-01-01

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

  19. Statistical analysis of support thickness and particle size effects in HRTEM imaging of metal nanoparticles.

    PubMed

    House, Stephen D; Bonifacio, Cecile S; Grieshaber, Ross V; Li, Long; Zhang, Zhongfan; Ciston, Jim; Stach, Eric A; Yang, Judith C

    2016-10-01

    High-resolution transmission electron microscopy (HRTEM) examination of nanoparticles requires their placement on some manner of support - either TEM grid membranes or part of the material itself, as in many heterogeneous catalyst systems - but a systematic quantification of the practical imaging limits of this approach has been lacking. Here we address this issue through a statistical evaluation of how nanoparticle size and substrate thickness affects the ability to resolve structural features of interest in HRTEM images of metallic nanoparticles on common support membranes. The visibility of lattice fringes from crystalline Au nanoparticles on amorphous carbon and silicon supports of varying thickness was investigated with both conventional and aberration-corrected TEM. Over the 1-4nm nanoparticle size range examined, the probability of successfully resolving lattice fringes differed significantly as a function both of nanoparticle size and support thickness. Statistical analysis was used to formulate guidelines for the selection of supports and to quantify the impact a given support would have on HRTEM imaging of crystalline structure. For nanoparticles ≥1nm, aberration-correction was found to provide limited benefit for the purpose of visualizing lattice fringes; electron dose is more predictive of lattice fringe visibility than aberration correction. These results confirm that the ability to visualize lattice fringes is ultimately dependent on the signal-to-noise ratio of the HRTEM images, rather than the point-to-point resolving power of the microscope. This study provides a benchmark for HRTEM imaging of crystalline supported metal nanoparticles and is extensible to a wide variety of supports and nanostructures. PMID:27421079

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

    SciTech Connect

    O`Keefe, M.A.

    1992-11-01

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

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

    SciTech Connect

    O'Keefe, M.A.

    1992-11-01

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

  2. 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.

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

    PubMed

    Kılınç, Ersin

    2016-01-01

    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 as determined 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).

  4. Hybrid magnetic materials formed by ferritin intercalated into a layered double hydroxide

    NASA Astrophysics Data System (ADS)

    Clemente-León, Miguel; Coronado, Eugenio; Primo, Vicent; Ribera, Antonio; Soriano-Portillo, Alejandra

    2008-12-01

    A hybrid magnetic material formed by ferritin intercalated into a layered double hydroxide (LDH) of Mg and Al (Mg/Al molar ratio 2) is prepared and characterized through powder X-ray diffraction (XRD), thermogravimetric analysis (TGA), Fourier transform infrared (FT-IR) spectroscopy, electron probe microanalysis (EPMA) and high resolution transmission electron microscopy (HRTEM). One observes an enhancement in the thermal stability of the ferritin molecules when they are inserted in the layered material. Magnetic measurements of the hybrid material exhibit the typical superparamagnetic behaviour of the ferritin molecule. On the other hand, the intercalation of ferritin into the LDH guarantees a homogeneous dispersion of the ferritin molecules, which do not aggregate even after calcination of the sample. This feature allows obtaining well-dispersed magnetic metal oxide nanoparticles upon calcination of the hybrid material.

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

    PubMed

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

    2008-10-14

    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 MoS(2) 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 WS(2) 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.

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

    SciTech Connect

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

    1996-11-01

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

  7. 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.

  8. 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

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

    PubMed

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

    2013-01-01

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

  10. HRTEM observation of bonding interface between Ce-TZP/Al2O3 nanocomposite and porcelain.

    PubMed

    Ban, Seiji; Nawa, Masahiro; Sugata, Fumio; Tsuruki, Jiro; Kono, Hiroshi; Kawai, Tatsushi

    2014-01-01

    The surface of a ceria-stabilized tetragonal zirconia polycrystal (Ce-TZP/Al2O3) nanocomposite was sandblasted by alumina particles and veneered with feldspathic porcelain via a conventional condensation method. The part of each specimen containing the interface layer was sliced to ultrathin sections with an argon ion slicer, and these sliced sections were observed using high-resolution transmission electron microscopy (HRTEM). For both interfaces, Ce-TZP/porcelain and Al2O3/porcelain, no transition layers due to abrupt changes in atomic distributions were observed. Besides, the porcelain layers of both interfaces consisted of homogeneous amorphous phases. These results suggested that both Ce-TZP and Al2O3 could be directly bonded to porcelain by Van der Waals forces arising from the close contact between them.

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

    NASA Astrophysics Data System (ADS)

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

    2015-12-01

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

  12. 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.

  13. Fabrication and magnetic property analysis of monodisperse manganese-zinc ferrite nanospheres

    NASA Astrophysics Data System (ADS)

    Zhang, Qi; Zhu, Meifang; Zhang, Qinghong; Li, Yaogang; Wang, Hongzhi

    2009-10-01

    Monodisperse Mn-Zn ferrite (Mn 1-xZn xFe 2O 4) nanospheres have been prepared via a simple solvothermal method. The as-synthesized samples were characterized in detail by X-ray diffraction pattern (XRD), transmission electron microscope (TEM), high-solution transmission electron microscope (HRTEM), select area electron diffraction pattern (SAED), scanning electron microscope (SEM), and vibrating sample magnetometer (VSM). The results show that a large number of the high-purity Mn 1-xZn xFe 2O 4 nanocrystallites were synthesized and these nanocrystallites oriented aggregated to nanospheres. The dependence of magnetic properties of Mn 1-xZn xFe 2O 4 nanospheres on the composition content x of Zn was studied. The maximum saturation magnetization value of the as-prepared sample (Mn 0.6Zn 0.4Fe 2O 4) reached 52.4 emu g -1.

  14. 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.

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

    SciTech Connect

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

    2010-11-15

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

  16. Structural and magnetic characterization of ZnCo2O4 thin film prepared by pulsed laser deposition

    NASA Astrophysics Data System (ADS)

    Wen, X. L.; Chen, Z.; Liu, E. H.; Lin, X.

    2015-12-01

    We report the structural and magnetic characterization of ZnCo2O4 (ZCO) thin films fabricated by pulsed laser deposition on sapphire substrates. Structural analysis measured by X-ray diffraction (XRD), high resolution transmission electron microscopy (HRTEM) and atomic force microscope (AFM) shows that the ZCO thin film grew in a layer-by-layer mode, and forms a cubic spinel structure with Fd-3m space group. Electronic states detected by X-ray photoelectron spectroscopy (XPS) prove that Co2+ ions occupied on the Zn sites in the ZCO film and oxygen vacancies exist. Magnetic measurements show a strong ferromagnetic behavior. The possible mechanisms for the ferromagnetic property are extensively discussed. Our work is believed to contribute a good understanding of the microscopic ferromagnetism origin of the high-Tc ZCO film, which is significant for expanding their applications into high-effective spin-electronic devices.

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

    NASA Astrophysics Data System (ADS)

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

    2015-08-01

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

  18. 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.

  19. Limitations to the Measurement of Oxygen Concentrations by HRTEM Imposed by Surface Roughness

    SciTech Connect

    Lupini, Andrew R; Chisholm, Matthew F; van Benthem, Klaus; Allen, L. J.; Oxley, Mark P; Findlay, Scott D.; Varela del Arco, Maria; Pennycook, Stephen J

    2005-01-01

    In an article published in Microscopy and Microanalysis recently (Jia et al., 2004), it was claimed that aberration-corrected high resolution transmission electron microscopy (HRTEM) allows the quantitative measurement of oxygen concentrations in ceramic materials with atomic resolution. Similar claims have recently appeared elsewhere, based on images obtained through aberration correction (Jia et al., 2003; Jia & Urban, 2004) or very high voltages (Zhang et al., 2003). Seeing oxygen columns is a significant achievement of great importance (Spence, 2003) that will doubtlessly allow some exciting new science; however, other models could provide a better explanation for some of the experimental data than variations in the oxygen concentration. Quantification of the oxygen concentrations was attempted by comparing experimental images with simulations in which the fractional occupancy in individual oxygen columns was reduced. The results were interpreted as representing nonstoichiometry within the bulk and at grain boundaries. This is plausible because previous studies have shown that grain boundaries can be nonstoichiometric (Kim et al., 2001), and it is indeed possible that oxygen vacancies are present at boundaries or in the bulk. However, is this the only possible interpretation? We show that for the thicknesses considered a better match to the images is obtained using a simple model of surface damage in which atoms are removed from the surface, which would usually be interpreted as surface damage or local thickness variation (from ion milling, for example).

  20. 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.

  1. Quantitative atom column position analysis at the incommensurate interfaces of a (PbS)(1.14)NbS(2) misfit layered compound with aberration-corrected HRTEM.

    PubMed

    Garbrecht, M; Spiecker, E; Tillmann, K; Jäger, W

    2011-02-01

    Aberration-corrected HRTEM is applied to explore the potential of NCSI contrast imaging to quantitatively analyse the complex atomic structure of misfit layered compounds and their incommensurate interfaces. Using the (PbS)(1.14)NbS(2) misfit layered compound as a model system it is shown that atom column position analyses at the incommensurate interfaces can be performed with precisions reaching a statistical accuracy of ±6pm. The procedure adopted for these studies compares experimental images taken from compound regions free of defects and interface modulations with a structure model derived from XRD experiments and with multi-slice image simulations for the corresponding NCSI contrast conditions used. The high precision achievable in such experiments is confirmed by a detailed quantitative analysis of the atom column positions at the incommensurate interfaces, proving a tetragonal distortion of the monochalcogenide sublattice.

  2. 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.

  3. TEM, HRTEM, electron holography and electron tomography studies of gamma' and gamma'' nanoparticles in Inconel 718 superalloy.

    PubMed

    Dubiel, B; Kruk, A; Stepniowska, E; Cempura, G; Geiger, D; Formanek, P; Hernandez, J; Midgley, P; Czyrska-Filemonowicz, A

    2009-11-01

    The aim of the study was the identification of gamma' and gamma'' strengthening precipitates in a commercial nickel-base superalloy Inconel 718 (Ni-19Fe-18Cr-5Nb-3Mo-1Ti-0.5Al-0.04C, wt %) using TEM dark-field, HRTEM, electron holography and electron tomography imaging. To identify gamma' and gamma'' nanoparticles unambiguously, a systematic analysis of experimental and theoretical diffraction patterns were performed. Using HRTEM method it was possible to analyse small areas of precipitates appearance. Electron holography and electron tomography techniques show new possibilities of visualization of gamma' and gamma'' nanoparticles. The analysis by means of different complementary TEM methods showed that gamma'' particles exhibit a shape of thin plates, while gamma' phase precipitates are almost spherical. PMID:19903242

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

    NASA Astrophysics Data System (ADS)

    Jozwik-Biala, I.; Jagielski, J.; Thomé, L.; Arey, B.; Kovarik, L.; Sattonnay, G.; Debelle, A.; Monnet, I.

    2012-09-01

    High Resolution Scanning Transmission Electron Microscopy (HRTEM) experiments were performed on Gd2Ti2O7 pyrochlore 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 Scanning Transmission Electron Microscopy (STEM) imaging modes: High- and Low-Angle Annular Dark Field imaging (HAADF and LAADF), it was possible to observe the radial substructure of tracks composed of an amorphous core surrounded by a damaged and strained crystalline envelope.

  5. 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.

  6. 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.

  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. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2016-09-01

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

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

    SciTech Connect

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

    2014-04-24

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

  11. 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 (βa) and scattering (αs) coefficients of the particles emitted by cook stoves were measured. The trend in βa and αs 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.

  12. Synthesis of Fe3O4/SiO2/CeO2 core-shell magnetic and their application as photocatalyst.

    PubMed

    Channei, D; Inceesungvorn, B; Wetchakun, N; Phanichphant, S

    2014-10-01

    The Fe3O4/SiO2/CeO2 core-shell magnetic has been successfully synthesized by three steps of hydrothermal, sonochemical and homogeneous precipitation by coating CeO2 nanoparticles onto Fe3O4/SiO2 magnetic core. The prepared samples were characterized by X-ray diffraction (XRD), Field-emission scanning electron microscopy (FESEM) connected with energy dispersive X-ray analysis system (EDS), high resolution transmission electron microscopy (HRTEM), Nitrogen adsorption-desorption analyses (BET), and vibrating sample magnetometer (VSM). The photocatalytic activities for Fe3O4/SiO2/CeO2 core-shell magnetic under UV and visible lights were measured by determining the degradation rate of formic and oxalic acid in spiral reactor for 120 min. The amounts of CO2 generated during the process were compared between the magnetic catalyst and bare CeO2. After the finished photocatalytic degradation, the magnetic catalyst was recovered by external magnetic field at the end of each experiment. The results showed that the photocatalytic activity of Fe3O4/SiO2/CeO2 core-shell magnetic had higher than that of bare CeO2 and was found to be constant for three cycles of the recycled use.

  13. 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.

  14. 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.

  15. 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.

  16. 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

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

    SciTech Connect

    Pransisco, Prengki; Shafie, Afza Guan, Beh Hoe

    2015-07-22

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

  18. 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.

  19. Porosity investigation of compacted bentonite using XRD profile modeling

    NASA Astrophysics Data System (ADS)

    Holmboe, Michael; Wold, Susanna; Jonsson, Mats

    2012-02-01

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

  20. Integration of TEM/Hrtem onservations and C-isotope geochemistry to characterize organic matter in early Archaean rocks

    NASA Astrophysics Data System (ADS)

    Glikson, M.; Golding, S.; Duck, L.; Webb, R.

    2009-04-01

    TEM was applied to observe and characterize carbonaceous materials (CM) extracted from black cherts in the 'white smoker type' deposit of the ca.3.5Ga (model Pb/Pb ages =3.49-3.51Ga) Dresser ormation, and the overlying black argillites of the 3.46Ga Salgash Subgroup, in the Pilbara of Western Australia. These were characterized by Transmission Electron Microscopy (TEM) coupled with electron dispersive spectral analysis (EDS), High Resolution TEM (HRTEM) to determine molecular ordering, and C-isotope geochemistry. Observations using TEM and HRTEM enabled morphological and fine structure distinctions between the various populations of CM both in the Dresser and Salgash samples. These formed the basis for their interpretations. Organic petrology using reflected light microscopy was applied to whole rock samples to observe mineral-organic relationship and structure relative to host rock texture. These supported insitu, syn-depositional mode for the Dresser Formation CM. Reflectance % (Ro) of CM determined on polished whole rock samples and polished resin-embedded CM concentrates enabled the reconstruction of its thermal history. These yielded several Ro populations in the Dresser Formation samples: probable microbial cells preserved in fluid inclusions within quartz crystals, severely thermally degraded CM possibly originally belonging to microbial cells, CM coating mineral grains and reworked CM particles. On the other hand, the Salgash suite of samples from the Apex Basalt Formation yielded consistent very high Ro values corresponding to graphite stage organic metamorphism. the weak optical anisotropy of the graphite points to a defferent mode of formation than regional metamorphism. Two main graphite forms have been identified, namely a platy and tubular. The tubular form when observed in HRTEM showed nano-tubes and fullerenes. Dresser Formation samples are isotopically light in the range of -32.1 to -38.2per mil supporting a biological source. Although in TEM four

  1. Optimum HRTEM image contrast at 20 kV and 80 kV--exemplified by graphene.

    PubMed

    Lee, Z; Meyer, J C; Rose, H; Kaiser, U

    2012-01-01

    The dependence of high-resolution transmission electron microscopy (HRTEM) image contrast of graphene on the adjustable parameters of an aberration-corrected microscope operated at 80 and 20 kV has been calculated and, for 80 kV, compared with measurements. We used density functional theory to determine the projected atom potential and obtained the image intensity by averaging over the energy distribution of the imaging electrons, as derived from the electron energy loss spectroscopy measurements. Optimum image contrast has been determined as a function of energy spread of the imaging electrons and chromatic aberration coefficient, showing that significant improvement of contrast can be achieved at 80 kV with the help of a monochromator, however at 20 kV only with chromatic aberration correction and bright atom contrast conditions.

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

    NASA Astrophysics Data System (ADS)

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

    2015-07-01

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

  3. 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.

  4. 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.

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

    NASA Technical Reports Server (NTRS)

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

    1992-01-01

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

  6. Magnetic composite BiOCl-SrFe12O19: a novel p-n type heterojunction with enhanced photocatalytic activity.

    PubMed

    Xie, Taiping; Xu, Longjun; Liu, Chenglun; Yang, Jun; Wang, Mei

    2014-02-01

    The magnetic composite BiOCl-SrFe12O19, a novel p-n type heterojunction was synthesized by hydrolysis with a medium temperature sintering method. The microstructure and magnetic properties of the prepared material were characterized by FTIR, XRD, SEM, TEM, HRTEM, SAED, and VSM. The results showed the [001] facet of BiOCl with high photocatalytic activity was exposed in the BiOCl-SrFe12O19. The heterostructured BiOCl-SrFe12O19 had better magnetic properties, contributing to its reuse and improvement in photocatalysis. Moreover, the composite was blessed with excellent photocatalytic activity and stability. In the BiOCl-SrFe12O19 system, SrFe12O19 not only inhibited the growth of BiOCl along the [001] direction to enhance the exposure of the [001] wafer, but also acted as a sensitizer absorbing light irradiation. The magnetic field generated from SrFe12O19 made BiOCl, under light irradiation, produce more photo-induced electrons and holes and simultaneously hampered their recombination. For the first time we propose the possible mechanism of how to enhance photocatalytic activity by a magnetic field effect originating from the magnetic photocatalyst itself. PMID:24297101

  7. Mirrored low-energy channel for the MiniXRD

    NASA Astrophysics Data System (ADS)

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

    2015-08-01

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

  8. 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.

  9. 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.

  10. 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

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

    PubMed

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

    2016-01-01

    Spine Mn(x)Co₁₋xAl₂O₄ (x = 0, 0.3 and 0.5) nanoparticles were synthesized using Sesamum indicum (S. indicum) plant extracted microwave-assisted combustion method. S. indicum plant extract simplifies the process, provides an alternative process for a simple, economical and environment friendly synthesis. The absence of surfactant/catalysts has led to a simple, cheap and fast method of synthesis of spinel nanoparticles. The as-synthesized spinel nanoparticles were characterized by X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy, high resolution scanning electron microscopy (HR-SEM), high resolution transmission electron microscopy (HR-TEM), energy dispersive X-ray analysis (EDX), Brunauer Emmett Teller (BET) surface area analysis, UV-Visible diffuse reflectance spectroscopy (DRS), Photoluminescence (PL) spectroscopy, and vibrating sample magnetometer. The formation of spinel nanoparticles was confirmed by HR-SEM and HR-TEM and their possible formation mechanisms were also proposed. Powder XRD, FT-IR, SAED and EDX results confirmed the formation of pure and single cubic phase CoAl₂O₄ with well-defined crystalline. The optical property was determined by DRS and PL spectra. VSM measurements revealed that pure and Mn-doped CoAl₂O₄ samples have weak ferromagnetic behavior and the magnetization values increases with increasing the concentration of Mn²⁺ ions in the CoAl₂O₄ lattice. The sample Mn₀.₅Co₀.₅Al₂O₄ possessed higher surface area and smaller crystallite size than other samples, which led to enhance the performance toward the selective oxidation of benzyl alcohol into benzaldehyde. PMID:27398473

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

    PubMed

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

    2016-01-01

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

  13. 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.

  14. 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

  15. Controlled synthesis and magnetic properties of monodispersed ceria nanoparticles

    SciTech Connect

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

    2015-02-15

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

  16. 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.

  17. Combined HRTEM, X-ray microchemical and EELS fine structure analysis of planar defects in YBa 2Cu 3O 7-δ

    NASA Astrophysics Data System (ADS)

    Dravid, V. P.; Zhang, Hong; Marks, L. D.; Zhang, J. P.

    1992-03-01

    High temperature superconductors in the systems YBa 2Cu 3O 7-δ (123) and decomposed YBa 2Cu 4O 7-δ (124) often contain planar faults with (001) as the nominal fault plane. Such planar defects have been analyzed using a unique combination of high resolution TEM (HRTEM) imaging and high resolution analytical electron microscopy (HRAEM). HRTEM confirmed that these planar faults are stacking faults with double or multiple insertion of crystal planes parallel to the c-plane of the crystal, most probably CuO planes. X-ray microanalysis clearly showed enrichment of copper associated with these defects. EELS fine structure of CuL 23 edge from the fault regions resembled that of pure CuO. The combined results indicate that the planar defects are in fact insertions of extra CuO planes in an otherwise regular 123 crystal unit cell.

  18. Synthesis of Iron Oxide Nanoparticles from Iron Acetylacetonate and Cyclopentadienyliron Dicarbonyl Dimer in Low Pressure Plasma — Effect of Plasma Parameters on Morphology and Magnetic Properties

    NASA Astrophysics Data System (ADS)

    Panchal, Vineet; Bhandarkar, Upendra; Neergat, Manoj; Suresh, K. G.

    2015-03-01

    Iron oxide nanoparticles are synthesized using organometallic precursors namely, iron (III) acetylacetonate and cyclopentadienyliron dicarbonyl dimer in a capacitively coupled low pressure plasma system. They are characterized using High Resolution Transmission Electron Microscopy (HRTEM), X-ray Diffraction (XRD), magnetization studies and Raman spectroscopy. The role of hydrogen and RF (Radio Frequency) power on the crystalline and magnetic properties of the nanoparticles is studied. Incorporation of hydrogen to the Plasma-Enhanced Chemical Vapor Deposition (PECVD) chamber during the synthesis facilitates both crystallization of iron oxide nanoparticles and reduction of carbon content in the product. The saturation magnetization of iron oxide nanoparticles synthesized using iron (III) acetylacetonate and cyclopentadienyliron dicarbonyl dimer in presence of hydrogen at 200 W RF power is higher than that synthesized in the absence of hydrogen at 50 W RF power. In case of nanoparticles synthesized using iron (III) acetylacetonate, the saturation magnetization increases from 1.5 emu g-1 to 19 emu g-1, and for the same synthesized from cyclopentadienyliron dicarbonyl dimer it increases from 3.2 emu g-1 to 22.4 emu g-1.

  19. Characteristics and genesis of maghemite in Chinese loess and paleosols: Mechanism for magnetic susceptibility enhancement in paleosols [rapid communication

    NASA Astrophysics Data System (ADS)

    Chen, Tianhu; Xu, Huifang; Xie, Qiaoqin; Chen, Jun; Ji, Junfeng; Lu, Huayu

    2005-12-01

    Morphological characteristics and microstructures of magnetic minerals extracted from Chinese loess and paleosols were investigated using powder X-ray diffraction (XRD) and high-resolution transmission electron microscopy (HRTEM). Our results indicate that maghemite in loess-paleosol sequences was transformed from magnetite through oxidation of magnetite. Maghemite transformed from eolian magnetite during chemical weathering has low-angle grain boundaries among maghemite nano-crystals. Some nano-crystalline maghemites with nanoporous texture resulted from microbe-induced precipitation of magnetite or transformation of poorly crystalline ferric Fe (oxy)hydroxides in presence of Fe-reducing bacteria. Aggregates of euhedral maghemite nano-crystals were transformed from magnetite magnetosomes. Both microbe-induced nanoporous magnetite and microbe-produced magnetite magnetosomes are directly related to microbial activities and pedogenesis of the paleosols. It is proposed that the formation of nano-crystalline maghemite with superparamagnetic property in paleosol results in the enhancement of magnetic susceptibility, although the total amount (weight percent) of magnetic minerals in both paleosol and loess units is similar. Our results also show that nano-crystalline and nanoporous magnetite grains prefer to transform into maghemite in semi-arid soil environments instead of hematite, although hematite is a thermodynamically stable phase. This result also indicates that a decrease in crystal size will increase stability of maghemite. It is also inferred that surface energy of maghemite is lower than that of hematite.

  20. VESPERS: A Beamline for Combined XRF and XRD Measurements

    NASA Astrophysics Data System (ADS)

    Feng, Renfei; Gerson, Andrea; Ice, Gene; Reininger, Ruben; Yates, Brian; McIntyre, Stewart

    2007-01-01

    VESPERS (VEry Sensitive Elemental and Structural Probe Employing Radiation from a Synchrotron) is a bending magnet beamline that is just beginning construction at the Canadian Light Source. The beamline has several novel design elements that are intended to increase its operating flexibility and availability to users. First, there is a requirement to deliver a microscopic beam with a variable bandwidth, thus enabling the generation of Laue diffraction patterns and high yield X-ray fluorescence spectra from the same region preferably simultaneously. Thus, the bandpass of the VESPERS monochromator can be readily changed to focus radiation into the same 2-4 micron diameter area that is either polychromatic or having a bandwidth of 10%, 1.6% or 0.01%. This allows the user to change the diffraction pattern to suit the complexity of the crystal and the spectral signal to noise ratio to suit the detection sensitivity required. Second, the beamline is designed to have two branches capable of operating simultaneously and virtually independently using the same primary optics. These design features are accomplished using four separate beams originating at four pinholes at the entry to the Primary Optical Enclosure. The compound focus design uses spherical mirrors to focus both polychromatic and pre-monochromatic beams onto the intermediate slits. A pair of bendable K-B mirrors in the experimental hutch is used to demagnify the beam further down to micron size. The photon energy of this beamline is 6-30 keV.

  1. Nanoscale chemical and structural study of Co-based FEBID structures by STEM-EELS and HRTEM

    PubMed Central

    2011-01-01

    Nanolithography techniques in a scanning electron microscope/focused ion beam are very attractive tools for a number of synthetic processes, including the fabrication of ferromagnetic nano-objects, with potential applications in magnetic storage or magnetic sensing. One of the most versatile techniques is the focused electron beam induced deposition, an efficient method for the production of magnetic structures highly resolved at the nanometric scale. In this work, this method has been applied to the controlled growth of magnetic nanostructures using Co2(CO)8. The chemical and structural properties of these deposits have been studied by electron energy loss spectroscopy and high-resolution transmission electron microscopy at the nanometric scale. The obtained results allow us to correlate the chemical and structural properties with the functionality of these magnetic nanostructures. PMID:22085532

  2. EXAFS and HRTEM evidence for As(III)-containing surface precipitates on nanocrystalline magnetite: implications for As sequestration.

    PubMed

    Morin, Guillaume; Wang, Yuheng; Ona-Nguema, Georges; Juillot, Farid; Calas, Guillaume; Menguy, Nicolas; Aubry, Emmanuel; Bargar, John R; Brown, Gordon E

    2009-08-18

    Arsenic sorption onto iron oxide spinels such as magnetite could contribute to immobilization of arsenite (AsO3(3-)), the reduced, highly toxic form of arsenic in contaminated anoxic groundwaters, as well as to putative remediation processes. Nanocrystalline magnetite (<20 nm) is known to exhibit higher efficiency for arsenite sorption than larger particles, sorbing as much as approximately 20 micromol/m2 of arsenite. To improve our understanding of this process, we investigated the molecular level structure of As(III)-containing sorption products on two types of fine-grained magnetite: (1) a biogenic one with an average particle diameter of 34 nm produced by reduction of lepidocrocite (gamma-FeOOH) by Shewanella putrefaciens and (2) a synthetic, abiotic, nanocrystalline magnetite with an average particle diameter of 11 nm. Results from extended X-ray absorption spectroscopy (EXAFS) for both types of magnetite with As(III) surface coverages of up to 5 micromol/m2 indicate that As(III) forms dominantly inner-sphere, tridentate, hexanuclear, corner-sharing surface complexes (3C) in which AsO3 pyramids occupy vacant tetrahedral sites on octahedrally terminated {111} surfaces of magnetite. Formation of this type of surface complex results in a decrease in dissolved As(III) concentration below the maximum concentration level recommended by the World Health Organization (10 microg/L), which corresponds to As(III) surface coverages of 0.16 and 0.19 micromol/m2 in our experiments. In addition, high-resolution transmission electron microscopy (HRTEM) coupled with energy dispersive X-ray spectroscopy (EDXS) analyses revealed the occurrence of an amorphous As(III)-rich surface precipitate forming at As(III) surface coverages as low as 1.61 micromol/m2. This phase hosts the majority of adsorbed arsenite at surface coverages exceeding the theoretical maximum site density of vacant tetrahedral sites on the magnetite {111} surface (3.2 sites/nm2 or 5.3 micromol/m2). This finding

  3. In situ synthesis and characterization of magnetic nanoparticles in shells of biodegradable polyelectrolyte microcapsules.

    PubMed

    Lyubutin, I S; Starchikov, S S; Bukreeva, T V; Lysenko, I A; Sulyanov, S N; Korotkov, N Yu; Rumyantseva, S S; Marchenko, I V; Funtov, K O; Vasiliev, A L

    2014-12-01

    Hollow microcapsules with the shell composed of biodegradable polyelectrolytes modified with the maghemite nanoparticles were fabricated by in situ synthesis. The nanoparticles were synthesized from the iron salt and the base directly on the capsule shells prepared by "layer by layer" technique. An average diameter of the capsule was about 6.7 μm while the average thickness of the capsule shell was 0.9 μm. XRD, HRTEM, Raman and Mössbauer spectroscopy data revealed that the iron oxide nanoparticles have the crystal structure of maghemite γ-Fe2O3. The nanoparticles were highly monodisperse with medium size of 7.5 nm. The Mössbauer spectroscopy data revealed that the nanoparticles have marked superparamagnetic behavior which was retained up to room temperature due to slow spin relaxation. Because of that, the microcapsules can be handled by an external magnetic field. Both these properties are important for target drug delivery. Based on the Mössbauer spectroscopy data, the spin blocking temperatures TB of about 90K was found for the particles with size D≤5 nm and TB≈250 K for particles with D≥6 nm. The anisotropy constants K were determined using the superparamagnetic approximation and in the low temperature approximation of collective magnetic excitation. PMID:25491824

  4. 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.

  5. 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.

  6. MAGNETS

    DOEpatents

    Hofacker, H.B.

    1958-09-23

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

  7. 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.

  8. Size dependence of the magnetic and hyperfine properties of nanostructured hematite ( α-Fe 2 O 3 ) powders prepared by the ball milling technique

    NASA Astrophysics Data System (ADS)

    André-Filho, J.; León-Félix, L.; Coaquira, J. A. H.; Garg, V. K.; Oliveira, A. C.

    2014-01-01

    In this work we present the study of hematite ( α-Fe2O3) nanostructures synthesized by the ball milling technique. The structural characterization and the crystallite size estimation have been carried out using the X-ray diffraction (XRD) technique. Data analyses indicate that the hematite phase (space group, R-3C) is preserved after the milling process. As the milling time is increased, a second phase ( α-Fe) appears. The mean crystallite size shows a decreasing tendency as the milling time is increased. High-resolution transmission electron microscopy (HRTEM) images show the formation of grains composed of crystallites with irregular shapes. Mössbauer spectra of milled powders carried out at 297 and 77 K are well modeled with a histogram distribution of hyperfine fields. The presence of one additional sextet which corresponds to the ∝-Fe phase is also determined in agreement with XRD data analysis. Magnetic measurements suggest the suppression of the Morin transition in the milled samples and the absence of thermal relaxation effects in agreement with the Mössbauer spectroscopy results.

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

    NASA Astrophysics Data System (ADS)

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

    2016-07-01

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

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

    PubMed

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

    2011-01-01

    The main aim of this study was to synthesize magnetic separable Nickel/powdered activated carbon (Ni/PAC) and its application as an adsorbent for removal of PFOS from aqueous solution. In this work, the synthesized adsorbent using simple method was characterized by using X-ray diffractionometer (XRD), surface area and pore size analyzer, vibrating sample magnetometer (VSM), and high resolution transmission electron microscope (HRTEM). The surface area, pore volume and pore size of synthesized PAC was 1521.8 m(2)g(-1), 0.96 cm(3)g(-1), 2.54 nm, respectively. Different kinetic models: the pseudo-first-order model, the pseudo-second-order model, and three adsorption isotherms--Langmuir, Freundlich and Temkin--were applied to study the sorption kinetics and isothermal behavior of PFOS onto the surface of an as-prepared adsorbent. The rate constant using the pseudo-second-order model for removal of 150 ppm PFOS was estimated as 8.82×10(-5) and 1.64×10(-4) for PAC and 40% Ni/PAC, respectively. Our results demonstrated that the composite adsorbents exhibited a clear magnetic hysteretic behavior, indicating the potential practical application in magnetic separation of adsorbents from aqueous solution phase as well. PMID:21961696

  11. Synthesis, structural, optical, and magnetic properties of Co doped, Sm doped and Co+Sm co-doped ZnS nanoparticles

    NASA Astrophysics Data System (ADS)

    Poornaprakash, B.; Poojitha, P. T.; Chalapathi, U.; Subramanyam, K.; Park, Si-Hyun

    2016-09-01

    The compositional, structural, optical and magnetic properties of ZnS, Zn0.98Co0.02S, Zn0.98Sm0.02S and Zn0.96Co0.02Sm0.02S nanoparticles synthesized by a hydrothermal method are presented and discussed. X-ray diffraction (XRD), high resolution transmission electron microscopy (HRTEM) and selected area electron diffraction (SAED) studies revealed that all the samples exhibited cubic structure without any impurity phases. X-ray photoelectron spectroscopy (XPS) results revealed that the Co and Sm ions existed in +2 and +3 states in these samples. The photoluminescence (PL) spectra of all the samples exhibited a broad emission in the visible region. The room temperature magnetization versus applied magnetic field (M-H) curves demonstrated that the Sm+Co doped nanoparticles exhibited enhanced ferromagnetic behavior compare to Co and Sm individually doped ZnS nanoparticles, which is probably due to the exchange interaction between conductive electrons with local spin polarized electrons on the Co2+ or Sm3+ ions. This study intensifies the understanding of the novel performances of co-doped ZnS nanoparticles and also provides possibilities to fabricate future spintronic devices.

  12. 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.

  13. Interface characterization of XUV multilayer reflectors using HRTEM (high-resolution transmission electron microscopy) and x-ray and XUV reflectance

    SciTech Connect

    Windt, D.L.; Hull, R.; Waskiewicz, W.K.; Kortright, J.B.

    1990-07-01

    We have examined the structure of XUV multilayer coatings using high-resolution transmission electron microscopy (HRTEM). Using a variety of techniques, we have measured the interface widths and the interface topography from the digitized TEM images, and have compared these results to x-ray and XUV reflectance measurements. We find that the structural parameters measured from the TEM images and those deduced from reflectance are consistent in light of the probable systematic errors associated with the measurement and interpretation techniques. 14 refs., 12 figs., 1 tab.

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

    NASA Astrophysics Data System (ADS)

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

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

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

    NASA Astrophysics Data System (ADS)

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

    2016-08-01

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

  16. 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.

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

    NASA Astrophysics Data System (ADS)

    Ostrooumov, M.

    2016-08-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2014-09-01

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

  19. An HRTEM investigation of the metastable low-temperature silica phase opal-CT in cherts and porcelanites from the Monterey Formation, CA

    SciTech Connect

    Cady, S.L.; Wenk, H.R. )

    1992-01-01

    High resolution transmission electron microscopy (HRTEM) is used to investigate the metastable low-temperature silica phase opal-CT in cherts and porcelanites from the Miocene Monterey Formation of California. Low-dose imaging techniques developed to image highly beam sensitive proteins were used in this study and have resulted in good phase contrast images of this hydrous silica phase. Detailed X-ray powder diffraction studies of stratigraphically equivalent rocks along the Santa Barbara coast indicate that the primary d-spacing of newly formed opal-CT differs in rocks with different ratios of silica and detrital minerals. Opal-CT forms progressively later and with a smaller primary d-spacing in rocks with increasing amounts of detrital minerals. In siliceous cherts opal-CT occurs as long needles that most often form dense spherulitic fiber bundles which are randomly dispersed within the rock matrix. The random orientation of fiber bundle nucleation centers does not appear to be associated with any obvious nucleation site, unlike the length-slow opal-CT fibers known as lussatite. Opal-CT needles produce optical diffractogram patterns that are compatible with tridymite and crystobalite. Streaking in the diffraction pattern of individual needles is attributed to a high density of planar defects parallel to their length. Planar defects are not as abundant in opal-CT needles formed in detrital-rich rocks suggesting the rapid growth of opal-CT in highly siliceous environments results in a greater proportion of stacking disorder in the needles. HRTEM provides a method for investigating the development of the microstructure of opal-CT during diagenesis.

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

    NASA Astrophysics Data System (ADS)

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

    2014-12-01

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

  1. 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.

  2. 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.

  3. 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.

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

    NASA Astrophysics Data System (ADS)

    Mishra, Ashutosh; Ninama, Samrath; Mishra, Niyati

    2012-06-01

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

  5. 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.

  6. Nanosecond magnetization reversal in nanocrystalline magnetic films

    NASA Astrophysics Data System (ADS)

    Rahman, I. Z.; Gandhi, A. A.; Khaddem-Mousavi, M. V.; Lynch, T. F.; Rahman, M. A.

    2007-03-01

    This paper reports on the investigation of dynamic magnetization reversal process in electrodeposited nanocrystalline Ni and Ni80Fe20 films by employing nanosecond magnetic pulse technique. The surface morphology has been investigated using SEM, EDAX, XRD and AFM analyses and static magnetic properties of the films are characterized by vibrating sample magnetometer (VSM). Two different techniques are designed and employed to study the nanosecond magnetization reversal process in nanocrystalline thin films: Magneto-Optical Kerr Effect (MOKE) and nanosecond pulsed field magnetometer. Results of dynamical behavior as a function of several variables such as magnitude of applied bias magnetic field, amplitude and width of the pulsed magnetic field are analyzed in detail using both techniques. A computer simulation package called Object Oriented Micro-Magnetic Framework (OOMMF) has been used to simulate the magnetic domain patterns of the samples.

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

    PubMed Central

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

    2016-01-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2016-08-01

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

  9. 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.

  10. 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.

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

    SciTech Connect

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

    1989-04-01

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

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

    SciTech Connect

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

    2007-02-02

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

  13. 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.

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

    NASA Astrophysics Data System (ADS)

    Ostrooumov, Mikhail

    2009-08-01

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

  15. 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.

  16. 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.

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

    PubMed

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

    2012-07-01

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

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

    PubMed

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

    2014-12-01

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

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

    PubMed

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

    2013-12-01

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

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

    PubMed

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

    2014-09-01

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

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

    PubMed

    Ostrooumov, Mikhail; Hernández-Bernal, Maria del Sol

    2011-12-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2013-06-01

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

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

    PubMed

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

    2012-07-01

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

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

    SciTech Connect

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

    2005-12-15

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

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

    SciTech Connect

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

    2008-12-12

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

  6. 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.

  7. 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.

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

    PubMed

    Zbik, Marek S; Frost, Ray L

    2010-06-15

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

  9. 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

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

    PubMed

    Ostrooumov, Mikhail

    2007-12-15

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

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

    PubMed

    Ostrooumov, Mikhail

    2007-12-15

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

  13. [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.

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

    NASA Astrophysics Data System (ADS)

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

    2014-11-01

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

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

    NASA 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

  16. 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

  17. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2012-05-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2014-02-01

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

  20. 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

  1. 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.

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

    PubMed

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

    2007-12-01

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

  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.

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

    SciTech Connect

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

    2001-06-19

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

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

    NASA Astrophysics Data System (ADS)

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

    2013-04-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2012-11-01

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

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

    NASA Astrophysics Data System (ADS)

    Allain, Monica; Heuser, Brent; Durfee, Curtis

    2001-03-01

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

  8. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2008-07-01

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

  10. 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.

  11. 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

  12. 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.

  13. 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.

  14. 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.

  15. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2011-07-01

    CuInSe2 (CIS nanostructured) thin films were prepared by ion exchange method at room temperature on ITO coated glass substrates in an alkaline medium. The as prepared thin films were irradiated by 120 MeV Au9+ swift heavy ion (SHI) at 5×1011 and 5×1012 ions/cm2 fluence respectively. To study the effect of irradiation, the pristine and irradiated nanostructured thin films were characterized by X ray Diffraction (XRD) and analyzed the improvement in crystalline quality and crystallite size. The observed structural modifications discussed considering the high electronic energy deposition by 120 MeV gold heavy (Au9+) ions in CuInSe2 thin films.

  17. 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.

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

    NASA Technical Reports Server (NTRS)

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

    2004-01-01

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

  19. 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.

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

    SciTech Connect

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

    2011-07-15

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

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

    SciTech Connect

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

    2015-06-24

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

  2. 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.

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

    PubMed

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

    2012-07-01

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

  4. 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

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

    NASA Astrophysics Data System (ADS)

    Xu, Hongwu; Guo, Xiaofeng; Bai, Jianming

    2016-09-01

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

  6. 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.

  7. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2016-07-01

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

  9. 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

  10. 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

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

    NASA Astrophysics Data System (ADS)

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

    2013-04-01

    The CheMin instrument on the Mars Science Laboratory (MSL) rover Curiosity uses a Co tube source and a CCD detector to acquire mineralogy from diffracted primary X-rays and chemical information from fluoresced X-rays. CheMin has been operating at the MSL Gale Crater field site since August 5, 2012 and has provided the first X-ray diffraction (XRD) analyses in situ on a body beyond Earth. Data from the first sample collected, the Rocknest eolian soil, identify a basaltic mineral suite, predominantly plagioclase (~An50), forsteritic olivine (~Fo58), augite and pigeonite, consistent with expectation that detrital grains on Mars would reflect widespread basaltic sources. Minor phases (each <2 wt% of the crystalline component) include sanidine, magnetite, quartz, anhydrite, hematite and ilmenite. Significantly, about a third of the sample is amorphous or poorly ordered in XRD. This amorphous component is attested to by a broad rise in background centered at ~27° 2θ (Co Kα) and may include volcanic glass, impact glass, and poorly crystalline phases including iron oxyhydroxides; a rise at lower 2θ may indicate allophane or hisingerite. Constraints from phase chemistry of the crystalline components, compared with a Rocknest bulk composition from the APXS instrument on Curiosity, indicate that in sum the amorphous or poorly crystalline components are relatively Si, Al, Mg-poor and enriched in Ti, Cr, Fe, K, P, S, and Cl. All of the identified crystalline phases are volatile-free; H2O, SO2 and CO2 volatile releases from a split of this sample analyzed by the SAM instrument on Curiosity are associated with the amorphous or poorly ordered materials. The Rocknest eolian soil may be a mixture of local detritus, mostly crystalline, with a regional or global set of dominantly amorphous or poorly ordered components. The Rocknest sample was targeted by MSL for "first time analysis" to demonstrate that a loose deposit could be scooped, sieved to <150 µm, and delivered to

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

    SciTech Connect

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

    2012-07-01

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

  13. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2016-09-01

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

  15. 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.

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

    NASA Technical Reports Server (NTRS)

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

    2006-01-01

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

  17. 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.

  18. 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.

  19. 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.

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

    PubMed

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

    2012-12-01

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

  1. 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.

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

    SciTech Connect

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

    2013-07-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2013-03-01

    We present the results of x-ray diffraction and x-ray absorption spectroscopy experiments in CuAlO2 under high pressure. We discuss the polarization dependence of the x-ray absorption near-edge structure at the Cu K-edge. XRD under high pressure evidences anisotropic compression, the a-axis being more compressible than the c-axis. EXAFS yields the copper-oxygen bond length, from which the only internal parameter of the delafossite structure is deduced. The combination of anisotropic compression and the internal parameter decrease results in a regularization of the AlO6 octahedra. The anisotropic compression is related to the chemical trends observed in the lattice parameters when Al is substituted by other trivalent cations. Both experiments evidence the existence of an irreversible phase transition that clearly manifests at 35 ± 2 GPa. The structure of the high-pressure polymorph could not be determined, but it implies a change of the Cu environment, which remains anisotropic. Precursor effects are observed from the lowest pressures, which are possibly related to crystal breaking at a submicroscopic scale with partial reorientation of the crystallites.

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

    PubMed

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

    2013-03-20

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

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

    NASA Astrophysics Data System (ADS)

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

    1993-12-01

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

  6. 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

  7. 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.

  8. 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.

  9. 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.

  10. 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

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

    NASA Astrophysics Data System (ADS)

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

    2010-12-01

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

  12. 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.

  13. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2013-07-01

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

  15. 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.

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

    PubMed

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

    2013-05-01

    Structural characterizations using XRD and (13)C NMR spectroscopy of two rodlike mesogens consisting of (i) three phenyl ring core with a polar cyano terminal and (ii) four phenyl ring core with flexible dodecyl terminal chain are presented. The three-ring-core mesogen with cyano terminal exhibits enantiotropic smectic A phase while the four-ring mesogen reveals polymesomorphism and shows enantiotropic nematic, smectic C, and tilted hexatic phases. The molecular organization in the three-ring mesogen is found to be partial bilayer smectic Ad type, and the interdigitation of the molecules in the neighboring layers is attributed to the presence of the polar terminal group. For the four-ring mesogen, the XRD results confirm the existence of the smectic C and the tilted hexatic mesophases. A thermal variation of the layer spacing across the smectic C phase followed by a discrete jump at the transition to the tilted hexatic phase is also observed. The tilt angles have been estimated to be about 45° in the smectic C phase and about 40° in tilted hexatic phase. (13)C NMR results indicate that in the mesophase the molecules are aligned parallel to the magnetic field. From the (13)C-(1)H dipolar couplings determined from the 2D experiments, the overall order parameter for the three-ring mesogen in its smectic A phase has been estimated to be 0.72 while values ranging from 0.88 to 0.44 have been obtained for the four-ring mesogen as it passes from the tilted hexatic to the nematic phase. The orientations of the different rings of the core unit with respect to each other and also with respect to the long axis of the molecule have also been obtained. PMID:23627902

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

    NASA Astrophysics Data System (ADS)

    Vashista, M.; Paul, S.

    2012-11-01

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

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

    PubMed

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

    2002-01-01

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

  19. 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.

  20. Preparation and characterization of magnetic nanoparticles with chitosan coating

    NASA Astrophysics Data System (ADS)

    Dung, Doan Thi Kim; Hoang Hai, Tran; Phuc, Le Hong; Long, Bui Duc; Khanh Vinh, Le; Nha Truc, Phan

    2009-09-01

    Magnetic chitosan nanoparticles were prepared by the suspension cross-linking technique for use in the application of magnetic carrier technology. The Fe3O4 magnetic nanoparticles were synthesized by co-precipitation of FeCl2 and FeCl3 solution in base medium for using in the preparation of the magnetic chitosan. The morphological and magnetic properties of the magnetic nanoparticles were characterized by different techniques (TEM, XRD, VSM, FTIR, etc.). The magnetic properties of chitosan - magnetic nanoparticles were analyzed by VSM, and MS around 15 emu/g.

  1. 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.

  2. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2015-11-01

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

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

    USGS Publications Warehouse

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

    2006-01-01

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

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

    PubMed

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

    2014-06-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2015-12-01

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

  7. 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.

  8. 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

  9. 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

  10. 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

  11. [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

  12. [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

  13. 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.

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

    PubMed

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

    2014-08-01

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

  15. 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.

  16. 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...

  17. 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.

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

    PubMed

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

    2011-08-28

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

  19. 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

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

    NASA Astrophysics Data System (ADS)

    Qin, Huibin; Yu, Hong; Chen, Yunxang

    2000-05-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2014-09-01

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

  2. 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.

  3. Crystallographic and magnetic order analysis of a banded limonite

    NASA Astrophysics Data System (ADS)

    Rice, D. A.; Cashion, J. D.; Bocquet, S.

    1994-12-01

    Mössbauer and XRD studies of the light and dark brown parts of a banded limonite showed the presence of kaolinite in the light brown regions. Relaxation behaviour was very well described by a recently proposed model based on magnetic ordering of clusters. The difference in relaxation behaviour of the samples was attributed to different concentrations of non-magnetic impurities.

  4. Identification of magnetic properties of few nm sized FePt crystalline particles by characterizing the intrinsic atom order using aberration corrected S/TEM.

    PubMed

    Biskupek, Johannes; Jinschek, Joerg R; Wiedwald, Ulf; Bendele, Markus; Han, Luyang; Ziemann, Paul; Kaiser, Ute

    2010-06-01

    Hard-magnetic nanomaterials like nanoparticles of FePt are of great interest because of their promising potential for data storage applications. The magnetic properties of FePt structures strongly differ whether the crystal phases are face centered cubic (fcc) or face centered tetragonal (fct). We evaluated aberration corrected HRTEM, electron diffraction and aberration corrected HAADF-STEM as methods to measure the chemical degree of order S that describes the ordering of Pt and Fe atoms within the crystals unit cells. S/TEM experiments are accompanied by image calculations. The findings are compared with results obtained from X-ray diffraction on a FePt film. Our results show that STEM is a reasonable fast approach over HRTEM and electron diffraction to locally determine the chemical degree of order S.

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

    NASA Astrophysics Data System (ADS)

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

    1998-12-01

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

  6. 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

  7. 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

  8. 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

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

    NASA Astrophysics Data System (ADS)

    Harikrishnan, V.; Ezhil Vizhi, R.

    2016-11-01

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

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

    NASA Astrophysics Data System (ADS)

    Habibi, Neda

    2014-10-01

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

  11. 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

  12. 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.

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

    SciTech Connect

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

    2013-09-01

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

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

    SciTech Connect

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

    2008-12-01

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

  15. 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.

  16. 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.

  17. Magnetic measurements on α-CS2U4O12

    NASA Astrophysics Data System (ADS)

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

    2014-04-01

    Magnetic and XRD measurements on α-CS2U4O12 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.

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

    NASA Astrophysics Data System (ADS)

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

    2007-07-01

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

  19. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2009-04-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2009-12-01

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

  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. 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.

  4. 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.

  5. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2013-04-01

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

  7. 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.

  8. 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.

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

    PubMed

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

    2016-01-01

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

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

    PubMed

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

    2009-01-01

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

  11. 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.

  12. 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.

  13. Chemical diffusion: Another factor affecting the magnetoresistance ratio in Ta/CoFeB/MgO/CoFeB/Ta magnetic tunnel junction

    SciTech Connect

    Yang, Y.; Wang, W. X.; Yao, Y.; Liu, H. F.; Han, X. F.; Yu, R. C.; Naganuma, H.; Sakul, T. S.

    2012-07-02

    This letter investigates the microstructure and mean inner potential (MIP) profile of Ta/CoFeB/MgO/CoFeB/Ta magnetic tunnel junctions (MTJs) by high resolution transmission electron microscopy (HRTEM) and electron holography, respectively. The inconspicuous crystallization of MgO barrier is confirmed by HRTEM in the post-annealed sample at 250 Degree-Sign C. An obvious MIP difference is displayed in the Ta layers between the top and bottom of the MTJ, and elemental content difference of them is confirmed by energy dispersive spectroscopy. These results imply that the chemical diffusion can also give rise to a lower tunnel magnetoresistance ratio besides the inconspicuous crystallization of MgO barrier.

  14. Magnetic Spinner

    NASA Astrophysics Data System (ADS)

    Ouseph, P. J.

    2006-12-01

    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 above two triangular magnets fixed to the base. The magnetic repulsive force experienced by the circular magnets is independent of their orientation; therefore, the holder of these magnets can be rotated without affecting its stability. The holder with the circular magnets can be oscillated up and down as a horizontally suspended physical pendulum.

  15. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2005-02-01

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

  17. 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)

  18. 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

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

    SciTech Connect

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

    2015-06-24

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

  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 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.

  2. 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.

  3. Synthesis and Characterization of Magnetic Metal-encapsulated Multi-walled Carbon Nanobeads

    PubMed Central

    2008-01-01

    A novel, cost-effective, easy and single-step process for the synthesis of large quantities of magnetic metal-encapsulated multi-walled carbon nanobeads (MWNB) and multi-walled carbon nanotubes (MWNT) using catalytic chemical vapour deposition of methane over Mischmetal-based AB3alloy hydride catalyst is presented. The growth mechanism of metal-encapsulated MWNB and MWNT has been discussed based on the catalytically controlled root-growth mode. These carbon nanostructures have been characterized using scanning electron microscopy (SEM), transmission electron microscopy (TEM and HRTEM), energy dispersive analysis of X-ray (EDAX) and thermogravimetric analysis (TGA). Magnetic properties of metal-filled nanobeads have been studied using PAR vibrating sample magnetometer up to a magnetic field of 10 kOe, and the results have been compared with those of metal-filled MWNT.

  4. 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.

  5. 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.

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

    PubMed

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

    2016-06-01

    Spinel Mn(x)Zn(1-x)Fe2O4 (0.0 ≤ x ≤ 1.0) nanoparticles (NPs) were successfully synthesized by a facile one-pot microwave combustion method using urea as the fuel. The formation of single phase cubic spinel structure was confirmed by powder X-ray diffraction (XRD), Rietveld analysis and Fourier transform infrared (FT-IR) spectroscopy and the calculated average crystallite size is in the range of 37.57 nm to 25.43 nm. The high resolution scanning electron microscopy (HR-SEM) and high resolution transmission electron microscopy (HR-TEM) results indicated that the as-prepared spinel Mn(x)Zn(1-x)Fe2O4 NPs showed high crystallinity and uniform size distribution with particles-like morphologies. The energy dispersive X-ray (EDX) analysis was confirmed the elemental composition and purity of the samples. The estimated band gap energy from UV-Visible diffuse reflectance spectroscopy (UV-Vis. DRS) is about 1.88 eV to 2.35 eV. The broad visible emission band is observed in the entire photoluminescence (PL) spectroscopy for all compositions. The variation of magnetization (M(s)) value of the samples was studied by vibrating sample magnetometer (VSM) and the lower compositions (x = 0.0, 0.2 and 0.4) show a superparamagnetism and the higher composition (x = 0.6, 0.8 and 1.0) show a ferromagnetic behavior with hysteresis and that the M(s) values increased with increasing Mn2+ content to reach a maximum value of 60.99 emu/g for MnFe2O4. All composition of spinel Mn(x)Zn(1-x)Fe2O4 NPs were successfully tested as catalyst for the oxidation of benzyl alcohol into benzaldehyde, which has resulted 83.29 and 96.51% conversion efficiency of ZnFe2O4 and Mn0.6Zn0.4Fe2O4 respectively. PMID:27427654

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

    PubMed

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

    2016-06-01

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

  8. 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…

  9. 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…

  10. Defect-induced magnetism: Test of dilute magnetism in Fe-doped hexagonal BaTiO3 single crystals

    NASA Astrophysics Data System (ADS)

    Chakraborty, Tanushree; Ray, Sugata; Itoh, Mitsuru

    2011-04-01

    Single crystalline Fe-doped hexagonal BaTiO3 samples with varying oxygen content are created by specifically intended post-growth annealing treatments, in order to check the influence of defects on the unusual high temperature ferromagnetism observed in this system. The various defects have been shown to play a crucial role in dilute magnetic systems and therefore, it is important to carry out this check for the Fe-doped BaTiO3 system also, in which unusual ferromagnetism was reported even in its bulk single crystalline form. The x-ray diffraction and dielectric studies carried out here have confirmed that the Fe doping of Ti is intrinsic, while the high resolution transmission electron microscopy (HRTEM) and x-ray photoemission spectroscopy (XPS) studies proved the absence of unwanted magnetic metal clusters in the sample. The transport studies show that the oxygen concentrations could be varied substantially by the thermal treatments. Finally, magnetization measurements on the samples demonstrated that ferromagnetism is stronger in samples with higher oxygen deficiency, which could interestingly be retreated under high oxygen atmosphere and reversibly be taken back to a lower magnetic state. The vacancy-induced ferromagnetism is further confirmed by EPR measurements, which is consistent with earlier studies and, consequently, put the doped BaTiO3 in the list of true dilute magnetic oxide (DMO) systems.

  11. 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

  12. 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.

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

    NASA Astrophysics Data System (ADS)

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

    1995-02-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2016-09-01

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

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

    PubMed

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

    2016-04-28

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

  16. 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.

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

    PubMed

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

    2014-01-01

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

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

    SciTech Connect

    Chetty, Raju Mallik, Ramesh Chandra

    2014-04-24

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

  19. Synthesis of Ultralong Polyaniline Nanorods by Magnetic Nanoparticles as Templates Under External Magnetic Field.

    PubMed

    Miao, Tingting; Li, Yijing; Zhang, Dongmei

    2016-06-01

    We report the successful synthesis of ultralong polyaniline nanorods (UL-PANI-NRs) via using water-soluble magnetic Fe3O4 nanoparticles as soft templates under the assistance of external magnetic field. It was found that the concentration of Fe3O4 nanoparticles, the aniline concentration and the use of an external magnetic field significantly affect the morphology of the PANI products. The following characterizations including transmission electron microscopy (TEM), Fourier-Transform Infrared Spectroscopy (FTIR), X-ray diffraction (XRD). and thermogravimetric analysis (TGA) were conducted to investigate the electronic structure and composition of as-prepared UL-PANI-NRs. Our preliminary result indicates that complicated polymer structures (such as ultralong rods with vertical branches) may be prepared by water-soluble magnetic Fe3O4 nanoparticles as soft templates under the assistance of alternatively external magnetic fields. PMID:27427623

  20. Synthesis of Ultralong Polyaniline Nanorods by Magnetic Nanoparticles as Templates Under External Magnetic Field.

    PubMed

    Miao, Tingting; Li, Yijing; Zhang, Dongmei

    2016-06-01

    We report the successful synthesis of ultralong polyaniline nanorods (UL-PANI-NRs) via using water-soluble magnetic Fe3O4 nanoparticles as soft templates under the assistance of external magnetic field. It was found that the concentration of Fe3O4 nanoparticles, the aniline concentration and the use of an external magnetic field significantly affect the morphology of the PANI products. The following characterizations including transmission electron microscopy (TEM), Fourier-Transform Infrared Spectroscopy (FTIR), X-ray diffraction (XRD). and thermogravimetric analysis (TGA) were conducted to investigate the electronic structure and composition of as-prepared UL-PANI-NRs. Our preliminary result indicates that complicated polymer structures (such as ultralong rods with vertical branches) may be prepared by water-soluble magnetic Fe3O4 nanoparticles as soft templates under the assistance of alternatively external magnetic fields.

  1. Gamma-ray irradiation on microsized Nd-Fe-B and Sr-ferrite magnets at low temperature.

    PubMed

    Han, Young Chul; Cha, Hyun Gil; Kim, Chang Woo; Kim, Young Hwan; Ji, Eun Sun; Kang, Young Soo

    2009-07-01

    The gamma-ray irradiation on microsized Nd-Fe-B and Sr-Fe permanent magnet at low temperature and room temperature was investigated. The change of shape and magnetic properties of two kinds of magnet powder before and after irradiation at low temperature was measured. The crystal structure of each permanent magnet powders was analyzed using X-ray powder diffraction (XRD) and the size and shape were characterized by scanning electron microscope (SEM). The changed magnetic properties of magnet such as saturation magnetization (M(s)) and coercivity (H(c)) were measured by VSM.

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

    PubMed

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

    2012-01-30

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

  3. 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

  4. Preparation of iron oxide nanoparticles by laser ablation in DMF under effect of external magnetic field

    NASA Astrophysics Data System (ADS)

    Ismail, Raid A.; Sulaiman, Ghassan M.; Abdulrahman, Safa A.

    2016-05-01

    We have studied the effect of applying an external magnetic field on the characteristics of iron oxide (IO) nanoparticles (NPs) synthesized by pulsed laser ablation in dimethylformamide (DMF). The NPs synthesized with and without applying of magnetic field were characterized by Fourier transformation infrared spectroscopy (FT-IR), UV-Vis absorption, scanning electron microscope (SEM), atomic force microscope (AFM), and X-ray diffraction (XRD). SEM results confirmed that the particle size was decreased after applying magnetic field.

  5. 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.

  6. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2009-11-01

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

  8. Magnetizing of permanent magnets using HTS bulk magnets

    NASA Astrophysics Data System (ADS)

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

    2012-01-01

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

  9. Fabrication of surface magnetic nanoclusters using low energy ion implantation and electron beam annealing

    NASA Astrophysics Data System (ADS)

    Kennedy, J.; Leveneur, J.; Williams, G. V. M.; Mitchell, D. R. G.; Markwitz, A.

    2011-03-01

    Magnetic nanoclusters have novel applications as magnetic sensors, spintronic and biomedical devices, as well as applications in more traditional materials such as high-density magnetic storage media and high performance permanent magnets. We describe a new synthesis protocol which combines the advantages of ion implantation and electron beam annealing (EBA) to produce surface iron nanoclusters. We compare the structure, composition and magnetic properties of iron nanoclusters fabricated by low dose 15 keV Fe implantation into SiO2 followed by 1000 °C EBA or furnace annealing. Atomic force microscopy (AFM) and high resolution transmission electron microscopy (HRTEM) images together with superconducting quantum interference device (SQUID) magnetometry measurements show that only EBA leads to the rapid formation of surface crystalline Fe spherical nanoclusters, showing magnetic moments per Fe atom comparable to that of bulk bcc Fe and superparamagnetic properties. We propose a fabrication mechanism which includes e-beam enhanced desorption of SiO2. This method has potential for fabricating nanoscale magnetic sensors integrated in microelectronic devices.

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

    SciTech Connect

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

    2015-06-24

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

  11. 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

  12. Study of the relation between Mg content and dissolution kinetics of natural lime stone using μXRF, μXRD and μXAS

    NASA Astrophysics Data System (ADS)

    Grunwaldt, H. S.; Zimina, A.; Göttlicher, J.; Steininger, R.; Grunwaldt, J.-D.

    2016-05-01

    The dissolution parameters of calcium carbonates play a key role in agriculture as they regulate the plant nutrients uptake and buffer the pH-value of the soil. The combination of μXRF, μXAS and μXRD mapping in the hard X-ray regime for the examination of both short- and long range order in natural limestones revealed that their dissolution properties depend both on the crystallinity of the mineral phases and their composition. The results particularly show that in many cases the presence of magnesium inhibits dissolution of the phases.

  13. 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.

  14. 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.

  15. 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.

  16. 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.

  17. Irradiation effects in 6H-SiC induced by neutron and heavy ions: Raman spectroscopy and high-resolution XRD analysis

    NASA Astrophysics Data System (ADS)

    Chen, Xiaofei; Zhou, Wei; Feng, Qijie; Zheng, Jian; Liu, Xiankun; Tang, Bin; Li, Jiangbo; Xue, Jianming; Peng, Shuming

    2016-09-01

    Irradiation effects of neutron and 3 MeV C+, Si+ in 6H-SiC were investigated by Raman spectroscopy and high-resolution XRD. The total disorder values of neutron irradiated SiC agree well with that of samples irradiated by ions at the same doses respectively. On the other hand, high-resolution XRD results shows that the lattice strain rate caused by neutron irradiation is 6.8%/dpa, while it is only 2.6%/dpa and 4.2%/dpa for Si+ and C+ irradiations respectively. Our results illustrate that the total disorder in neutron irradiated SiC can be accurately simulated by MeV Si+ or C+ irradiations at the same dose, but for the lattice strain and strain-related properties like surface hardness, the depth profile of irradiation damages induced by energetic ions must be considered. This research will contribute to a better understanding of the difference in irradiation effects between neutron and heavy ions.

  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. Characterization of wet precipitation by X-ray diffraction (XRD) and scanning electron microscopy (SEM) in the metropolitan area of Porto Alegre, Brazil.

    PubMed

    Migliavacca, Daniela Montanari; Teixeira, Elba Calesso; Gervasoni, Fernanda; Conceição, Rommulo Vieira; Rodriguez, Maria Teresa Raya

    2009-11-15

    The purpose of this study is to assess the composition of wet precipitation in three sites of the metropolitan area of Porto Alegre. Besides the variables usually considered, such as pH, conductivity, major ions (Cl(-), NO(3)(-), F(-), SO(4)(2-), Na(+), K(+), Mg(2+), NH(4)(+) and Ca(2+)) and metallic elements (Cd, Co, Cr, Cu, Fe, Mn and Ni), the suspended matter was examined by X-ray diffraction (XRD) and scanning electron microscopy (SEM), with energy dispersive system (EDS), for better identification of possible anthropogenic material in this wet precipitation. Results showed an alkaline pH in the samples analyzed and higher concentrations for Na(+), Cl(-) and SO(4)(2-). The acidification and neutralization potential between anions (SO(4)(2-)+NO(3)(-)) and cations (Ca(2+)+Mg(2+)+K(+)+NH(4)(+)) showed a good correlation (0.922). The metallic elements with highest values were Zn, Fe and Mn. Results of XRD identified the presence of some minerals such as quartz, feldspar, mica, clay, carbonates and sulfates. In samples analyzed with SEM, we detected pyroxene, biotite, amphibole and oxides. Cluster analysis (CA) was applied to the data matrix to identify potential pollution sources of metals (natural or anthropogenic) and the association with minerals found in the analysis of SEM.

  20. 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.

  1. 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.

  2. 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.

  3. 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.

  4. 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.

  5. 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

  6. 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.

  7. Polymer nanocomposites exhibiting magnetically tunable microwave properties

    NASA Astrophysics Data System (ADS)

    Stojak, K.; Pal, S.; Srikanth, H.; Morales, C.; Dewdney, J.; Weller, T.; Wang, J.

    2011-04-01

    Polymer nanocomposites (PNCs) have been synthesized using Rogers polymer and CoFe2O4 nanoparticles (CFO NPs). X-ray diffraction (XRD) confirms the inverse spinel crystal structure of CFO NPs and transmission electron microscopy (TEM) images show the uniform dispersion of nanoparticles (10 nm ± 1) into the polymer matrix. Magnetic measurements indicate superparamagnetic response near room temperature for all PNCs. A blocking temperature TB ~ 298 K was observed and does not vary for different loading fractions of CFO NPs for the PNCs. The saturation magnetization (Ms) was found to be 11 emu g - 1 for 30 wt% CFO, increasing to 32 emu g - 1 for the 80 wt% CFO loaded PNC. A large value of coercivity (Hc = 19 kOe) is also observed at 10 K and is not affected by varying CFO loading. Microwave measurements show significant absorption in the 80 wt% CFO loading PNC and the quality factor shows a strong enhancement with applied magnetic field.

  8. 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.

  9. 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.

  10. 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.

  11. 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.

  12. Annealing effects on the microstructure and magnetic domain structures of duplex stainless steel studied by in situ technique

    NASA Astrophysics Data System (ADS)

    Guo, L. Q.; Zhao, X. M.; Li, M.; Zhang, W. J.; Bai, Y.; Qiao, L. J.

    2012-10-01

    The effects of annealing temperature on the microstructure and the magnetic domain structures of duplex stainless steel 2507 were investigated by the magnetic force microscopy (MFM), X-ray diffraction (XRD), and electron backscattered diffraction (EBSD). The MFM and XRD results indicated that the volume fraction of ferrite phase increased with increasing annealing temperature, but the lattice constants kept constant. Moreover, with the rise of annealing temperature, the magnetic domain structure in the ferrite phase varied gradually, where the magnetic domain became thinner and the distribution turned more homogeneous. These results gave a direct evidence for the changes of microstructure and magnetic domain structure induced by the annealing treatment. EBSD analysis showed that the orientation of ferrite grains changed after annealing treatments, which coincided with the changes of the microstructure and the magnetic domain structures.

  13. Raman-Mössbauer-XRD studies of selected samples from "Los Azulejos" outcrop: A possible analogue for assessing the alteration processes on Mars

    NASA Astrophysics Data System (ADS)

    Lalla, E. A.; Sanz-Arranz, A.; Lopez-Reyes, G.; Sansano, A.; Medina, J.; Schmanke, D.; Klingelhoefer, G.; Rodríguez-Losada, J. A.; Martínez-Frías, J.; Rull, F.

    2016-06-01

    The outcrop of "Los Azulejos" is visible at the interior of the Cañadas Caldera in Tenerife Island (Spain). It exhibits a great variety of alteration processes that could be considered as terrestrial analogue for several geological processes on Mars. This outcrop is particularly interesting due to the content of clays, zeolite, iron oxides, and sulfates corresponding to a hydrothermal alteration catalogued as "Azulejos" type alteration. A detailed analysis by portable and laboratory Raman systems as well as other different techniques such as X-ray diffraction (XRD) and Mössbauer spectroscopy has been carried out (using twin-instruments from Martian lander missions: Mössbauer spectrometer MIMOS-II from the NASA-MER mission of 2001 and the XRD diffractometer from the NASA-MSL Curiosity mission of 2012). The mineral identification presents the following mineral species: magnetite, goethite, hematite, anatase, rutile, quartz, gregoryite, sulfate (thenardite and hexahydrite), diopside, feldspar, analcime, kaolinite and muscovite. Moreover, the in-situ Raman and Micro-Raman measurements have been performed in order to compare the capabilities of the portable system specially focused for the next ESA Exo-Mars mission. The mineral detection confirms the sub-aerial alteration on the surface and the hydrothermal processes by the volcanic fluid circulations in the fresh part. Therefore, the secondary more abundant mineralization acts as the color agent of the rocks. Thus, the zeolite-illite group is the responsible for the bluish coloration, as well as the feldspars and carbonates for the whitish and the iron oxide for the redish parts. The XRD system was capable to detect a minor proportion of pyroxene, which is not visible by Raman and Mössbauer spectroscopy due to the "Azulejos" alteration of the parent material on the outcrop. On the other hand, Mössbauer spectroscopy was capable of detecting different types of iron-oxides (Fe3+/2+-oxide phases). These analyses

  14. 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.

  15. 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.

  16. Electroplating hard magnetic SmCo for magnetic microactuator applications

    NASA Astrophysics Data System (ADS)

    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 Al2O3 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 °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 Hci 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.

  17. Magnetic Recording.

    ERIC Educational Resources Information Center

    Lowman, Charles E.

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

  18. Magnetic shielding

    DOEpatents

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

    1985-02-12

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

  19. A new approach in quantitative in-situ XRD of cement pastes: Correlation of heat flow curves with early hydration reactions

    SciTech Connect

    Hesse, Christoph; Goetz-Neunhoeffer, Friedlinde; Neubauer, Juergen

    2011-01-15

    XRD measurements of the hydration of synthetical cement (SyCem) were used to calculate the resulting heat flow from changes in the phase content. Calculations were performed by application of thermodynamic data. The comparison with data recorded from heat flow calorimetry was in good agreement with the calculated heat flow. The initial maximum of heat flow mainly is caused by the aluminate reaction. During the entire main period the silicate reaction dominates hydration with a high and long first maximum of heat flow. The second but less intense heat flow maximum - only visible as a shoulder in most of the technical cements - can be attributed to an acceleration of the aluminate reaction with the enhanced dissolution of C{sub 3}A and the final formation of ettringite. Moreover, the investigation showed that the dissolution process of C{sub 3}A is directly controlled by the availability of the calcium sulfate phases.

  20. Incorporation of Co(II) in dealuminated BEA zeolite at lattice tetrahedral sites evidenced by XRD, FTIR, diffuse reflectance UV-Vis, EPR, and TPR.

    PubMed

    Dzwigaj, S; Che, M

    2006-06-29

    A CoSiBEA zeolite is prepared by a two-step postsynthesis method that consists of first creating vacant T-sites with associated silanol groups by dealumination of TEABEA zeolite with nitric acid and then impregnating the resulting SiBEA zeolite with an aqueous solution of Co(NO3)2. The incorporation of Co into lattice sites of SiBEA is evidenced by XRD. The consumption of OH groups is monitored by FTIR. The presence of Co in its II oxidation state and in tetrahedral coordination is evidenced by diffuse reflectance UV-vis and EPR spectroscopy. The very high reduction temperature (1120 K) of cobalt in CoSiBEA zeolite determined by TPR confirms that Co interacts strongly with the zeolite support, consistent with lattice tetrahedral (T(d)) coordination.

  1. 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).

  2. 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.

  3. Free volume in ionic liquids: a connection of experimentally accessible observables from PALS and PVT experiments with the molecular structure from XRD data.

    PubMed

    Beichel, Witali; Yu, Yang; Dlubek, Günter; Krause-Rehberg, Reinhard; Pionteck, Jürgen; Pfefferkorn, Dirk; Bulut, Safak; Bejan, Dana; Friedrich, Christian; Krossing, Ingo

    2013-06-14

    In the current work, free volume concepts, primarily applied to glass formers in the literature, were transferred to ionic liquids (ILs). A series of 1-butyl-3-methylimidazolium ([C4MIM](+)) based ILs was investigated by Positron Annihilation Lifetime Spectroscopy (PALS). The phase transition and dynamic properties of the ILs [C4MIM][X] with [X](-) = [Cl](-), [BF4](-), [PF6](-), [OTf](-), [NTf2](-) and [B(hfip)4](-) were reported recently (Yu et al., Phys. Chem. Chem. Phys., 2012, 14, 6856-6868). In this subsequent work, attention was paid to the connection of the free volume from PALS (here the mean hole volume, ) with the molecular structure, represented by volumes derived from X-ray diffraction (XRD) data. These were the scaled molecular volume Vm,scaled and the van der Waals volume V(vdw). Linear correlations of at the "knee" temperature ((T(k))) with V(m,scaled) and V(vdw) gave good results for the [C4MIM](+) series. Further relationships between volumes from XRD data with the occupied volume Vocc determined from PALS/PVT (Pressure Volume Temperature) measurements and from Sanchez-Lacombe Equation of State (SL-EOS) fits were elaborated (V(occ)(SL-EOS) ≈ 1.63 V(vdw), R(2) = 0.981 and V(occ)(SL-EOS) ≈ 1.12 V(m,scaled), R(2) = 0.980). Finally, the usability of V(m,scaled) was justified in terms of the Cohen-Turnbull (CT) free volume theory. Empirical CT type plots of viscosity and electrical conductivity showed a systematic increase in the critical free volume with molecular size. Such correlations allow descriptions of IL properties with the easily accessible quantity V(m,scaled) within the context of the free volume.

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

    NASA Astrophysics Data System (ADS)

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

    2016-10-01

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

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

    SciTech Connect

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

    2008-01-01

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

  6. The presence of mercury selenide in various tissues of the striped dolphin: evidence from μ-XRF-XRD and XAFS analyses.

    PubMed

    Nakazawa, Emiko; Ikemoto, Tokutaka; Hokura, Akiko; Terada, Yasuko; Kunito, Takashi; Tanabe, Shinsuke; Nakai, Izumi

    2011-07-01

    Marine mammals accumulate mercury in their tissues at high concentration and detoxify by forming mercury selenide (HgSe, tiemannite) mainly in the liver. We investigated the possibility of formation of HgSe in various tissues (liver, kidney, lung, spleen, pancreas, muscle and brain) other than the liver of the striped dolphin (Stenella coeruleoalba). We applied a combination method of micro-X-ray fluorescence (μ-XRF) imaging and micro-X-ray diffraction (μ-XRD) using a synchrotron radiation X-ray microbeam to analyze the tissue samples directly with minimal sample preparation. By this method, many accumulation points for Hg and Se on a micron scale were found in thin sections of the spleen and liver tissue and consequently, the XRF spectra and the XRD pattern of the hot spots confirmed the presence of tiemannite, HgSe. On the other hand, the insoluble fractions after enzyme digestion of the nuclear and mitochondrial fractions of all tissues were subjected to X-ray absorption fine structure (XAFS) analysis. XAFS analysis confirmed the presence of HgSe in all the tissues examined (liver, kidney, lung, spleen, pancreas, muscle and brain) of the striped dolphin. The presence of HgSe in all the tissues examined suggests that Se would be involved in the detoxification process of Hg in various tissues other than the liver. This contribution seems to be large especially in the liver and spleen but relatively small in the kidney, pancreas and brain, because the proportion of insoluble fraction containing HgSe was lower in these tissues (25 to 46%). This is the first report on the presence of tiemannite HgSe in various tissues of marine mammals. PMID:21468440

  7. HT-XRD study of synthetic ferrian magnesian spodumene: the effect of site dimension on the P21/c-->C2/c phase transition

    NASA Astrophysics Data System (ADS)

    Cámara, F.; Iezzi, G.; Oberti, R.

    Ferrian magnesian spodumene was synthesized in the MLFSH system at P=0.4 GPa, T=700 °C, fO2=NNO+2.3. The space group at room T is P21/c [a=9.638(3) Å, b=8.709(2) Å, c=5.258(2) Å, β=109.83(3)∘, V=415.2 Å3]. The structure is topologically equivalent to that of ferrian spodumene, LiFeSi2O6, and has two symmetrically independent tetrahedral chains, A and B, and two independent octahedral sites, M1 and M2. The crystal-chemical composition was determined combining EMP, SIMS and single-crystal XRD analysis, yielding M2(Li0.85Mg0.09Fe2+0.06) M1(Fe3+0.85Mg0.15)Si2O6. Li is ordered at the M2 site and Fe3+ is ordered at the M1 site, whereas Mg (and Fe2+) distribute over both octahedral sites. Structure refinements done at different temperatures (25, 70, 95, 125, 150 and 200 °C) allowed characterization of a reversible displacive P21/c-->C2/c transition at 106 °C. Previous HT-XRD studies of Li-clinopyroxenes had shown that the transition temperature is inversely related to the size of the M1 cation. For the crystal of this work, the aggregate ionic radius at M1 is longer than that of ferrian spodumene, for which the transition temperature is -44 °C. The higher transition temperature observed can only be explained on the basis of the shorter aggregate radius at the M2 site (due to the presence of Mg substituting after Li), in keeping with the results obtained for ferromagnesian P21/c pyroxenes. The effects of all the chemical substitutions must be considered when modelling transition temperatures and thermodynamic behaviour in clinopyroxenes.

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

    NASA Astrophysics Data System (ADS)

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

    2016-11-01

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

  9. Preparation and Properties of ε-Fe3N-Based Magnetic Fluid

    PubMed Central

    2008-01-01

    In this work, ε-Fe3N nanoparticles and ε-Fe3N-based magnetic fluid were synthesized by chemical reaction of iron carbonyl and ammonia gas. The size of ε-Fe3N nanoparticles was tested by TEM and XRD. Stable ε-Fe3N-based magnetic fluid was prepared by controlling the proper ratio of carrier liquid and surfactant. The saturation magnetization of stable ε-Fe3N-based magnetic fluid was calculated according to the volume fraction of the particles in the fluid. The result shows that both the calculated and measured magnetizations increase by increasing the particle concentration. With the increasing concentration of the ε-Fe3N particles, the measured value of the magnetic fluid magnetization gradually departs from the calculated magnetization, which was caused by agglomeration affects due to large volume fraction and large particle size.

  10. Structural and magnetic properties of nano-crystalline Ni-Zn ferrites synthesized using egg-white precursor

    NASA Astrophysics Data System (ADS)

    Gabal, M. A.; El-Shishtawy, Reda M.; Al Angari, Y. M.

    2012-07-01

    Nano-crystalline nickel-zinc ferrites of different compositions; Ni1-xZnxFe2O4 (x=0.0-1.0) were prepared by a precursor method involving egg-white and metal nitrates. An appropriate mechanism for the egg-white-metal complexation was suggested. Differential thermal analysis-thermogravimetry, X-ray diffraction (XRD), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR), vibrating sample magnetometer and AC-magnetic susceptibility measurements were carried out to investigate chemical, structural and magnetic aspects of Ni-Zn ferrites. XRD confirmed the formation of spinel cubic structure. The average crystallite size was calculated using line broadening in XRD patterns. Structural parameters like lattice constant, X-ray density, bond lengths and inter-cationic distance were determined from XRD data. TEM showed agglomerated particles with average size agreed well with that estimated using XRD. FT-IR spectra confirm the formation of spinel structure and further lends support to the proposed cation distribution. Zn-content was found to have a significant influence on the magnetic properties of the system. The changes in the magnetic properties can be attributed to the influence of the cationic stoichiometry and their occupancy in the specific sites.

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

    SciTech Connect

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

    2008-08-04

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

  12. Magnetic Bearing

    NASA Technical Reports Server (NTRS)

    1996-01-01

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

  13. 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.

  14. Hollow mesoporous carbon spheres with magnetic cores and their performance as separable bilirubin adsorbents.

    PubMed

    Guo, Limin; Cui, Xiangzhi; Li, Yongsheng; He, Qianjun; Zhang, Lingxia; Bu, Wenbo; Shi, Jianlin

    2009-09-01

    Hollow mesoporous carbon spheres with magnetic cores are directly replicated from hollow mesoporous aluminosilicate spheres with hematite cores by a simple incipient-wetness impregnation technique. The amount of magnetic cores and the saturation magnetization value can be easily tuned by changing the concentration of iron nitrate solution used in the synthesis procedure. As-prepared hollow mesoporous carbon spheres with magnetic cores are used as separable bilirubin adsorbents and show very good adsorptive properties. The characteristics of as-prepared composites are examined by XRD, N(2) sorption, TEM, vibrating-sample magnetometry, and UV/Vis spectroscopy. PMID:19582733

  15. Synthesis and magnetic study of carbon coated iron oxide nanoparticles by laser ablation in solution

    NASA Astrophysics Data System (ADS)

    Prajapat, C. L.; Sharma, P.; Gonal, M. R.; Vatsa, R. K.; Singh, M. R.; Ravikumar, G.

    2016-05-01

    Magnetic Iron oxides nanoparticles (NPs) were prepared by Laser Ablation in Solution method. Formation and average size of iron oxide NPs (~8 nm) is confirmed by XRD pattern and magnetization studies. Detailed magnetic studies have been carried out using SQUID magnetometer. The saturation magnetization for the iron oxide NPs was found to be 60.07 emu/g. Below the blocking temperature of 150 K the hysteresis loop shows ferromagnetic nature, whereas it shows superparamagnetic behavior at 300 K, for the synthesized NPs.

  16. 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

  17. Magnetic Reconnection

    NASA Video Gallery

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

  18. 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)

  19. 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.

  20. 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)

  1. 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.

  2. 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.

  3. 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

  4. 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

  5. MAGNETIC IMAGING OF NANOCOMPOSITE MAGNETS

    SciTech Connect

    VOLKOV,V.V.ZHU,Y.

    2003-08-03

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

  6. Induced magnetic anisotropy in Si-free nanocrystalline soft magnetic materials: A transmission x-ray diffraction study

    NASA Astrophysics Data System (ADS)

    Parsons, R.; Yanai, T.; Kishimoto, H.; Kato, A.; Ohnuma, M.; Suzuki, K.

    2015-05-01

    In order to better understand the origin of field-induced anisotropy (Ku) in Si-free nanocrystalline soft magnetic alloys, the lattice spacing of the bcc-Fe phase in nanocrystalline Fe94-xNb6Bx (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 (λs) of nanocrystalline Fe94-xNb6Bx 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 λs 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 Ku values (˜100 J/m3) was estimated via the inverse magnetostrictive effect using the measured λs values and was compared to the lattice spacing estimations made by t-XRD. The lattice strain required to produce Ku 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 Ku cannot be explained through the magnetoelastic effect.

  7. 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.

  8. CONDENSED MATTER: ELECTRONIC STRUCTURE, ELECTRICAL, MAGNETIC, AND OPTICAL PROPERTIES: Growth mechanism and photoluminescence of the SnO2 nanotwists on thin film and the SnO2 short nanowires on nanorods

    NASA Astrophysics Data System (ADS)

    Wang, Bing; Xu, Ping

    2009-01-01

    SnO2 nanotwists on thin film and SnO2 short nanowires on nanorods have been grown on single silicon substrates by using Au-Ag alloying catalyst assisted carbothermal evaporation of SnO2 and active carbon powders. The morphology and the structure of the prepared nanostructures are determined on the basis of field-emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), selected area electronic diffraction (SAED), high-resolution transmission electron microscopy (HRTEM), x-ray diffraction (XRD), Raman and photoluminescence (PL) spectra analysis. The new peaks at 356, 450, and 489 nm in the measured PL spectra of two kinds of SnO2 nanostructures are observed, implying that more luminescence centres exist in these SnO2 nanostructures due to nanocrystals and defects. The growth mechanism of these nanostructures belongs to the vapour-liquid-solid (VLS) mechanism.

  9. 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

  10. 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.

  11. 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.

  12. 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

  13. 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.

  14. Nanocrystalline YCrO3 with onion-like structure and unusual magnetic behaviour

    NASA Astrophysics Data System (ADS)

    Bedekar, Vinila; Shukla, R.; Tyagi, A. K.

    2007-04-01

    Nanocrystalline YCrO3 powder was synthesized by a combustion technique using glycine as the fuel and the corresponding metal nitrates as oxidants. Three different oxidant-to-fuel ratios namely fuel-deficient, stoichiometric and fuel-excess ratios were chosen to explore the possibility to prepare single-phasic YCrO3. The crystallite size for the phase pure product after calcination at 600 °C was found to be 36 nm by x-ray line broadening. The agglomerate behaviour was investigated by light scattering studies. The TEM observations clearly highlight the pronounced crystallinity for YCrO3. A striking observation was the presence of onion-like layers in HR-TEM micrographs. Magnetic measurements reveal the weak ferromagnetic nature of YCrO3 nanoparticles, although the bulk YCrO3 is reported to be an antiferromagnetic material.

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

    NASA Astrophysics Data System (ADS)

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

    2010-10-01

    Simple coprecipitation method has been used to produce nanoparticles of MgO (magnesia), MgOṡAl2O3 (spinel), Y2O3 (yttria) and Fe3O4 (ferrite). The raw materials were, in respective, magnesium powder, magnesium and aluminium powders, ytrria powder, and natural sand. The coprecipitation included the use of suitable acid and base to dissolve the powders or sand and to produce precipitates, as well as the use of water to wash and purify the precipitates, and drying at relatively low temperatures, namely lower than 100° C, followed by heating at 450° C, 750° C, 600° C and 200° C to produce magnesia, spinel, yttria and ferrite nanopowders, respectively. X-ray diffractometry was used to characterise the purity and nanocrystallinity of the final powders. It was found qualitatively that the powders were of high purity. Further line-broadening analysis using single-line and Rietveld-based softwares was performed to reveal the nanocrystallinity of the powders. Different line breadth values were found for the powders, indicating different crystallite sizes. It was also found that, particularly for spinel and yttria, the diffraction peaks exhibited `longer' tails, indicating broader crystallite size distribution. The average crystallite size for the powders ranged from 3 to 70 nm. The results could then be used as `fingerprints' for nanocrystallinity using x-ray diffractometry. The XRD crystallite sizes for yttria and ferrite nanocrystals are in fair agreement with their counterparts from electron microscopy observation.

  16. 1-Alkyl-1-methylpiperazine-1,4-diium salts: Synthetic, acid-base, XRD-analytical, FT-IR, FT-Raman spectral and quantum chemical study

    NASA Astrophysics Data System (ADS)

    Němečková, Dana; Mary, Y. Sheena; Panicker, C. Yohannan; Varghese, Hema Tresa; Van Alsenoy, Christian; Procházková, Markéta; Pazdera, Pavel; Al-Saadi, Abdulaziz A.

    2015-08-01

    We report the preparation and results of vibrational spectral analysis, which were obtained using both FT-IR and FT-Raman spectroscopy, for three 1-alkyl-1-methylpiperazine-1,4-diium salts (AMPSs), where alkyl is benzyl 4a, n-octadecyl 4b, and methyl 4c, respectively. These were prepared by multistep synthesis from piperazine. The acid-base study of AMPSs was performed and corresponding acid-base constants were obtained. Single crystals of AMPSs suitable for XRD-analysis were obtained and analyzed. The complete vibrational assignments of wavenumbers were made on the basis of a potential energy distribution. The HOMO and LUMO analysis was used to determine the charge transfer within the molecules. The calculated first hyperpolarizabilities of AMPSs 4a-4c are 48.34, 57.77 and 123.41 times that of urea. As can be seen from the MEP plots, the negative electrostatic potential regions are mainly localized over the chlorine and oxygen atoms for compounds 4a and 4b and chlorine and iodine atoms of compound 4c, and are possible sites for electrophilic attack.

  17. 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.

  18. 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.

  19. 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.

  20. 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

  1. 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.

  2. Magnetic neurosurgery.

    PubMed

    Howard, M A; Grady, M S; Ritter, R C; Gillies, G T; Broaddus, W C; Dacey, R G

    1996-01-01

    Because of the complex shape of many brain structures, the ideal brain probe would be highly flexible and give the neurosurgeon the ability to independently and precisely control movement of the probe tip. A magnetic surgery system has been developed that implements this concept. Flexible brain probes with small permanent magnetic tips are placed on the brain surface through a small burr hole and then magnetically manipulated within the brain. Drive forces are produced by an array of six superconducting magnets suspended within a cryostatic helmet. They produce a maximum force of 3 times the threshold needed to move the probe through the parenchymal tissues at its normal speed of 1 mm/s. Computer-controlled magnetic impulses precisely direct the probe movement in any direction desired with movement accuracy of 0.47 mm in phantom gels. Probe position is monitored 3 times per second with orthogonally oriented microchannel plate X-ray systems, X-ray dose from a 3-hour simulated procedure is comparable to that of a chest X-ray. In vivo and in vitro feasibility studies have been carried out in dog and pig brains. Preclinical trials are planned for clinical applications including implantation of flexible brachytherapy threads.

  3. 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).

  4. 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.

  5. 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.

  6. 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.

  7. 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

  8. 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.

  9. 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.

  10. 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.

  11. 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

  12. Effects of uniformities of deposition of respirable particles on filters on determining their quartz contents by using the direct on-filter X-ray diffraction (DOF XRD) method.

    PubMed

    Chen, Ching-Hwa; Tsaia, Perng-Jy; Lai, Chane-Yu; Peng, Ya-Lian; Soo, Jhy-Charm; Chen, Cheng-Yao; Shih, Tung-Sheng

    2010-04-15

    In this study, field samplings were conducted in three workplaces of a foundry plant, including the molding, demolding, and bead blasting, respectively. Three respirable aerosol samplers (including a 25-mm aluminum cyclone, nylon cyclone, and IOSH cyclone) were used side-by-side to collect samples from each selected workplace. For each collected sample, the uniformity of the deposition of respirable dusts on the filter was measured and its free silica content was determined by both the DOF XRD method and NIOSH 7500 XRD method (i.e., the reference method). A same trend in measured uniformities can be found in all selected workplaces: 25-mm aluminum cyclone>nylon cyclone>IOSH cyclone. Even for samples collected by the sampler with the highest uniformity (i.e., 25-mm aluminum cyclone), the use of the DOF XRD method would lead to the measured free silica concentrations 1.15-2.89 times in magnitude higher than that of the reference method. A new filter holder should be developed with the minimum uniformity comparable to that of NIOSH 7500 XRD method (=0.78) in the future. The use of conversion factors for correcting quartz concentrations obtained from the DOF XRD method based on the measured uniformities could be suitable for the foundry industry at this stage. PMID:20006439

  13. Immobilization of invertase on chitosan coated γ-Fe2O3 magnetic nanoparticles to facilitate magnetic separation.

    PubMed

    Waifalkar, P P; Parit, S B; Chougale, A D; Sahoo, Subasa C; Patil, P S; Patil, P B

    2016-11-15

    Industrially important invertase enzyme was immobilized on chitosan coated sol gel derived γ-Fe2O3 magnetic nanoparticles (MNPs) to enable it for repetitive use by magnetic separation. MNPs were characterized by X-ray diffraction (XRD), dynamic light scattering (DLS), field emission scanning electron microscope (FE-SEM), Fourier transform infrared (FTIR) spectrometer and magnetic measurements. FTIR studies confirmed successful immobilization of invertase on MNPs. The ability to convert sucrose into invert syrup was enhanced in immobilized invertase compared to that of free enzyme. Further it was found that invertase immobilized on MNPs (IIMNPs) were more stable at varying pH and temperature conditions. Magnetic separation technique was successfully employed for reuse of the IIMNPs for 20 times without significant loss of activity. PMID:27501039

  14. Classification of hydrous meteorites (CR, CM and C2 ungrouped) by phyllosilicate fraction: PSD-XRD modal mineralogy and planetesimal environments

    NASA Astrophysics Data System (ADS)

    Howard, K. T.; Alexander, C. M. O.'D.; Schrader, D. L.; Dyl, K. A.

    2015-01-01

    The relative differences in the degree of hydration should be reflected in any classification scheme for aqueously altered meteorites. Here we report the bulk mineralogies and degree of hydration in 37 different carbonaceous chondrites: Renazzo-like (CR), Mighei-like (CM), and ungrouped (type 2) samples. This is achieved by quantifying the modal abundances of all major (phases present in abundances >1 wt.%) minerals using Position Sensitive Detector X-ray Diffraction (PSD-XRD). From these modal abundances, a classification scheme is constructed that is based on the normalized fraction of phyllosilicate (total phyllosilicate/total anhydrous silicate + total phyllosilicate). Samples are linearly ranked from type 3.0 - corresponding to a phyllosilicate fraction of <0.05, to type 1.0 - corresponding to a total phyllosilicate fraction of >0.95. Powdered meteorite samples from any hydrated carbonaceous chondrite group can be ranked on this single classification scale. The resulting classifications for CRs exhibit a range from type 2.8 to 1.3, while for CMs the range is 1.7-1.2. The primary manifestation of aqueous alteration is the production of phyllosilicate, which ceased when the fluid supply was exhausted, leading to the preservation of anhydrous silicates in all samples. The variability in hydration indicates that either accretion of ices was heterogeneous or fluid was mobilized. From the bulk mineral abundances of the most hydrated samples, we infer that the initial mass fraction of H2O inside of their parent body(ies) asteroids was <20 wt.%. Bulk carbonaceous chondrite mineralogy evolved towards increasingly oxidizing assemblages as the extent of bulk hydration increased. This is consistent with the escape of reducing H2 gas that is predicted to have been produced from water during hydration reactions.

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

    SciTech Connect

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

    2010-10-24

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

  16. HRTEM study comparing naturally and experimentally weathered pyroxenoids

    SciTech Connect

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

    1995-01-01

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

  17. 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.

  18. Superconducting Magnets for Magnetic Resonance Imaging

    NASA Astrophysics Data System (ADS)

    Feenan, Peter

    2000-03-01

    MRI is now a well established diagnostic technique in medicine. The richness of information provided by magnetic resonance gives rise to a variety of techniques which in turn leads to a variety of magnet designs. Magnet designers must consider suitable superconduting materials for the magnet, but need also to consider the overall fomat of the magnet to maximise patient comfort, access for clinicians and convenience of use - in some examples magnets are destined for use within the operating theatre and special considerations are required for this. Magnet types include; (1) low-field general purpose imagers, (2) extremity imaging, (3) open magnets with exellent all-round access often employing iron or permanent magnetic materials, (4) high-field magnets, and (5) very high-field (7 Tesla and more) magnets for spectroscopy and functional imaging research. Examples of these magnet varieties will be shown and some of the design challenges discussed.

  19. 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.

  20. Magnetic Liquids

    NASA Technical Reports Server (NTRS)

    1987-01-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2016-11-01

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

  2. Grain Size Control of the Magnetic Nanoparticles by Solid State Route Modification

    NASA Astrophysics Data System (ADS)

    Barreto, A. C. H.; Santiago, V. R.; Freire, R. M.; Mazzetto, S. E.; Sasaki, J. M.; Vasconcelos, I. F.; Denardin, J. C.; Mele, Giuseppe; Carbone, Luigi; Fechine, P. B. A.

    2013-07-01

    The CoFe2O4 and NiFe2O4 nanoparticles were synthesized exploiting a co-precipitation method and afterward calcinated at 400 °C through two different experimental apparatus: a conventional muffle and rotatory oven. X-ray diffraction (XRD) analysis revealed that nanocrystalline ferrites grew with a face center cubic structure (fcc) and Fd3 m symmetry space group. XRD, transmission electron microscopy, and magnetic measurements confirmed the compositional homogeneity and the narrow size particle distribution (6-8 nm) of the sample thermally treated in a rotary oven, in all likelihood due to the sample's constant turning movement. The size of the magnetic particles is extremely important and influences the choice of a potential technological application. For this reason, our study emerges as a new and simple innovating procedure to control the size of magnetic nanoparticles.

  3. Effect of Sc3+ on structural and magnetic properties of Mn-Zn nano ferrites

    NASA Astrophysics Data System (ADS)

    Jagadeesha Angadi, V.; Matteppanavar, Shidaling; Srinatha, N.; Melagiriyappa, E.; Rudraswamy, B.

    2016-05-01

    In the present investigation, for the first time, we report on the effect of Sc3+ on the structural and magnetic properties of Mn0.5Zn0.5ScyFe2-yO4 (y = 0.01, 0.03 and 0.05) nanoferrites synthesized by solution combustion method using the mixture of fuels. As synthesized powders were characterized for the detailed structural analysis by X-ray diffractometer (XRD), Fourier transmission infrared spectroscopy (FTIR) and room temperature magnetic properties by using vibrating sample magnetometer (VSM). The results of XRD and FTIR confirm that the formation of nano crystalline, single-phased Mn-Zn ferrite with cubic spinel structure belongs to Fd-3m space group. The room temperature magnetic studies shows that, the saturation magnetization (MS), remanence magnetization (MR) and magnetic moment (ηB), magnetic particle size (Dm) have found to increase with Sc3+ ion concentration up to x = 0.3 and then decrease. The values of αY-K and the magnetic particle size (Dm) are found to be in the range of 68-75° and 10-19 nm respectively, with Sc3+ concentration.

  4. Preparation, Characterization of High-Luminescent and Magnetic Eu3+, Dy3+ Doped Superparamagnetic Nano-Fe3O4.

    PubMed

    Huan, Weiwei; Ji, Guoyuan; Cheng, Chao; An, Jie; Yang, Yuxiang; Liu, Xiangnong

    2015-02-01

    Pure superparamagnetic nano-Fe3O4 (SPMNPs) and Ln3+ (Eu3+, Dy3+) doped SPMNPs are successfully synthesized by reverse micelle method. The structure, morphology, magnetic properties and PL properties of the samples were characterized by XRD, FT-IR, TEM, PPMS, EDS and luminescence spectrometer respectively. The influences of Ln3+ doping amount on magnetic properties and PL properties were investigated in detail. The results show, with increasing of the Lna+ doping amount increasing, the morphologies and particle sizes of the doped Fe304 nanoparticles change, leading to saturation magnetization and coercivity changing accordingly. The change of lattice parameter and particle size was discussed based on Rietveld analysis of XRD pattern of the doped Fe3O4 nanoparticles. The coincidence of the ZFC and FC magnetization curves within the temperature range from 120.6 to 300 K, indicating that Fe3O4 nanoparticles are single domain super-paramagnetic. PMID:26353732

  5. 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.

  6. [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

  7. [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

  8. 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

  9. Remarkable effect of the preparation technique on the state of cobalt ions in BEA zeolites evidenced by FTIR spectroscopy of adsorbed CO and NO, TPR and XRD.

    PubMed

    Mihaylova, Angelina; Hadjiivanov, Konstantin; Dzwigaj, Stanislaw; Che, Michel

    2006-10-01

    The state of cobalt in two BEA zeolites was studied by XRD, TPR, and FTIR spectroscopy using CO and NO as probe molecules. One of the samples, CoAlBEA (0.4 wt % of Co), was prepared by conventional ion exchange and the other, CoSiBEA (0.7 wt % Co), by a two-step postsynthesis method involving dealuminated SiBEA zeolite. The introduction of Co into SiBEA leads to an increase of unit cell parameters of the BEA structure and to the consumption of silanol groups in vacant T-sites of the dealuminated zeolite. In contrast, no structural changes are observed after incorporation of cobalt into AlBEA by ion-exchange. The reduction temperature of cobalt in CoSiBEA zeolite (1130 K), is much higher than for CoAlBEA and indicates a strong interaction of cobalt ions with SiBEA. Low-temperature CO adsorption on CoAlBEA results in (i) H-bonded CO, (ii) Co(3+)-CO adducts (2,208 cm(-1)) and (iii) a small amount of Co(2+)-CO complexes (2,188 cm(-1)). In agreement with these results, NO adsorption leads to the appearance of (i) NO(+) (2,133 cm(-1), formed with the participation of the zeolite acidic hydroxyls), (ii) Co(3+)-NO (1932 cm(-1)), and (iii) a small amount of Co(2+)(NO)(2) dinitrosyls (nu(s) = 1,898 and nu(as) = 1,814 cm(-1)). Low-temperature CO adsorption on CoSiBEA leads to formation of two kinds of Co(2+)-CO adducts (2,185 and 2,178 cm(-1)). No Co(3+) cations are detected. In line with these results, adsorption of NO reveals the existence of two kinds of Co(2+)(NO)(2) dinitrosyls (nu(s) = 1,888 and nu(as) = 1,808 cm(-1) and nu(s) = 1,878 and nu(as) = 1,799 cm(-1), respectively).

  10. Structural, magnetic and microstructural studies of composition-modified Sm-Co ribbons

    NASA Astrophysics Data System (ADS)

    Jiang, Xiujuan

    magnetization and coercivity was observed. Microstructural analysis and microchemistry information obtained from TEM/HRTEM and 3D atom probe revealed the possible reasons behind the improvement.

  11. Magnetic bearing. [for supplying magnetic fluxes

    NASA Technical Reports Server (NTRS)

    Studer, P. A. (Inventor)

    1975-01-01

    A magnetic bearing is described which includes a pair of coaxial, toroidal, and permanent magnets having axially directed poles. Like poles of the permanent magnets are adjacent to each other, whereby the permanent magnets have a tendency to be urged apart along the common axis. An electromagnet is wound coaxially with the permanent magnets in such a manner that the poles are axially directed. Between the poles of each permanent magnet there is a low magnetic reluctance circuit including two series air gaps. Between the poles of the electromagnet a low reluctance path including only one air gap of each of the low magnetic reluctance circuits is provided. The low reluctance path for the electromagnet includes a ring axially translatable relative to the permanent magnets. The ring forms opposite faces of the air gaps in the magnetic circuits for each permanent magnet.

  12. Magnetic comparison of abiogenic and biogenic alteration products of lepidocrocite

    NASA Astrophysics Data System (ADS)

    Till, J. L.; Guyodo, Y.; Lagroix, F.; Ona-Nguema, G.; Brest, J.

    2014-06-01

    Lepidocrocite is a potentially important Fe-bearing precursor phase for the production of nanoscale Fe-oxide particles in the environment. We present a detailed magnetic characterization of various alteration products of lepidocrocite resulting from thermal dehydroxylation reactions and bacterially induced bioreduction and remineralization, accompanied by characterization with x-ray diffraction (XRD) and transmission electron microscopy. Dehydroxylation during annealing at moderate temperatures produces a topotactic transformation from lepidocrocite to maghemite when heated in an oxidizing atmosphere, or to magnetite when heated in a reducing atmosphere. The abiotic Fe-oxide products form an oriented framework of strongly interacting superparamagnetic crystallites and are characterized by a distinctive porous nanostructure observed by electron microscopy. Lepidocrocite bioreduction by the iron-reducing bacterium Shewanella putrefaciens ATCC 8071 produces nanoscale particles of a strongly magnetic phase. This Fe(II)-bearing mineral produced by bioreduction is highly crystalline and euhedral in shape, with a broad grain size distribution and is indicated by magnetic and XRD measurements to be a cation-excess magnetite. We highlight the distinguishing microscopic characteristics of magnetite from both abiotic and bacterially induced mineralization that should allow them to be identified in natural settings. Moreover, both mechanisms of alteration represent potential pathways for the direct formation of strongly magnetic fine-grained Fe-oxide particles in sedimentary environments.

  13. 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,

  14. 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.

  15. 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...

  16. Synthesis of magnetic nanofibers using femtosecond laser material processing in air

    PubMed Central

    2011-01-01

    In this study, we report formation of weblike fibrous nanostructure and nanoparticles of magnetic neodymium-iron-boron (NdFeB) via femtosecond laser radiation at MHz pulse repetition frequency in air at atmospheric pressure. Scanning electron microscopy (SEM) analysis revealed that the nanostructure is formed due to aggregation of polycrystalline nanoparticles of the respective constituent materials. The nanofibers diameter varies between 30 and 70 nm and they are mixed with nanoparticles. The effect of pulse to pulse separation rate on the size of the magnetic fibrous structure and the magnetic strength was reported. X-ray diffraction (XRD) analysis revealed metallic and oxide phases in the nanostructure. The growth of magnetic nanostructure is highly recommended for the applications of magnetic devices like biosensors and the results suggest that the pulsed-laser method is a promising technique for growing nanocrystalline magnetic nanofibers and nanoparticles for biomedical applications. PMID:21711890

  17. Synthesis of magnetic nanofibers using femtosecond laser material processing in air

    NASA Astrophysics Data System (ADS)

    Alubaidy, Mohammed-Amin; Venkatakrishnan, Krishnan; Tan, Bo

    2011-05-01

    In this study, we report formation of weblike fibrous nanostructure and nanoparticles of magnetic neodymium-iron-boron (NdFeB) via femtosecond laser radiation at MHz pulse repetition frequency in air at atmospheric pressure. Scanning electron microscopy (SEM) analysis revealed that the nanostructure is formed due to aggregation of polycrystalline nanoparticles of the respective constituent materials. The nanofibers diameter varies between 30 and 70 nm and they are mixed with nanoparticles. The effect of pulse to pulse separation rate on the size of the magnetic fibrous structure and the magnetic strength was reported. X-ray diffraction (XRD) analysis revealed metallic and oxide phases in the nanostructure. The growth of magnetic nanostructure is highly recommended for the applications of magnetic devices like biosensors and the results suggest that the pulsed-laser method is a promising technique for growing nanocrystalline magnetic nanofibers and nanoparticles for biomedical applications.

  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 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.

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

    PubMed Central

    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

  1. Temperature-induced phenomena in systems of magnetic nanoparticles

    NASA Astrophysics Data System (ADS)

    Bhuiya, Abdul Wazed

    Magnetic nanoparticle ensembles have received a lot of attention, stemming in part from their current and potential applications in biomedicine and in the development of high-density magnetic storage media. Key to the functionality of these systems are microscopic structures and mechanisms that make them exhibit unique properties and behave differently from their bulk counterparts. We studied microscopic structures and processes that dictate macroscopic properties, behavior and functionality of magnetic nanoparticle ensembles. As the temperature T strongly influences the magnetic behavior of these systems, we studied temperature dependent magnetic properties using AC-susceptibility and DC-magnetization measurements carried out over a broad range of temperatures, between 3 and 300 K. We extracted structural information from X-ray diffraction (XRD) and direct imaging techniques and correlate it with magnetic properties, in an attempt at better understanding the microscopic structures and magnetic mechanisms responsible for the macroscopic magnetic behavior. We studied ensembles of magnetic nanoparticles: nickel ferrite immobilized in a solid matrix and cobalt ferrite immersed in carrier fluid respectively, in order to explore their potential use in biomedical applications and magnetic recording. For both NiFe2O4(NFO) and Co0.2Fe2.8O4 (CFO) relaxation mechanisms were determined. Structural properties and average particle sizes were derived from XRD, including synchrotron XRD, and direct imaging techniques such as scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Temperature dependent magnetic measurements, FC-ZFC DC magnetometry, as well as AC complex susceptibility measurements at frequencies between 10 and 10,000 Hz were carried out within the temperature range 3Kmagnetization and AC susceptibility measurements were performed using a Physical Property Measurement System (PPMS), which allows measurements in magnetic fields up

  2. Magnetic Cellulose Nanocrystal Based Anisotropic Polylactic Acid Nanocomposite Films: Influence on Electrical, Magnetic, Thermal, and Mechanical Properties.

    PubMed

    Dhar, Prodyut; Kumar, Amit; Katiyar, Vimal

    2016-07-20

    This paper reports a single-step co-precipitation method for the fabrication of magnetic cellulose nanocrystals (MGCNCs) with high iron oxide nanoparticle content (∼51 wt % loading) adsorbed onto cellulose nanocrystals (CNCs). X-ray diffraction (XRD), Fourier transform infrared (FTIR), and Raman spectroscopic studies confirmed that the hydroxyl groups on the surface of CNCs (derived from the bamboo pulp) acted as anchor points for the adsorption of Fe3O4 nanoparticles. The fabricated MGCNCs have a high magnetic moment, which is utilized to orient the magnetoresponsive nanofillers in parallel or perpendicular orientations inside the polylactic acid (PLA) matrix. Magnetic-field-assisted directional alignment of MGCNCs led to the incorporation of anisotropic mechanical, thermal, and electrical properties in the fabricated PLA-MGCNC nanocomposites. Thermomechanical studies showed significant improvement in the elastic modulus and glass-transition temperature for the magnetically oriented samples. Differential scanning calorimetry (DSC) and XRD studies confirmed that the alignment of MGCNCs led to the improvement in the percentage crystallinity and, with the absence of the cold-crystallization phenomenon, finds a potential application in polymer processing in the presence of magnetic field. The tensile strength and percentage elongation for the parallel-oriented samples improved by ∼70 and 240%, respectively, and for perpendicular-oriented samples, by ∼58 and 172%, respectively, in comparison to the unoriented samples. Furthermore, its anisotropically induced electrical and magnetic properties are desirable for fabricating self-biased electronics products. We also demonstrate that the fabricated anisotropic PLA-MGCNC nanocomposites could be laminated into films with the incorporation of directionally tunable mechanical properties. Therefore, the current study provides a novel noninvasive approach of orienting nontoxic bioderived CNCs in the presence of low

  3. Magnetic Cellulose Nanocrystal Based Anisotropic Polylactic Acid Nanocomposite Films: Influence on Electrical, Magnetic, Thermal, and Mechanical Properties.

    PubMed

    Dhar, Prodyut; Kumar, Amit; Katiyar, Vimal

    2016-07-20

    This paper reports a single-step co-precipitation method for the fabrication of magnetic cellulose nanocrystals (MGCNCs) with high iron oxide nanoparticle content (∼51 wt % loading) adsorbed onto cellulose nanocrystals (CNCs). X-ray diffraction (XRD), Fourier transform infrared (FTIR), and Raman spectroscopic studies confirmed that the hydroxyl groups on the surface of CNCs (derived from the bamboo pulp) acted as anchor points for the adsorption of Fe3O4 nanoparticles. The fabricated MGCNCs have a high magnetic moment, which is utilized to orient the magnetoresponsive nanofillers in parallel or perpendicular orientations inside the polylactic acid (PLA) matrix. Magnetic-field-assisted directional alignment of MGCNCs led to the incorporation of anisotropic mechanical, thermal, and electrical properties in the fabricated PLA-MGCNC nanocomposites. Thermomechanical studies showed significant improvement in the elastic modulus and glass-transition temperature for the magnetically oriented samples. Differential scanning calorimetry (DSC) and XRD studies confirmed that the alignment of MGCNCs led to the improvement in the percentage crystallinity and, with the absence of the cold-crystallization phenomenon, finds a potential application in polymer processing in the presence of magnetic field. The tensile strength and percentage elongation for the parallel-oriented samples improved by ∼70 and 240%, respectively, and for perpendicular-oriented samples, by ∼58 and 172%, respectively, in comparison to the unoriented samples. Furthermore, its anisotropically induced electrical and magnetic properties are desirable for fabricating self-biased electronics products. We also demonstrate that the fabricated anisotropic PLA-MGCNC nanocomposites could be laminated into films with the incorporation of directionally tunable mechanical properties. Therefore, the current study provides a novel noninvasive approach of orienting nontoxic bioderived CNCs in the presence of low

  4. Structural reinvestigation of Li3FeN2: Evidence of cationic disorder through XRD, solid-state NMR and Mössbauer spectroscopy

    NASA Astrophysics Data System (ADS)

    Panabière, E.; Emery, N.; Lorthioir, C.; Sougrati, M. T.; Jumas, J.-C.; Bach, S.; Pereira-Ramos, J.-P.; Smith, R. I.; Willmann, P.

    2016-08-01

    A significant cationic disorder is evidenced on Li3FeN2 prepared through solid-state reaction under controlled atmosphere. This derivative anti fluorite type structure (orthorhombic, space group Ibam, a=4.870(1) Å, b=9.652(1) Å and c=4.789(1) Å), solved first through single crystal X-ray diffraction [7], is usually described by Li+ and Fe+3 ordered distribution in tetrahedral sites formed by the nitrogen network, leading to [FeN4/2]3- edge-sharing tetrahedral chains. From 7Li/6Li Nuclear Magnetic Resonance spectroscopy, 57Fe Mössbauer spectroscopy and powder X-ray and neutron diffraction, we demonstrate that about 4% of lithium sites are filled by iron and about 11% of iron sites are occupied by Li, which can explain the discrepancy within the Gudat's model observed on larger scale solid-state synthesis samples.

  5. 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

  6. Ferroelectricity in spiral magnets.

    PubMed

    Mostovoy, Maxim

    2006-02-17

    It was recently observed that the ferroelectrics showing the strongest sensitivity to an applied magnetic field are spiral magnets. We present a phenomenological theory of inhomogeneous ferroelectric magnets, which describes their thermodynamics and magnetic field behavior, e.g., dielectric susceptibility anomalies at magnetic transitions and sudden flops of electric polarization in an applied magnetic field. We show that electric polarization can also be induced at domain walls and that magnetic vortices carry electric charge. PMID:16606047

  7. Structural and magnetic properties of turmeric functionalized CoFe2O4 nanocomposite powder

    NASA Astrophysics Data System (ADS)

    Mehran, E.; Farjami Shayesteh, S.; Sheykhan, M.

    2016-10-01

    The structural and magnetic properties of the synthesized pure and functionalized CoFe2O4 magnetic nanoparticles (NPs) are studied by analyzing the results from the x-ray diffraction (XRD), transmission electron microscopy (TEM), FT-IR spectroscopy, thermogravimetry (TG), and vibrating sample magnetometer (VSM). To extract the structure and lattice parameters from the XRD analysis results, we first apply the pseudo-Voigt model function to the experimental data obtained from XRD analysis and then the Rietveld algorithm is used in order to optimize the model function to estimate the true intensity values. Our simulated intensities are in good agreement with the experimental peaks, therefore, all structural parameters such as crystallite size and lattice constant are achieved through this simulation. Magnetic analysis reveals that the synthesized functionalized NPs have a saturation magnetization almost equal to that of pure nanoparticles (PNPs). It is also found that the presence of the turmeric causes a small reduction in coercivity of the functionalized NPs in comparison with PNP. Our TGA and FTIR results show that the turmeric is bonded very well to the surface of the NPs. So it can be inferred that a nancomposite (NC) powder of turmeric and nanoparticles is produced. As an application, the anti-arsenic characteristic of turmeric makes the synthesized functionalized NPs or NC powder a good candidate for arsenic removal from polluted industrial waste water. Project supported by the University of Guilan and the Iran Nanotechnology Initiative Council.

  8. Vertical Si nanowire arrays fabricated by magnetically guided metal-assisted chemical etching

    NASA Astrophysics Data System (ADS)

    Chun, Dong Won; Kim, Tae Kyoung; Choi, Duyoung; Caldwell, Elizabeth; Kim, Young Jin; Paik, Jae Cheol; Jin, Sungho; Chen, Renkun

    2016-11-01

    In this work, vertically aligned Si nanowire arrays were fabricated by magnetically guided metal-assisted directional chemical etching. Using an anodized aluminum oxide template as a shadow mask, nanoscale Ni dot arrays were fabricated on an Si wafer to serve as a mask to protect the Si during the etching. For the magnetically guided chemical etching, we deposited a tri-layer metal catalyst (Au/Fe/Au) in a Swiss-cheese configuration and etched the sample under the magnetic field to improve the directionality of the Si nanowire etching and increase the etching rate along the vertical direction. After the etching, the nanowires were dried with minimal surface-tension-induced aggregation by utilizing a supercritical CO2 drying procedure. High-resolution transmission electron microscopy (HR-TEM) analysis confirmed the formation of single-crystal Si nanowires. The method developed here for producing vertically aligned Si nanowire arrays could find a wide range of applications in electrochemical and electronic devices.

  9. A silicon dioxide modified magnetic nanoparticles-labeled lateral flow strips for HBs antigen.

    PubMed

    Zhang, Xueqing; Jiang, Lin; Zhang, Chunlei; Li, Ding; Wang, Can; Gao, Feng; Cui, Daxiang

    2011-12-01

    Herein we reported a new type of silicon dioxide wrapped magnetic nanoparticles-labeled lateral flow strip for detection of HBs antigen in sera. The SiO2 wrapped Fe3O4 nanocomposites were prepared and characterized by HR-TEM, FTIR and magnetometer. As-prepared nanocomposites were used to label anti-HBV surface monoclonal antibody, the lateral flow strips were constructed, and 100 specimens of sera were collected and tested. Results showed that the prepared SiO2 wrapped Fe3O4 nanocomposites were shell/core structure, well dispersed, with the size of 25 nm in diameter, the thickness of the shell was about 3 nm, their magnetic saturation intensity was 44.3 meu g(-1). Clinical sera specimens test results showed that the prepared lateral flow strips were with the detection limitation of 5 pg/mL by naked eye observation, and 0.1 pg/mL by CCD reader or MAR Analyzer, specificity was 100%. In conclusion, one kind of silicon dioxide wrapped magnetic nanoparticles-labeled lateral flow strip for ultrasensitive detection of HBs antigen was successfully developed, its ease of use, sensitiveness and low-cost make it well-suited for population-based on-the-site hepatitis B screening.

  10. 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

  11. Gas-phase synthesis of magnetic metal/polymer nanocomposites

    NASA Astrophysics Data System (ADS)

    Starsich, Fabian H. L.; Hirt, Ann M.; Stark, Wendelin J.; Grass, Robert N.

    2014-12-01

    Highly magnetic metal Co nanoparticles were produced via reducing flame spray pyrolysis, and directly coated with an epoxy polymer in flight. The polymer content in the samples varied between 14 and 56 wt% of nominal content. A homogenous dispersion of Co nanoparticles in the resulting nanocomposites was visualized by electron microscopy. The size and crystallinity of the metallic fillers was not affected by the polymer, as shown by XRD and magnetic hysteresis measurements. The good control of the polymer content in the product nanocomposite was shown by elemental analysis. Further, the successful polymerization in the gas phase was demonstrated by electron microscopy and size measurements. The presented effective, dry and scalable one-step synthesis method for highly magnetic metal nanoparticle/polymer composites presented here may drastically decrease production costs and increase industrial yields.

  12. Gas-phase synthesis of magnetic metal/polymer nanocomposites.

    PubMed

    Starsich, Fabian H L; Hirt, Ann M; Stark, Wendelin J; Grass, Robert N

    2014-12-19

    Highly magnetic metal Co nanoparticles were produced via reducing flame spray pyrolysis, and directly coated with an epoxy polymer in flight. The polymer content in the samples varied between 14 and 56 wt% of nominal content. A homogenous dispersion of Co nanoparticles in the resulting nanocomposites was visualized by electron microscopy. The size and crystallinity of the metallic fillers was not affected by the polymer, as shown by XRD and magnetic hysteresis measurements. The good control of the polymer content in the product nanocomposite was shown by elemental analysis. Further, the successful polymerization in the gas phase was demonstrated by electron microscopy and size measurements. The presented effective, dry and scalable one-step synthesis method for highly magnetic metal nanoparticle/polymer composites presented here may drastically decrease production costs and increase industrial yields. PMID:25422410

  13. 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.

  14. Experimental investigation of thermal conductivity of magnetic nanofluids

    NASA Astrophysics Data System (ADS)

    Parekh, Kinnari; Lee, H. S.

    2012-06-01

    Two different magnetic nanofluids comprising of magnetite and Mn-Zn ferrite particles were synthesized in light hydrocarbon oil using continuous chemical process. Powder XRD and TEM image show single phase spinel structure with size of 10 nm and 6.7 nm, respectively for magnetite and Mn-Zn ferrite. Thermal conductivity of nanofluids has been studied as a function of volume fraction under transverse magnetic field. Magnetite nanofluid shows 17% enhancements in thermal conductivity for 4.7% volume fraction while Mn-Zn ferrite shows 45% enhancement at 10% volume fraction. In presence of transverse magnetic field the magnetite nanofluids shows further enhancement from 17% to 30% while no change in thermal conductivity has been observed for Mn-Zn ferrite. These results are explained considering the dipolar coupling co-efficient which for magnetite particles favors chain structures.

  15. Radiolabeled D-Penicillamine Magnetic Nanocarriers for Targeted Purposes.

    PubMed

    Özyüncü, Seniha Yolcular; Teksöz, Serap; Içhedef, Çiğdem; Medinel, E Ilker; Avci, Çiğir Biray; Gündüz, Cumhur; Ünak, Perihan

    2016-04-01

    The aim of this study is to synthesize D-Penicillamine (D-PA) conjugated magnetic nanocarriers for targeted purposes. Magnetic nanoparticles were prepared by partial reduction method and surface modification was done with an amino silane coupling agent's (structural properties), AEAPS, the particles were characterized by Scanning Electron Microscope (SEM), X-ray Diffraction (XRD). After that D-PA was linked with the magnetic nanoparticles (MNPs) and has been radiolabeled with [99mTc(CO)3]+ core. Quality controls of [99mTc(CO)3-MNP-D-PA] were established by Cd(Te) detector. The radiolabeling efficiency of magnetic nanoparticles ([99mTc(CO)3-MNP-D-PA]) was about 97.05% with good in vitro stability during the 24 hour period. As a parallel study, radiolabeled D-PA complex ([99mTc(CO)3-D-PA]) was prepared with a radiolabeling yield of 97.93%. At the end, biologic activities of binding complexes were investigated on MCF7 human breast cancer cells. Our results show that, radiolabeled magnetic nanoparticles with core [99mTc(CO)3]+ ([99mTc(CO)3-MNP-D-PA]) showed the highest uptake on MCF7 cells which were applied magnetic field in the wells. In that case, result of this study emphasizes that radiolabeled magnetic nanoparticles with core [99mTc(CO)3]+ would support new occurrences of new agents. PMID:27451783

  16. Self-reversal and apparent magnetic excursions in Arctic sediments

    NASA Astrophysics Data System (ADS)

    Channell, J. E. T.; Xuan, C.

    2009-06-01

    The Arctic oceans have been fertile ground for the recording of apparent excursions of the geomagnetic field, implying that the high latitude field had unusual characteristics at least over the last 1-2 Myrs. Alternating field demagnetization of the natural remanent magnetization (NRM) of Core HLY0503-6JPC from the Mendeleev Ridge (Arctic Ocean) implies the presence of primary magnetizations with negative inclination apparently recording excursions in sediments deposited during the Brunhes Chron. Thermal demagnetization, on the other hand, indicates the presence of multiple (often anti-parallel) magnetization components with negative inclination components having blocking temperatures predominantly, but not entirely, below ~ 350 °C. Thermo-magnetic tests, X-ray diffraction (XRD) and scanning electron microscopy (SEM) indicate that the negative inclination components are carried by titanomaghemite, presumably formed by seafloor oxidation of titanomagnetite. The titanomaghemite apparently carries a chemical remanent magnetization (CRM) that is partially self-reversed relative to the detrital remanent magnetization (DRM) carried by the host titanomagnetite. The partial self-reversal could have been accomplished by ionic ordering during oxidation, thereby changing the balance of the magnetic moments in the ferrimagnetic sublattices.

  17. Magnetic Nanoparticle Sensors

    PubMed Central

    Koh, Isaac; Josephson, Lee

    2009-01-01

    Many types of biosensors employ magnetic nanoparticles (diameter = 5–300 nm) or magnetic particles (diameter = 300–5,000 nm) which have been surface functionalized to recognize specific molecular targets. Here we cover three types of biosensors that employ different biosensing principles, magnetic materials, and instrumentation. The first type consists of magnetic relaxation switch assay-sensors, which are based on the effects magnetic particles exert on water proton relaxation rates. The second type consists of magnetic particle relaxation sensors, which determine the relaxation of the magnetic moment within the magnetic particle. The third type is magnetoresistive sensors, which detect the presence of magnetic particles on the surface of electronic devices that are sensitive to changes in magnetic fields on their surface. Recent improvements in the design of magnetic nanoparticles (and magnetic particles), together with improvements in instrumentation, suggest that magnetic material-based biosensors may become widely used in the future. PMID:22408498

  18. 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.

  19. Electrically Tunable Magnetism in Magnetic Topological Insulators.

    PubMed

    Wang, Jing; Lian, Biao; Zhang, Shou-Cheng

    2015-07-17

    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 modification of magnetism. Remarkably, the electric field could even induce the magnetic quantum phase transition from ferromagnetism to paramagnetism. We further propose a transistor device in which the dissipationless charge transport of chiral edge states is controlled by an electric field. In particular, the field-controlled ferromagnetism in a magnetic topological insulator can be used for voltage based writing of magnetic random access memories in magnetic tunnel junctions. The simultaneous electrical control of magnetic order and chiral edge transport in such devices may lead to electronic and spintronic applications for topological insulators.

  20. 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.

  1. 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.

  2. 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.

  3. 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.

  4. 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.

  5. 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.

  6. Magnet innovations for linacs

    SciTech Connect

    Halbach, K.

    1986-06-01

    It is possible to produce large magnetic fields at the aperture of permanent magnet quadrupoles, even when the magnetic aperture is very small. That, combined with their compactness, makes permanent magnet quadrupoles very powerful components of small aperture linacs. Results will be presented about past and present work on both fixed and variable strength permanent magnets suitable for use in and around linacs.

  7. Magnetic field sensor

    NASA Astrophysics Data System (ADS)

    Silva, Nicolas

    2012-09-01

    Earlier papers1-3 in this journal have described experiments on measuring the magnetic fields of current-carrying wires and permanent magnets using magnetic field probes of various kinds. This paper explains how to use an iPad and the free app MagnetMeter-3D Vector Magnetometer and Accelerometer4 (compass HD) to measure the magnetic fields.

  8. 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.

  9. Structural, electronic, and magnetic investigation of magnetic ordering in MBE-grown CrxSb2-xTe3 thin films

    NASA Astrophysics Data System (ADS)

    Collins-McIntyre, L. J.; Duffy, L. B.; Singh, A.; Steinke, N.-J.; Kinane, C. J.; Charlton, T. R.; Pushp, A.; Kellock, A. J.; Parkin, S. S. P.; Holmes, S. N.; Barnes, C. H. W.; van der Laan, G.; Langridge, S.; Hesjedal, T.

    2016-07-01

    We report the structural, electronic, and magnetic study of Cr-doped Sb2Te3 thin films grown by a two-step deposition process using molecular-beam epitaxy (MBE). The samples were investigated using a variety of complementary techniques, namely, x-ray diffraction (XRD), atomic force microscopy, SQUID magnetometry, magneto-transport, and polarized neutron reflectometry (PNR). It is found that the samples retain good crystalline order up to a doping level of x=0.42 (in Cr x Sb2-x Te3), above which degradation of the crystal structure is observed by XRD. Fits to the recorded XRD spectra indicate a general reduction in the c-axis lattice parameter as a function of doping, consistent with substitutional doping with an ion of smaller ionic radius. The samples show soft ferromagnetic behavior with the easy axis of magnetization being out-of-plane. The saturation magnetization is dependent on the doping level, and reaches from ˜2 μ_\\text{B} to almost 3 μ_\\text{B} per Cr ion. The transition temperature (T{c}) depends strongly on the Cr concentration and is found to increase with doping concentration. For the highest achievable doping level for phase-pure films of x=0.42 , a T{c} of 125 K was determined. Electric transport measurements find surface-dominated transport below ˜10 K. The magnetic properties extracted from anomalous Hall effect data are in excellent agreement with the magnetometry data. PNR studies indicate a uniform magnetization profile throughout the film, with no indication of enhanced magnetic order towards the sample surface.

  10. Structural, electronic, and magnetic investigation of magnetic ordering in MBE-grown CrxSb2‑xTe3 thin films

    NASA Astrophysics Data System (ADS)

    Collins-McIntyre, L. J.; Duffy, L. B.; Singh, A.; Steinke, N.-J.; Kinane, C. J.; Charlton, T. R.; Pushp, A.; Kellock, A. J.; Parkin, S. S. P.; Holmes, S. N.; Barnes, C. H. W.; van der Laan, G.; Langridge, S.; Hesjedal, T.

    2016-07-01

    We report the structural, electronic, and magnetic study of Cr-doped Sb2Te3 thin films grown by a two-step deposition process using molecular-beam epitaxy (MBE). The samples were investigated using a variety of complementary techniques, namely, x-ray diffraction (XRD), atomic force microscopy, SQUID magnetometry, magneto-transport, and polarized neutron reflectometry (PNR). It is found that the samples retain good crystalline order up to a doping level of x=0.42 (in Cr x Sb2‑x Te3), above which degradation of the crystal structure is observed by XRD. Fits to the recorded XRD spectra indicate a general reduction in the c-axis lattice parameter as a function of doping, consistent with substitutional doping with an ion of smaller ionic radius. The samples show soft ferromagnetic behavior with the easy axis of magnetization being out-of-plane. The saturation magnetization is dependent on the doping level, and reaches from ∼2 μ_\\text{B} to almost 3 μ_\\text{B} per Cr ion. The transition temperature (T{c}) depends strongly on the Cr concentration and is found to increase with doping concentration. For the highest achievable doping level for phase-pure films of x=0.42 , a T{c} of 125 K was determined. Electric transport measurements find surface-dominated transport below ∼10 K. The magnetic properties extracted from anomalous Hall effect data are in excellent agreement with the magnetometry data. PNR studies indicate a uniform magnetization profile throughout the film, with no indication of enhanced magnetic order towards the sample surface.

  11. 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

  12. 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.

  13. 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.

  14. 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.

  15. Magnetic interactions in cubic iron oxide magnetic nanoparticle bound to zeolite

    NASA Astrophysics Data System (ADS)

    Singh, L. Herojit; Pati, Sudhanshu S.; Coaquira, J. A. H.; Matilla, John; Guimarães, Edi M.; Oliveira, A. C.; Kuzmann, E.; Garg, Vijayendra K.

    2016-10-01

    Magnetic interaction of the magnetite (Fe3O4) nanoparticles grown on zeolite has been studied. XRD patterns show that in the presence of 25-75 mg of zeolite the average particle size of Fe3O4 decreases to ≈6 nm, but with the increase of zeolite content (75 mgmagnetization decreases from 63 to 53 emu/g. Mössbauer studies show the presence of different Fe3O4 microenvironments, possibly in pores and on the surface of zeolite. Transformation of the superparamagnetic doublet to sextet at 80 K can indicate a variation in the magnetic interaction. At low temperature the interaction between Fe3O4 at the pore and at the surface enhances the magnetic ordering. The nanoparticles in the pores of zeolite are connected with the surface particles in low zeolite content and get isolated as the amount of zeolite increases.

  16. Magnetic and Magnetocaloric Properties of High-Energy Ball-Milled Nanocrystalline CeMn2Ge2 Compound

    NASA Astrophysics Data System (ADS)

    Kaya, Melike; Dincer, Ilker; Akturk, Selcuk; Elerman, Yalcin

    2016-10-01

    CeMn2Ge2 nanopowders have been obtained by high-energy ball milling for 5 and 10 hours from bulk compound to investigate the effect of milling time on magnetic and magnetocaloric properties. CeMn2Ge2 nanopowders have been characterized by X-ray diffraction (XRD), scanning electron microscopy with energy-dispersive X-ray spectroscopy, transmission electron microscopy, and magnetization measurements. The average grain size of the nanoparticles from XRD measurements is about 12.2 and 8 nm for 5-hour and 10-hour ball-milled samples, respectively. The investigations reveal that magnetic entropy change (∆ S m) can be altered by changing the particle size of the compound. Maximum ∆ S m is -2.45 and -1.30 J kg-1 K-1 for the 5- and 10-hour ball-milled nanopowders, respectively.

  17. Comparative investigation of CuFe2O4 nano and microstructures for structural, morphological, optical and magnetic properties

    NASA Astrophysics Data System (ADS)

    Raja, G.; Gopinath, S.; Raj, R. Azhagu; Shukla, Arun K.; Alhoshan, Mansour S.; Sivakumar, K.

    2016-09-01

    CuFe2O4 nanocrystals were synthesized by the sol-gel method (SGM) and microwave method (MM) by using sucrose as a fuel. The structural, morphological, optical and magnetic properties of the products were determined and characterized in detail by X-ray diffraction (XRD), high resolution scanning electron microscopy (HR-SEM), photoluminescence (PL) spectroscopy and vibrating sample magnetometer (VSM). The XRD results confirmed the formation of cubic phase CuFe2O4. The formation of CuFe2O4 nano and microstructures were confirmed by HR-SEM. Photoluminescence emissions were determined by PL spectra, respectively. The relatively high saturation magnetization (78.22 emu/g) of CuFe2O4-MM shows that it is ferromagnetic and low saturation magnetization (35.98 emu/g) of CuFe2O4O-SGM confirms the super paramagnetic behavior.

  18. Magnetic and Magnetocaloric Properties of High-Energy Ball-Milled Nanocrystalline CeMn2Ge2 Compound

    NASA Astrophysics Data System (ADS)

    Kaya, Melike; Dincer, Ilker; Akturk, Selcuk; Elerman, Yalcin

    2016-07-01

    CeMn2Ge2 nanopowders have been obtained by high-energy ball milling for 5 and 10 hours from bulk compound to investigate the effect of milling time on magnetic and magnetocaloric properties. CeMn2Ge2 nanopowders have been characterized by X-ray diffraction (XRD), scanning electron microscopy with energy-dispersive X-ray spectroscopy, transmission electron microscopy, and magnetization measurements. The average grain size of the nanoparticles from XRD measurements is about 12.2 and 8 nm for 5-hour and 10-hour ball-milled samples, respectively. The investigations reveal that magnetic entropy change (∆S m) can be altered by changing the particle size of the compound. Maximum ∆S m is -2.45 and -1.30 J kg-1 K-1 for the 5- and 10-hour ball-milled nanopowders, respectively.

  19. 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.

  20. Structural, vibrational and magnetic properties of Ni{sub 1−x}Co{sub x}Fe{sub 2}O{sub 4} ferrites

    SciTech Connect

    Nandan, Brajesh Bhatnagar, M. C.

    2015-08-28

    The ferrite with chemical formula Ni{sub 1−x}Co{sub x}Fe{sub 2}O{sub 4} (x= 0.00, 0.50, 1.00) were prepared using sol-gel method. X-ray diffraction (XRD), Raman spectroscopy and physical property measurement system (PPMS) were used to characterize the structural, vibrational and magnetic properties. XRD pattern confirmed single crystalline spinel structure of Nickel ferrite with Co substitution. Lattice parameter variation confirms the substitution of Co{sup 2+} ions at the place of Ni{sup 2+} into the nickel ferrite. Raman scattering at room temperature is used to study the redistribution of Ni and Co cations between tetrahedral (A) and octahedral (B) sites. A shift is observed in Co substitute nickel ferrite in both XRD and Raman studies. M-H hysteresis is carried out at room temperature. Saturation magnetization of the samples is increased with the Co{sup 2+} ions substitution.

  1. 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.

  2. 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.

  3. 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.

  4. 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.

  5. 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.

  6. Ferromagnetic Resonance Studies of Magnetic Recording Media

    NASA Astrophysics Data System (ADS)

    Yu, Yuwu

    1995-01-01

    Angular dependence of maximum remanence (ADMR) and/or x-ray diffraction (XRD) techniques have been used to determine particle orientation distributions for various recording media, including gamma -rm Fe_2O_3, Co- gamma-rm Fe_2O_3, CrO_2, Ba-ferrite, and MP tapes. A distribution of column directions for metal evaporated (ME) tape has been determined from transmission electron microscopy (TEM) pictures. However, the ferromagnetic resonance (FMR) results suggest a much more narrow distribution of magnetic anisotropy directions. For Ba-ferrite tapes, the distribution functions measured by ADMR are consistent with those by XRD if interparticle interactions are accounted for. The predetermined distribution function has been used to fit FMR spectra for the above tapes. Landau-Lifshitz damping constants have been measured with high accuracy for particulate recording media. An excellent correlation has been found between the damping constants and the switching constants for these media. The results suggest that the FMR technique may be useful in predicting the switching speed of particulate recording media. The FMR technique is also useful in looking for methods of increasing the damping constant of recording media. Possible methods of increasing the switching speed of Ba-ferrite media have been studied. The reduction of Ba-ferrite particles in a hydrogen atmosphere increases the damping constant significantly. It is predicted that reduced Ba-ferrite probably switches faster than ordinary Ba-ferrite. Qualitative discussions on the origin of damping for various recording media have been presented within the framework of magnon relaxation theory. The dependence of the damping constant on magnetic properties, such as particle orientation, media coercivity, and particle interactions are also discussed.

  7. 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

  8. Effect of sol-gel pH on XRD peak broadening, lattice strain, ferroelectric domain orientation, and optical bandgap of nanocrystalline Pb1.1(Zr0.52Ti0.48)O3

    NASA Astrophysics Data System (ADS)

    Pakizeh, E.; Moradi, M.; Ahmadi, A.

    2014-02-01

    Nanocrystalline Pb1.1(Zr0.52Ti0.48)O3 (PZT) samples were prepared using a citrate-nitrate sol-gel process near the morphotropic phase boundary. The effect of pH on the lattice parameters (tetragonality and lattice constants), crystal structure [strain broadening, relative phase content, ferroelectric domain (FD) orientation and nanocrystallite size], microstructure (grain size and particle morphology) and optical bandgap was investigated. The samples were characterized using X-ray diffraction (XRD), the size strain plot (SSP) method, Fourier-transform infrared spectroscopy, and the classical Tauc relation. The particle morphology was investigated using field-emission scanning electron microscopy. The XRD results revealed a perovskite structure and coexisting tetragonal and rhombohedral phases for all PZT samples. Lattice strain and peak broadening were determined from SSP and XRD results. The behavior of these parameters was in agreement for all pH values. The optical bandgap for PZT was estimated from UV-vis absorption spectra. We found that for PZT the maximum relative tetragonal phase content, c/a ratio, and FD orientation along the a-axis occurred at pH 4.

  9. 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.

  10. One-step synthesis of magnetic chitosan polymer composite films

    NASA Astrophysics Data System (ADS)

    Cesano, Federico; Fenoglio, Gaia; Carlos, Luciano; Nisticò, Roberto

    2015-08-01

    In this study, a magnetic iron oxide-chitosan composite film is synthesized by one-step method and thoroughly investigated in order to better understand its inorganic/organic properties. A deep physico-chemical characterization of the magnetic films has been performed. In particular, the material composition was evaluated by means of XRD and ATR-FTIR spectroscopy, whereas the thermal stability and the subsequent inorganic phase transitions involving iron oxide species were followed by TGA analyses carried out at different experimental conditions (i.e. inert and oxidative atmosphere). The magnetic properties of the films were tested at the bulk and at the surface level, performing respectively magnetization hysteresis curve and magnetic force microscopy (MFM) surface mapping. Results indicate that the synthesized material can be prepared through a very simple synthetic procedure and suggests that it can be successfully applied for instance to environmental applications, such as the adsorption of contaminants from solid and liquid media thanks to its pronounced magnetic properties, which favour its recover.

  11. Cobalt nanoparticles doped emaraldine salt of polyaniline: A promising room temperature magnetic semiconductor

    NASA Astrophysics Data System (ADS)

    Hatamie, Shadie; Kulkarni, M. V.; Kulkarni, S. D.; Ningthoujam, R. S.; Vatsa, R. K.; Kale, S. N.

    2010-12-01

    Incorporation of magnetic nanoparticles in polymers with organic functional groups working as semiconducting substrate is of immense interest in the field of dilute magnetic semiconductors (DMS) and spintronics. In this article we report on synthesis and evaluation of dilutely doped (0-10 wt%) cobalt nanoparticles in emaraldine salt (ES) of polyaniline in the presence of dodecyl benzene sulfonic acid (DBSA) and p-toluene sulfonic acid (p-TSA) using a sonochemical-assisted-reduction approach as a possible DMS candidate. The X-ray diffraction pattern and high resolution transmission electron microscopy (HRTEM) image show the ES to be polycrystalline, in which 10 nm sized Co nanoparticles get embedded in its FCC structural form. From Fourier transform infrared (FT-IR) and UV-visible (UV-vis) spectroscopy studies, it is predicted that cobalt particles get electrostatically bound to the specific SO3- ion sites of ES, thereby modifying torsional degrees of freedom of the system. The applied field dependent magnetization study shows that the sample exhibits hysteresis loop with a minimal doping of 3 wt% of Co nanoparticles and increases with the amount of Co nanoparticles in ES due to dipolar interaction. The electron transport data show that with increase in Co wt% there is a gradual shift from ohmic to non-ohmic response to the sample bias, accompanied by opening of electrical hysteresis and an increased resistance. The non-linear response of higher doped systems has been attributed to the combination of direct and Fowler-Nordheim tunneling phenomena in these systems. Persistence of optical and transport properties of the polymer, with an introduction of magnetic moment in the system, envisages the system to be a fine magnetic semiconductor.

  12. 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)

  13. 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.

  14. Magnetic properties of hematite (α-Fe2O3) nanoparticles prepared by hydrothermal synthesis method

    NASA Astrophysics Data System (ADS)

    Tadic, Marin; Panjan, Matjaz; Damnjanovic, Vesna; Milosevic, Irena

    2014-11-01

    Hematite (α-Fe2O3) nanoparticles are successfully synthesized by using the hydrothermal synthesis method. An X-ray powder diffraction (XRPD) of the sample shows formation of the nanocrystalline α-Fe2O3 phase. A transmission electron microscopy (TEM) measurements show spherical morphology of the hematite nanoparticles and narrow size distribution. An average hematite nanoparticle size is estimated to be about 8 nm by TEM and XRD. Magnetic properties were measured using a superconducting quantum interference device (SQUID) magnetometry. Investigation of the magnetic properties of hematite nanoparticles showed a divergence between field-cooled (FC) and zero-field-cooled (ZFC) magnetization curves below Tirr = 103 K (irreversibility temperature). The ZFC magnetization curve showed maximum at TB = 52 K (blocking temperature). The sample did not exhibit the Morin transition. The M(H) (magnetization versus magnetic field) dependence at 300 K showed properties of superparamagnetic iron oxide nanoparticles (SPION). The M(H) data were successfully fitted by the Langevin function and magnetic moment μp = 657 μB and diameter d = 8.1 nm were determined. Furthermore, magnetic measurements showed high magnetization at room temperature (MS = 3.98 emu/g), which is desirable for application in spintronics and biomedicine. Core-shell structure of the nanoparticles was used to describe high magnetization of the hematite nanoparticles.

  15. 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.

  16. 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.

  17. Poly-l-lysine-coated magnetic nanoparticles as intracellular actuators for neural guidance

    PubMed Central

    Riggio, Cristina; Calatayud, Maria Pilar; Hoskins, Clare; Pinkernelle, Josephine; Sanz, Beatriz; Torres, Teobaldo Enrique; Ibarra, Manuel Ricardo; Wang, Lijun; Keilhoff, Gerburg; Goya, Gerardo Fabian; Raffa, Vittoria; Cuschieri, Alfred

    2012-01-01

    Purpose It has been proposed in the literature that Fe3O4 magnetic nanoparticles (MNPs) could be exploited to enhance or accelerate nerve regeneration and to provide guidance for regenerating axons. MNPs could create mechanical tension that stimulates the growth and elongation of axons. Particles suitable for this purpose should possess (1) high saturation magnetization, (2) a negligible cytotoxic profile, and (3) a high capacity to magnetize mammalian cells. Unfortunately, the materials currently available on the market do not satisfy these criteria; therefore, this work attempts to overcome these deficiencies. Methods Magnetite particles were synthesized by an oxidative hydrolysis method and characterized based on their external morphology and size distribution (high-resolution transmission electron microscopy [HR-TEM]) as well as their colloidal (Z potential) and magnetic properties (Superconducting QUantum Interference Devices [SQUID]). Cell viability was assessed via Trypan blue dye exclusion assay, cell doubling time, and MTT cell proliferation assay and reactive oxygen species production. Particle uptake was monitored via Prussian blue staining, intracellular iron content quantification via a ferrozine-based assay, and direct visualization by dual-beam (focused ion beam/scanning electron microscopy [FIB/SEM]) analysis. Experiments were performed on human neuroblastoma SH-SY5Y cell line and primary Schwann cell cultures of the peripheral nervous system. Results This paper reports on the synthesis and characterization of polymer-coated magnetic Fe3O4 nanoparticles with an average diameter of 73 ± 6 nm that are designed as magnetic actuators for neural guidance. The cells were able to incorporate quantities of iron up to 2 pg/cell. The intracellular distribution of MNPs obtained by optical and electronic microscopy showed large structures of MNPs crossing the cell membrane into the cytoplasm, thus rendering them suitable for magnetic manipulation by external

  18. Magnetic-flux pump

    NASA Technical Reports Server (NTRS)

    Hildebrandt, A. F.; Elleman, D. D.; Whitmore, F. C. (Inventor)

    1966-01-01

    A magnetic flux pump is described for increasing the intensity of a magnetic field by transferring flux from one location to the magnetic field. The device includes a pair of communicating cavities formed in a block of superconducting material, and a piston for displacing the trapped magnetic flux into the secondary cavity producing a field having an intense flux density.

  19. Magnetic multilayer structure

    DOEpatents

    Herget, Philipp; O'Sullivan, Eugene J.; Romankiw, Lubomyr T.; Wang, Naigang; Webb, Bucknell C.

    2016-07-05

    A mechanism is provided for an integrated laminated magnetic device. A substrate and a multilayer stack structure form the device. The multilayer stack structure includes alternating magnetic layers and diode structures formed on the substrate. Each magnetic layer in the multilayer stack structure is separated from another magnetic layer in the multilayer stack structure by a diode structure.

  20. 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.

  1. Contactless Magnetic Slip Ring

    NASA Technical Reports Server (NTRS)

    Kumagai, Hiroyuki (Inventor); Deardon, Joe D. (Inventor)

    1997-01-01

    A contactless magnetic slip ring is disclosed having a primary coil and a secondary coil. The primary and secondary coils are preferably magnetically coupled together, in a highly reliable efficient manner, by a magnetic layered core. One of the secondary and primary coils is rotatable and the contactless magnetic slip ring provides a substantially constant output.

  2. 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…

  3. 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

  4. Linear magnetic bearing

    NASA Technical Reports Server (NTRS)

    Studer, P. A. (Inventor)

    1983-01-01

    A linear magnetic bearing system having electromagnetic vernier flux paths in shunt relation with permanent magnets, so that the vernier flux does not traverse the permanent magnet, is described. Novelty is believed to reside in providing a linear magnetic bearing having electromagnetic flux paths that bypass high reluctance permanent magnets. Particular novelty is believed to reside in providing a linear magnetic bearing with a pair of axially spaced elements having electromagnets for establishing vernier x and y axis control. The magnetic bearing system has possible use in connection with a long life reciprocating cryogenic refrigerator that may be used on the space shuttle.

  5. 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.

  6. 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

  7. 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.

  8. Stacked magnet superconducting bearing

    SciTech Connect

    Rigney, T.K. II; Saville, M.P.

    1993-06-15

    A superconducting bearing is described, comprising: a plurality of permanent magnets magnetized end-to-end and stacked side-by-side in alternating polarity, such that flux lines flow between ends of adjacent magnets; isolating means, disposed between said adjacent magnets, for reducing flux leakage between opposing sides of said adjacent magnets; and a member made of superconducting material having at least one surface in communication with said flux lines.

  9. 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.

  10. Facility Measures Magnetic Fields

    NASA Technical Reports Server (NTRS)

    Honess, Shawn B.; Narvaez, Pablo; Mcauley, James M.

    1991-01-01

    Partly automated facility measures and computes steady near magnetic field produced by object. Designed to determine magnetic fields of equipment to be installed on spacecraft including sensitive magnetometers, with view toward application of compensating fields to reduce interfernece with spacecraft-magnetometer readings. Because of its convenient operating features and sensitivity of its measurements, facility serves as prototype for similar facilities devoted to magnetic characterization of medical equipment, magnets for high-energy particle accelerators, and magnetic materials.

  11. 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.

  12. 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.

  13. Ferromagnetism in diluted magnetic Zn-Co-doped CeO2-δ

    NASA Astrophysics Data System (ADS)

    Santos, T. S.; Folly, W. S. D.; Macêdo, M. A.

    2012-08-01

    Several oxides doped with transition metals can be used in spintronics devices due to their conductive and magnetic properties at room temperature. In this work, samples of Ce1-2xZnxCoxO2-δ were obtained by an alternative sol-gel proteic process for x=0.01, 0.05 and 0.1. The structural properties of samples were analyzed by XRD and Raman spectroscopy. Magnetization measurements revealed a ferromagnetic behavior at room temperature probably induced by oxygen vacancies.

  14. Magnetic properties of Ni/NiO nanocomposites synthesized by one step solution combustion method

    NASA Astrophysics Data System (ADS)

    Ganeshchandra Prabhu, V.; Shajira, P. S.; Lakshmi, N.; Junaid Bushiri, M.

    2015-12-01

    Ni/NiO nanocomposites were synthesized using solution combustion method and characterized with X-ray diffraction (XRD), transmission electron microscopy (TEM), selected area electron diffraction (SAED), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDAX) and carbon, hydrogen, nitrogen (CHN) analyser. The Ni or NiO content in Ni/NiO nanocomposites vary with the quantity of HNO3 used for the synthesis. Magnetic coercivity (Hc) of Ni/NiO nanocomposites is found to be 413 Oe which can be used in magnetic applications. A feeble exchange bias of 7 Oe is seen from the NiO rich Ni/NiO.

  15. 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.

  16. 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.

  17. Structural and magnetic properties of Vanadium Doped M- Type Barium Hexaferrite (BaFe12-xVxO19)

    NASA Astrophysics Data System (ADS)

    Awadallah, Ahmad; Mahmood, Sami H.; Maswadeh, Yazan; Bsoul, Ibrahim; Aloqaily, Aynour

    2015-10-01

    Precursor powders of barium hexaferrite doped with vanadium, BaFe12-xVxO19 with (x = 0.1, 0.2, 0.3, 0.4, 0.5), were prepared using the ball milling technique and then sintered at different temperatures for 2 h. The structural properties of the prepared samples were investigated by X-ray diffraction (XRD) and scanning electron microscopy (SEM), while the magnetic properties were examined by the vibrating sample magnetometry (VSM). XRD and SEM studies of the samples sintered at 1100° C indicated the presence of Ba3V2O8 and α-Fe2O3 non-magnetic oxide phases in addition to BaM hexaferrite phase. The fractions of the nonmagnetic oxide phases were found to increase with increasing x, and sintering the samples at temperatures higher than 1100° C was found to reduce the amounts of these non-magnetic phases only slightly. However, the addition of barium in excess of the stoichiometric ratio was found to remove the α-Fe2O3 oxide, and improve the saturation magnetization of the samples significantly. In addition, washing these samples with HCl was found to improve the saturation magnetization further. The effect of sintering the samples at higher temperatures was also found to reduce the coercivity due to growth of the particle size. However, the coercivity of all samples remained high enough for potential permanent magnet and magnetic recording applications.

  18. Magnetic novae

    NASA Astrophysics Data System (ADS)

    Zemko, Polina; Orio, Marina

    2016-07-01

    We present the results of optical and X-ray observations of two quiescent novae, V2491 Cyg and V4743 Sgr. Our observations suggest the intriguing possibility of localization of hydrogen burning in magnetic novae, in which accretion is streamed to the polar caps. V2491 Cyg was observed with Suzaku more than 2 years after the outburst and V4743 Sgr was observed with XMM Newton 2 and 3.5 years after maximum. In the framework of a monitoring program of novae previously observed as super soft X-ray sources we also obtained optical spectra of V4743 Sgr with the SALT telescope 11.5 years after the eruption and of V2491 Cyg with the 6m Big Azimutal Telescope 4 and 7 years post-outburst. In order to confirm the possible white dwarf spin period of V2491 Cyg measured in the Suzaku observations we obtained photometric data using the 90cm WIYN telescope at Kitt Peak and the 1.2 m telescope in Crimea. We found that V4743 Sgr is an intermediate polar (IP) and V2491 Cyg is a strong IP candidate. Both novae show modulation of their X-ray light curves and have X-ray spectra typical of IPs. The Suzaku and XMM Newton exposures revealed that the spectra of both novae have a very soft blackbody-like component with a temperature close to that of the hydrogen burning white dwarfs in their SSS phases, but with flux by at least two orders of magnitude lower, implying a possible shrinking of emitting regions in the thin atmosphere that is heated by nuclear burning underneath it. In quiescent IPs, independently of the burning, an ultrasoft X-ray flux component originates at times in the polar regions irradiated by the accretion column, but the soft component of V4743 Sgr disappeared in 2006, indicating that the origin may be different from accretion. We suggest it may have been due to an atmospheric temperature gradient on the white dwarf surface, or to continuing localized thermonuclear burning at the bottom of the envelope, before complete turn-off. The optical spectra of V2491 Cyg and V

  19. 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.

  20. 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.

  1. 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.

  2. 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.

  3. The effects of size and orientation on magnetic properties and exchange bias in Co3O4 mesoporous nanowires

    NASA Astrophysics Data System (ADS)

    Zeng, R.; Wang, J. Q.; Chen, Z. X.; Li, W. X.; Dou, S. X.

    2011-04-01

    Co3O4 mesoporous nanowires with average single crystalline grain sizes of about 8 nm, 12nm, 25 nm, and 45 nm were synthesized by sintering of microwave-assisted hydrothermal processed belt-Co(OH)2 precursors at 300-500 °C for 2 h. Microstructure analysis was conducted by x-ray diffraction, x-ray photoelectron spectroscopy, Raman spectroscopy, scanning electron microscopy (SEM), field emission SEM (FESEM), transmission electron microscopy (TEM), and high resolution TEM (HRTEM) to confirm the composition, structure, and orientation in the nanowires. Systematic magnetic measurements have also been conducted on the nanowires. It was found that the size and orientation have significant effects on the magnetic and exchange bias properties. The interesting finding was made that room temperature ferromagnetism appeared at 350 °C in the high orientation samples. Systematic comparison and analysis of the relationships among the grain size, microstructure, orientation (texture), surface electric structure (O vacancies), and defects with magnetic properties (ferromagnetism, coercive field, exchange bias, etc.) are presented in this work.

  4. 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.

  5. 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

  6. 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.

  7. 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.

  8. Large gap magnetic suspension system

    NASA Technical Reports Server (NTRS)

    Abdelsalam, Moustafa K.; Eyssa, Y. M.

    1991-01-01

    The design of a large gap magnetic suspension system is discussed. Some of the topics covered include: the system configuration, permanent magnet material, levitation magnet system, superconducting magnets, resistive magnets, superconducting levitation coils, resistive levitation coils, levitation magnet system, and the nitrogen cooled magnet system.

  9. Multifunctionality in molecular magnetism.

    PubMed

    Pinkowicz, Dawid; Czarnecki, Bernard; Reczyński, Mateusz; Arczyński, Mirosław

    2015-01-01

    Molecular magnetism draws from the fundamental ideas of structural chemistry and combines them with experimental physics resulting in one of the highest profile current topics, namely molecular materials that exhibit multifunctionality. Recent advances in the design of new generations of multifunctional molecular magnets that retain the functions of the building blocks and exhibit non-trivial magnetic properties at higher temperatures provide promising evidence that they may be useful for the future construction of nanoscale devices. This article is not a complete review but is rather an introduction into thefascinating world of multifunctional solids with magnetism as the leitmotif. We provide a subjective selection and discussion of the most inspiring examples of multifunctional molecular magnets: magnetic sponges, guest-responsive magnets, molecular magnets with ionic conductivity, photomagnets and non-centrosymmetric and chiral magnets.

  10. Magnetic infrasound sensor

    DOEpatents

    Mueller, Fred M.; Bronisz, Lawrence; Grube, Holger; Nelson, David C.; Mace, Jonathan L.

    2006-11-14

    A magnetic infrasound sensor is produced by constraining a permanent magnet inside a magnetic potential well above the surface of superconducting material. The magnetic infrasound sensor measures the position or movement of the permanent magnet within the magnetic potential well, and interprets the measurements. Infrasound sources can be located and characterized by combining the measurements from one or more infrasound sensors. The magnetic infrasound sensor can be tuned to match infrasound source types, resulting in better signal-to-noise ratio. The present invention can operate in frequency modulation mode to improve sensitivity and signal-to-noise ratio. In an alternate construction, the superconductor can be levitated over a magnet or magnets. The system can also be driven, so that time resolved perturbations are sensed, resulting in a frequency modulation version with improved sensitivity and signal-to-noise ratio.

  11. Magnetic balltracking: Tracking the photospheric magnetic flux

    NASA Astrophysics Data System (ADS)

    Attie, R.; Innes, D. E.

    2015-02-01

    Context. One aspect of understanding the dynamics of the quiet Sun is to quantify the evolution of the flux within small-scale magnetic features. These features are routinely observed in the quiet photosphere and were given various names, such as pores, knots, magnetic patches. Aims: This work presents a new algorithm for tracking the evolution of the broad variety of small-scale magnetic features in the photosphere, with a precision equal to the instrumental resolution. Methods: We have developed a new technique to track the evolution of the individual magnetic features from magnetograms, called "magnetic balltracking". It quantifies the flux of the tracked features, and it can track the footpoints of magnetic field lines inferred from magnetic field extrapolation. The algorithm can detect and quantify flux emergence, as well as flux cancellation. Results: The capabilities of magnetic balltracking are demonstrated with the detection and the tracking of two cases of magnetic flux emergence that lead to the brightening of X-ray loops. The maximum emerged flux ranges from 1018 Mx to 1019 Mx (unsigned flux) when the X-ray loops are observed. Movies associated to Figs. 6 and 18 are available in electronic form at http://www.aanda.org

  12. 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.

  13. Vehicle with magnetic engine

    SciTech Connect

    Wortham, C.

    1993-06-15

    A vehicle is described comprising a vehicle frame fitted with axles and wheels rotatably carried by the axles; an engine block mounted on the frame; a plurality of magnetic cylinders provided in the engine block and a plurality of magnetic pistons disposed in the magnetic cylinders, respectively, in reciprocating relationship, the magnetic cylinders having a first magnetic polarity in one end and a second magnetic polarity in the opposite end for alternately attracting and repelling the magnetic pistons, respectively; a crankshaft journalled for rotation in the engine block; power transmission means connecting the crankshaft to at least one of the axles in driving relationship; and connecting rods connecting the crankshaft to the magnetic pistons, respectively, whereby reciprocation of the magnetic pistons in the magnetic cylinders effects rotation of the crankshaft; a cylinder head provided on the engine block and piston electromagnetic means provided in the cylinder head above the magnetic cylinders and the magnetic pistons, respectively for alternately attracting and repelling the magnetic pistons; at least one battery carried by the frame; and polarity timing means electrically connected to the battery and the piston electromagnetic means, for alternating the polarity of the piston electromagnet means, whereby electric current is supplied to the piston electromagnetic means in current-reversing relationship to alternately attract and repel the magnetic pistons in reciprocating relationship responsive to operation of the polarity timing means.

  14. Optimization of magnetic powdered activated carbon for aqueous Hg(II) removal and magnetic recovery.

    PubMed

    Faulconer, Emily K; von Reitzenstein, Natalia V Hoogesteijn; Mazyck, David W

    2012-01-15

    Activated carbon is known to adsorb aqueous Hg(II). MPAC (magnetic powdered activated carbon) has the potential to remove aqueous Hg to less than 0.2 μg/L while being magnetically recoverable. Magnetic recapture allows simple sorbent separation from the waste stream while an isolated waste potentially allows for mercury recycling. MPAC Hg-removal performance is verified by mercury mass balance, calculated by quantifying adsorbed, volatilized, and residual aqueous mercury. The batch reactor contained a sealed mercury-carbon contact chamber with mixing and constant N(2) (g) headspace flow to an oxidizing trap. Mercury adsorption was performed using spiked ultrapure water (100 μg/L Hg). Mercury concentrations were obtained using EPA method 245.1 and cold vapor atomic absorption spectroscopy. MPAC synthesis was optimized for Hg removal and sorbent recovery according to the variables: C:Fe, thermal oxidation temperature and time. The 3:1 C:Fe preserved most of the original sorbent surface area. As indicated by XRD patterns, thermal oxidation reduced the amorphous characteristic of the iron oxides but did not improve sorbent recovery and damaged porosity at higher oxidation temperatures. Therefore, the optimal synthesis variables, 3:1 C:Fe mass ratio without thermal oxidation, which can achieve 92.5% (± 8.3%) sorbent recovery and 96.3% (± 9%) Hg removal. The mass balance has been closed to within approximately ± 15%. PMID:22104766

  15. 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

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

    PubMed

    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⁡(C o /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

  17. Lattice strain induced magnetism in substituted nanocrystalline cobalt ferrite

    NASA Astrophysics Data System (ADS)

    Kumar, Rajnish; Kar, Manoranjan

    2016-10-01

    Strontium (Sr) substituted cobalt ferrite i.e. Co1-xSrxFe2O4 (x=0.00, 0.01, 0.015, 0.02, 0.05, 0.1) have been synthesized by the citric acid modified sol-gel method. Crystal structure and phase purity have been studied by the X-ray powder diffraction technique. The Rietveld refinement of XRD pattern using the space group Fd 3 bar m shows monotonically increasing of lattice parameter with the increase in Sr concentration. Magnetic hysteresis loops measurement has been carried out at room temperature using a vibrating sample magnetometer (VSM) over a field range of ±1.5 T. Magnetocrystalline anisotropy constant were calculated by employing the Law of Approach (LA) to the saturation. It is observed that magnetocrystalline anisotropy has anomaly for x=0.01 (Co0.99Sr0.01Fe2O4) sample. Strain mediated modification of magnetic properties in Sr substituted cobalt ferrite has been observed. The saturation magnetization for doping concentration i.e. x=0.01 abruptly increase while for x>0.01 decreases with the increase in Sr concentration. A correlation between lattice strain and magnetic behavior in non-magnetic Sr- substituted nano-crystalline cobalt ferrite has been reported.

  18. Magnetic and Ferroelectric Anisotropy in Multiferroic FeVO4

    NASA Astrophysics Data System (ADS)

    Abdelhamid, Ehab; Dixit, Ambesh; Kimura, Kenta; Kimura, Tsuyoshi; Jayakumar, Onattu; Naik, Vaman; Naik, Ratna; Lawes, Gavin; Nadgorny, Boris

    FeVO4 has been studied as a model system for understanding the magnetoelectric interaction mechanisms in low symmetry multiferroics. Triclinic FeVO4 is characterized by two antiferromagnetic phase transitions, occurring at TN 1 = 22 K and TN 2 = 15 K, with the latter transition signaling a break in the space inversion symmetry, accompanied by the development of a non-collinear magnetic order which induces ferroelectricity. Earlier measurements on polycrystalline FeVO4 doped with magnetic (Cr and Mn) as well as non magnetic (Zn) dopants indicate the stability of the two antiferromagnetic transition temperatures. In this work, single crystals of both undoped and doped FeVO4 were grown from flux. To track the changes in lattice parameters induced by changing the doping concentration (measured by EDAX), XRD and Raman spectra were obtained. By recording the magnetization along two different crystal orientations, we were able to confirm the easy magnetic axis in this structure. Finally, we obtain the crystal's ferroelectric polarization along two different directions in an attempt to further understand the mechanism responsible for the ferroelectric transition. This work is supported by the NSF under DMR-1306449.

  19. 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%.

  20. 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.