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Wyniki wyszukiwania dla: synchrotron powder diffraction
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Measuring radioactive powder samples on the highresolution powder diffraction beamline at the European Synchrotron Radiation Facility
PublikacjaThis laboratory note describes a new sample preparation technique to enable high-resolution powder diffraction experiments at the European Synchrotron Radiation Facility on radioactive samples. The sample preparation involves setting the active material in resin and several layers of encapsulation suitable for measurement at the beamline. This has allowed low-temperature measurements on very small quantities of samples, providing...
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Measuring radioactive powder samples on the high-resolution powder diffraction beamline at the European Synchrotron Radiation Facility
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Electric and magnetic properties of Lanthanum Barium Cobaltite
PublikacjaThe cubic Ba0.5La0.5CoO3‐δ was synthesized using solid state reaction. The structural properties were determined by the simultaneous refinement of Synchrotron Powder X‐ray Diffraction and Neutron Powder Diffraction data. Iodometric titration was used to examine the oxygen stoichiometry and average cobalt oxidation state. Low‐temperature magnetic studies show soft ferromagnetic character of fully oxidized material, with θP = 198(3)...
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High-Temperature Structural and Electrical Properties of BaLnCo2O6 Positrodes
PublikacjaThe application of double perovskite cobaltites BaLnCo2O6−δ (Ln = lanthanide element) in electrochemical devices for energy conversion requires control of their properties at operating conditions. This work presents a study of a series of BaLnCo2O6−δ (Ln = La, Pr, Nd) with a focus on the evolution of structural and electrical properties with temperature. Symmetry, oxygen non-stoichiometry, and cobalt valence state have been examined...
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Structure and water uptake in BaLnCo2O6−δ (Ln =La, Pr, Nd, Sm, Gd, Tb and Dy)
PublikacjaThe structure of BaLnCo2O6-δ (Ln =La, Pr, Nd, Sm, Gd, Tb and Dy) was studied by the means of synchrotron radiation powder X-ray diffraction, neutron powder diffraction and Transmission Electron Microscopy (TEM), while water uptake properties were analysed with the use of thermogravimetry (TG) and water adsorption isotherms. The structure refinement revealed that the dominant phase in all compositions was orthorhombic with an ordering...
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Structure and paramagnetism in weakly correlated Y8Co5
PublikacjaWe report the basic physical properties of monoclinic Y8Co5 determined by means of magnetic susceptibility, electrical resistivity, and specific heat measurements. The crystal structure of Y8Co5 is monoclinic (P21/c) with lattice parameters a = 7.0582(6) Å, b = 7.2894(6) Å, c = 24.2234(19) Å, and β = 102.112(6)° as refined by using synchrotron powder x-ray diffraction data. The compound shows temperature independent paramagnetism...
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Potential Skyrmion Host Fe(IO3)3: Connecting Stereoactive Lone-Pair Electron Effects to the Dzyaloshinskii-Moriya Interaction
PublikacjaMagnetic skyrmions, which are topologically distinct magnetic spin textures, are gaining increased attention for their unique physical properties and potential applications in spintronic devices. Here we present a design strategy for skyrmion host candidates based on combinations of magnetic spin, asymmetric building units having stereoactive lone-pair electrons, and polar lattice symmetry. To demonstrate the viability of the proposed...
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Spin and Orbital Effects on Asymmetric Exchange Interaction in Polar Magnets: M(IO3)2 (M = Cu and Mn)
PublikacjaMagnetic polar materials feature an astonishing range of physical properties, such as magnetoelectric coupling, chiral spin textures, and related new spin topology physics. This is primarily attributable to their lack of space inversion symmetry in conjunction with unpaired electrons, potentially facilitating an asymmetric Dzyaloshinskii–Moriya (DM) exchange interaction supported by spin–orbital and electron–lattice coupling. However,...
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X-RAY DIFFRACTION STUDY OF BISMUTH LAYER-STRUCTURED MULTIFERROIC CERAMICS
PublikacjaGoal of the present research was to apply a solid state reaction route to fabricate bismuth layer-structured multiferroic ceramics described with the formula Bi5FeTi3O15 and reveal the influence of processing conditions on its crystal structure and phase composition. Simple oxide powders Bi2O3, TiO2 and Fe2O3 were used to fabricate Aurivillius-type bismuth layer-structured ferroelectrics. Pressureless sintering in ambient air was...
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Synthesis, characterization and Luminescent Properties of New Coordination Polymers Based on p-tert Butylcalix[4]arene-tetracarboxylic acid and Lanthanine cations
PublikacjaA series of new coordination polymers based on p-tert-butylcalix[4]arene-tetracarboxylic acid with Eu3+, Tb3+wrer prepared by hydro and solvothermal methods. the obtained solid compounds were characterized by infrared and luminescence spectroscopy, powder X-ray diffraction, scianning electron microscopy and thermogravimetric anylisis. The infrared curves and the x-ray diffraction patterns indicate that the same crystalline structure...
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Synthesis and structure of Bi 5 FeTi 3 O 15 ceramics
PublikacjaAim of the present research was to fabricate and study crystal structure and phase composition of Bi5FeTi3O15 (BTFO) ceramics exhibiting Aurivillius - type structure. By means of simultaneous thermal analysis and X-ray diffraction analysis the process of synthesis of BTFO ceramics has been studied. Mixed oxide method followed by pressureless sintering was used for ceramics preparation. Three endothermic thermal effects have been...
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Study of the atomic structure and morphology of the Pt3Co nanocatalyst
PublikacjaThe local structure and chemical disorder of a commercially available Pt3Co nanocatalyst supported on high surface area carbon were investigated. High-quality XAFS spectra were collected at the ELETTRA synchrotron XAFS 11.1 beamline. XAFS spectra analysis have been performed accounting for the reduction of the coordination number and degeneracy of three-body configurations, resulting from transmission electron microscopy (TEM)...
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Spin-glass behavior in a binary Pr 3 Ir intermetallic compound
PublikacjaPolycrystalline Pr3Ir was synthesized by arc melting. Its cementite-type crystal structure (Pnma) was confirmed by powder X-ray diffraction and estimated lattice parameters are in agreement with literature. Physical properties were measured by means of the ac and dc magnetic susceptibility, electrical resistivity and heat capacity. Our results indicate spin-glass behavior in Pr3Ir with a freezing temperature Tf = 6.58 K and activation...
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Stabilization of the pyrochlore phase of Mn2Sb2O7 by double substitution
PublikacjaPolycrystalline samples of (Ce4+Mn2+3)(Ga3+Sb5+3)O14 were synthesized by a high-temperature solid-state reaction. In contrast with the parent Mn2Sb2O7 compound that adopts a rhombohedral or monoclinic structure at T > 600 °C, the pyrochlore structure of CeMn3GaSb3O14 is retained up to at least T = 1070°C. High-resolution synchrotron x-ray diffraction measurements show no sign of a superstructure or distortion from cubic symmetry...
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Formation of intermetallic compounds in the solid-liquid composites of the Ga-Ni system
PublikacjaThe processes of formation of intermetallic compounds in the composite system of liquid gallium-nickel powder by the methods of x-ray diffraction, scanning electron microscopy and differential thermal analysis have been studied. A change in the phase composition was discovered and the influence of thermal treatment of the composites under investigation on the phase formation processes was analyzed. The mechanism of gallium enriched...
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Investigation of magnetic order in a new intermetallic compound Nd2PtGe3
PublikacjaIn the present study we report a successful synthesis of the new intermetallic compound Nd2PtGe3 by an arc-melting method. The powder X-ray diffraction analysis indicates that this compound crystallizes in an disordered variant of the AlB2-type structure (space group P6/mmm, no. 191) with lattice parameters a = 4.2455 Å and c = 4. 1933 Å. The compound exhibits a cluster-glass transition below Tf = 2.9 K, characterized through ac...
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High resolution X-ray diffractometry and reflectometry of semiconductor nano- and micro- structures based on X-ray refractive optics
PublikacjaIn this thesis proposed, discussed and studied novel synchrotron X-ray diffractometry and reflectometry methods based on a refractive optics. The experimental results obtained from the ID06 beamline at ESRF, Grenoble, France are presented and analyzed in this work to demonstrate a high angular and space resolution in addition to the opportunity to manage in situ and on operando experiments with the help of proposed X-ray optical...
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Precipitation of Spherical Vaterite Particles via Carbonation Route in the Bubble Column and the Gas-Lift Reactor
PublikacjaSpherical vaterite particles were produced by carbonation of calcium chloride solution with addition of ammonia to facilitate CO2 absorption. Synthesis of calcium carbonate was carried out in a bubble column or gas-lift reactor. The course of the reaction was monitored by pH measurements. Precipitated solids were analyzed by Fourier-transformed infrared spectroscopy, x-ray powder diffraction and scanning electron microscopy, and...
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Evolution of charge density wave order in continuous solid solutions Lu(Ni1-xCox)C2
PublikacjaPseudo-ternary solid solutions, Lu(Ni1-xCox)C2 (0 ≤ x ≤ 1), were studied by means of powder X-ray diffraction, differential thermal analysis as well as electrical resistivity and heat capacity measurements. The crystal structure of the Lu(Ni1-xCox)C2 series, as investigated by means of X-ray powder diffraction, is of structure type CeNiC2, space group Amm2, Pearson symbol oS8. The structural analysis reveals a non-monotonous evolution,...
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KTaO3-based nanocomposites for air treatment
PublikacjaA series of single semiconductors and their nanocomposites combination (such as KTaO3 + CdSe + SrTiO3; KTaO3 + CdS +WO3; KTaO3 + CdS + MoS2) were prepared using hydrothermal route. Photocatalytic activity of as-prepared nanocomposites was estimated by photocatalytic degradation of toluene in the gas phase using light-emitting diodes (LEDs, 375 nm) in four subsequent cycles. The nanocomposites were characterized by scanning electron...
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The electronic characterization of the cubic Laves-phase superconductor CaRh2
PublikacjaWe present the synthesis and experimental characterization of the electronic properties of the cubic Laves phase superconductor CaRh2. Its crystal structure was confirmed by powder X-ray diffraction and its ambient temperature lattice parameter (a = 7.5326(6) Å) is in good agreement with the literature. Magnetization, resistivity and heat-capacity measurements indicate that CaRh2 is a moderate-coupling type-II superconductor (λe-p = 0.89)...
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Impact of low-temperature sintering on the Fe-based amorphous coatings
PublikacjaBulk metallic glasses (BMGs) have gained a lot of attention in recent years due to their outstanding properties such as high hardness and excellent wear and corrosion resistance. However, they are restricted in industrial applications due to their extreme brittleness. Iron based amorphous coatings from BMGs are the best solution to use them by overcoming the problem of extreme brittleness. The coatings can be sprayed by various...
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Evolution of Physical Properties of RE 3 Ni 5 Al 19 Family (RE = Y, Nd, Sm, Gd, Tb, Dy, Ho, and Er)
PublikacjaSingle crystals of RE3Ni5Al19 series (RE = Y, Nd, Sm, Gd, Tb, Dy, Ho, and Er) are grown using the Al self-flux method. The crystal structure is examined by both single crystal and powder X-ray diffraction. Physical properties are studied for the first time for RE3Ni5Al19 (RE = Y, Nd, Gd, Tb, Dy, Ho, and Er) by means of magnetic susceptibility, electrical resistivity, and heat capacity measurements. Complex magnetic behaviors, with...
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Solvothermal synthesis and structural characterization of three polyoxotitanium-organic acid clusters
PublikacjaThree new titanium oxo-clusters Ti4O2(OiPr)10(OOCPhMe)2 (I), Ti6O4(OEt)8(OOCPhMe)8 (II) and Ti6O6(OEt)6(OOCCHPh2)6 (III) were obtained by easy one-step solvothermal reactions of titanium(IV) isopropoxide, alcohols and carboxylic acids. The three compounds were characterized by single-crystal and powder X-ray diffraction, TGA/DSC, optical and electron microscopy, and FTIR and NMR spectroscopy. X-ray powder diffraction and spectroscopy...
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Crystal structure and low-energy Einstein mode in ErV2Al20 intermetallic cage compound
PublikacjaSingle crystals of a new ternary aluminide ErV2Al20 were grown using a self-flux method. The crystal structure was determined by powder X-ray diffraction measurements and Rietveld refinement, and physical properties were studied by means of electrical resistivity, magnetic susceptibility and specific heat measurements. These measurements reveal that ErV2Al20 is a Curie-Weiss paramagnet down to 1.95 K with an effective magnetic...
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Pr-doped TiO2: The effect of metal content on photocatalytic activity
PublikacjaThe Pr-TiO2 nanoparticles were prepared by using the sol-gel method. As-prepared samples were characterized by BET measurements, X-ray powder diffraction analysis (XRD) and UV-Vis spectra. Visible and ultraviolet light photocatalytic activity of the sample was studied by photodegradation of phenol while considering the influence of the dopant concentration. TiO2 doped with 0.25 mol% of praseodymium showed the highest photocatalytic...
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Synthesis, structure and physical properties of new intermetallic spin glass-like compounds RE2PdGe3 (RE = Tb and Dy)
PublikacjaNew intermetallic compounds Tb2Pd1.25Ge2.75 and Dy2Pd1.25Ge2.75 have been synthesized using the arc-melting method. The crystallographic structure and magnetic, electronic transport, and thermal properties are reported. The crystal structure obtained from powder x-ray diffraction analysis suggests that these compounds crystallize in the AlB2-type structure (space group P6/mmm, no. 191) with lattice parameters a = 4.228 53(5)/4.230 54...
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New heterometallic Co/Zn, Ag/Co, and Ag/Zn imidazolates: structural characterization and catalytic activity in the oxidation of organic compounds
PublikacjaNanocrystalline powders of monometallic and bimetallic imidazolates of Co, Zn, and Ag were produced by a reaction carried out in water. The powders were characterized by powder X-ray diffraction and the crystal structures of new compounds Ag2ZnIm4 and Ag2CoIm4 (Im = imidazolate) were solved. Heterometallic Co/Zn imidazolates showed the standard ZIF-8 crystal structure while Ag/Zn and Ag/Co systems were isostructural with the copper...
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Synthesis, single crystal growth and properties of Sr5Pb3ZnO12
PublikacjaAbstract The novel Sr5Pb3ZnO12 oxide was synthesized by the solid-state reaction method. The crystal structure was studied by means of the powder x-ray diffraction Rietveld method and was found to be similar to 3 other previously known Sr5Pb3MO12 compounds (M = Co, Ni, Cu). Crystals of several hundred microns in size of the new phase were grown in molten sodium chloride and imaged using confocal optical and scanning electron microscopy....
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Fibrillar aggregates in powdered milk
PublikacjaThis research paper addresses the hypothesis that powdered milk may contain amyloid fibrils. Amyloids are fibrillar aggregates of proteins. Up to this time, research on the presence of amyloids in food products are scarce. To check the hypothesis we performed thioflavin T fluorescence assay, X-ray powder diffraction, atomic force microscopy and fluorescence microscopy imaging. Our preliminary results show that commercially available...
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Fabrication of Bi6Fe2Ti3O18 Ceramics by Mixed Oxide Method
PublikacjaIn the present study Bi6Fe2Ti3O18 (BFTO) ceramics has been fabricated by solid state reaction from the mixture of simple oxides viz. Bi2O3, TiO2 and Fe2O3. Stoichiometric mixture of the powders was thermally analyzed so parameters of the thermal treatment were determined. The EDS measurements have shown conservation of the chemical composition of the ceramic powder after calcination. Hot-pressing method was used for final densification...
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Intermetallic disordered magnet Gd2Pt1.1Ge2.9 and its relation to other AlB2 -type compounds
PublikacjaThe intermetallic germanide Gd 2 Pt 1.1 Ge 2.9 was synthesized using an arc-melting method. The crystal structure was characterized using powder x-ray diffraction, revealing a disordered ternary AlB 2 -type structure (space group P 6 / m m m , No. 191) with lattice parameters a = 4.2092 ( 1 ) Å and c = 4.0546 ( 2 ) Å . Physical properties were investigated by magnetic susceptibility and heat capacity measurements, which...
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Utilization of oriented crystal growth for screening of aromatic carboxylic acids cocrystallization with urea
PublikacjaThe possibility of molecular complex formation in the solid state of urea with benzoic acid analogues was measured directly on the crystallite films deposited on the glass surface using powder X-ray diffractometry (PXRD). Obtained solid mixtures were also analyzed using Fourier transform infrared spectroscopy (FTIR). The simple droplet evaporation method was found to be efficient, robust, fast and cost-preserving approach for first...
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Hydrothermal reactions: From the synthesis of ligand to new lanthanide 3D-coordination polymers
PublikacjaThe organic ligand 2,5-piperazinedione-1,4-diaceticacid (H2PDA) was synthesized under hydrothermal conditions starting from the iminodiacetic acid and catalyzed by oxalic acid. The X-ray powder diffraction data indicates that the compound crystallizes in the P21/c space group as reported in the literature. The ligand was also characterized by elemental analysis, magnetic nuclear resonance, infrared spectroscopy and thermogravimetric...
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Concentration‐Induced Hetero‐Valent Partial‐Inverse Occupation of Infrared Phosphor
PublikacjaInfrared luminescent materials have evoked much attention from chemists and material scientists. Although substantial progress is made in materials design, the luminescent mechanism remains ambiguous in the complex structures, presenting major barriers to developing novel infrared luminescent materials. Herein, this study aims to deliberate a complete discussion on infrared phosphors with concentration-induced hetero-valent partial-inverse...
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On the origin of surface imposed anisotropic growth of salicylic and acetylsalicylic acids crystals during droplet evaporation
PublikacjaIn this paper droplet evaporative crystallization of salicylic acid (SA) and acetylsalicylic acid (ASA) crystals on different surfaces, such as glass, polyvinyl alcohol (PVA), and paraffin was studied. The obtained crystals were analyzed using powder X-ray diffraction (PXRD) technique. In order to better understand the effect of the surface on evaporative crystallization, crystals deposited on glass were scraped off. Moreover,...
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Propensity of salicylamide and ethenzamide cocrystallization with aromatic carboxylic acids
PublikacjaThe cocrystallization of salicylamide (2-hydroxybenzamide, SMD) and ethenzamide (2-ethoxybenzamide, EMD) with aromatic carboxylic acids was examined both experimentally and theoretically. The supramolecular synthesis taking advantage of the droplet evaporative crystallization (DEC) technique was combined with powder diffraction and vibrational spectroscopy as the analytical tools. This led to identification of eleven new cocrystals...
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Effect of plasma sprayed and laser re-melted Al2O3 coatings on hardness and wear properties of stainless steel
PublikacjaCommercially available austenic stainless steel substrate was coated with commercially available, raw Al2O3 powder applied by means of plasma spraying method and then re-melted with CO2 laser beam of various parameters. Tribological and mechanical properties of the 120 J/mm and 160 J/mm laser re-melted coatings were compared with the tribological and mechanical properties of the “as-sprayed” coating. The influence of the laser...
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Ceramic composites for single-layer fuel cells
PublikacjaComposite materials consisting of acceptor doped lanthanum orthoniobate electrolyte phase (La0.98Ca0.02NbO4) and Li2O:NiO:ZnO semiconducting phase were synthesized. The precursor powder of La0.98Ca0.02NbO4 was prepared in nanocrystalline (mechanosynthesis) and microcrystalline (solid-state synthesis) form. The composite can be applied in a single-layer fuel cell, because of the presence of two phases acting as an anode and a cathode...
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Enhanced Electrochemical Performance of MnCo1.5Fe0.5O4Spinel for Oxygen Evolution Reaction through Heat Treatment
PublikacjaMnCo1.5Fe0.5O4 spinel oxide was synthesized using the sol−gel technique, followed by heat treatment at various temperatures (400, 600, 800, and 1000 °C). The prepared materials were examined as anode electrocatalysts for watersplitting systems in alkaline environments. Solid-state characterization methods, such as powder X-ray diffraction and X-ray absorption spectroscopy (XAS), were used to analyze the materials’ crystallographic...
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Copper-based 2D-coordination polymer as catalyst for allylation of aldehydes
PublikacjaA copper-tartrate, [Cu2(Tart)2(H2O)2]·4H2O, was synthesized at room temperature in aqueous media using copper chloride and D-tartaric acid. The compound crystallizes in the monoclinic system P21 space group and was characterized by infrared spectroscopy, thermogravimetry, X-ray powder diffraction and the results are in good agreement with the single crystal...
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MgPdSb─An Electron-Deficient Half-Heusler Phase
PublikacjaThe half-Heusler family consists of many semiconducting intermetallic compounds, virtually all of them having a valence electron count (VEC) of 18. We have studied an electron-deficient (VEC = 17) phase MgPdSb and its Pd-stuffed variant MgPd1.25Sb. The cubic F4̅3m crystal structure was confirmed by the Rietveld refinement of powder X-ray diffraction (XRD) data. The lattice parameter is a = 6.284 and 6.335 Å for MgPdSb and MgPd1.25Sb,...
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Superconductivity in the intermetallic compound Zr5Al4
PublikacjaPolycrystalline Zr5Al4 was synthesized using the arc-melting method. Powder X-ray diffraction confirms the previously reported crystal structure of the Ti5Ga4-type P63/mcm with lattice parameters: a = 8.4312(6) A , and c = 5.7752(8) A . Electrical resistivity and low-temperature magnetic susceptibility measurements indicate that Zr5Al4 exhibits superconducting behavior below 2 K. The normalized heat capacity jump at Tc= 1.82 K...
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Rattling-enhanced superconductivity in MV2Al20 (M = Sc, Lu, Y) intermetallic cage compounds
PublikacjaPolycrystalline samples of four intermetallic compounds: MV2Al20 (M=Sc, Y, La, and Lu) were synthesized using an arc-melting technique. The crystal structures were analyzed by means of powder x-ray diffraction and Rietveld analysis, and the physical properties were studied by means of heat capacity, electrical resistivity, and magnetic susceptibility measurements down to 0.4 K. For ScV2Al20, LuV2Al20, and YV2Al20, superconductivity...
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Single crystal growth and physical properties of MCo2Al9 (M= Sr, Ba)
PublikacjaSingle crystals of SrCo2Al and BaCo2Al9 were grown using a self-flux method. A LeBail analysis of the powder X-ray diffraction patterns show that both compounds crystallize in a hexagonal (P6/mmm) crystal structure with lattice parameters: a = 7.8995(1) Å, c = 3.9159(1) Å for SrCo2Al9, and a = 7.9162(2) Å, c = 3.9702(1) Å for BaCo2Al9 aluminide. The low temperature analysis of the heat capacity measurements give a Sommerfeld...
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Two-step synthesis of niobium doped Na–Ca–(Mg)–P–Si–O glasses
PublikacjaNiobium doped biosolubility glasses in the Na–Ca–(Mg)–P–Si–O system were prepared by using an untypical two-step synthesis route. The parent glass was melted in air atmosphere at 1350 °C followed by re-melting the glass in Nb crucible with the addition of metallic Mg/Ca powder in the nitrogen atmosphere. The second melting step was carried out at 1450–1650 °C, using an induction furnace. The topography and structure of the obtained...
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Spectroscopic evaluation on pseudopolymorphs of sodium naproxen
PublikacjaThis paper demonstrates the assessment of vibrational spectroscopy methods such as middle infrared, near infrared and Raman spectroscopy (FTIR, FT-NIR, Raman) for the identification of pseudopolymorphic forms of a model active pharmaceutical ingredient (API) - sodium naproxen (NpxNa). NpxNa, in the form of three different pseudopolymorphs, was investigated by methods dedicated for solid state characterization: DSC (differential...
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The influence of Be addition on the structure and thermal properties of alkali-silicate glasses
PublikacjaBe-Na-(Li)-Si oxide glasses containing up to 15 mol% of BeO were prepared. Their structure was characterized by X-ray powder diffraction and Raman as well as infrared spectroscopic techniques, while their chemical compositions were examined by Inductively Coupled Plasma Optical Emission Spectrometry. All materials were found to be amorphous and contain Al contaminations from minor dissolution of the alumina crucibles. The results...
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Pt-rich intermetallic APt8P2 (A = Ca and La)
PublikacjaThe combination of experimental and theoretical investigation of two new Pt-rich intermetallic compounds: APt8P2 (A = Ca and La) is presented, including solid-state synthesis, crystal structure determination, physical properties characterization and chemical bonding analysis. APt8P2 was obtained through the high-temperature pellet synthesis. According to both single crystal and powder X-ray diffraction results, APt8P2 crystallize...
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Influence of pore formers on electrical properties of CaTi0.9Fe0.1O3-δ perovskite-type ceramics
PublikacjaPorous CaTi0.9Fe0.1O3-δ (CTF) perovskites were synthesized by the standard solid state method at different sintering temperatures with carbon black (CB), corn starch (CS) and potato starch (PS) as pore-forming agents. The ceramic samples of porosity between 9% and 42% with 5 - 40 μm pore sizes, were obtained by a 6 h sintering at either 1130º C or 1200º C of precursor powder prepared at 1470º C. X-ray diffraction analysis proved...