Improved critical current density in ex situ processed MgB2 tapes by the size reduction of grains and crystallites by high-energy ball milling

We have fabricated Fe-sheathed MgB₂ tapes through an ex situ process in a powder-in-tube (PIT) technique using powders ball milled under various conditions. Although the ex situ processed wires and tapes using the high-energy ball milled MgB₂ powders have been studied and the decrease of grain and crystallite sizes of MgB₂ and the critical current density (J_c) improvement of those conductors were reported so far, the use of filling powders milled at a higher rotation speed than previously reported further decreases the crystallite size and improves the J_c properties. The improved J_c values at 4.2 K and 10 T were nearly twice as large as those previously reported. Those milled powders and hence as-rolled tapes easily receive contamination in air. Thus, the transport J_c properties are easily deteriorated and scattered unless the samples are handled with care. The optimized heat treatment temperature (T_opt) of those tape samples at which best performance in the J_c property is obtained decreases by more than 100 °C, compared with that of tapes using the as-received MgB₂ powder.     

The effects of annealing temperature on the in-field Jc and surface pinning in silicone oil doped MgB2 bulks and wires

The effects of sintering temperature on the lattice parameters, full width at half maximum (FWHM), strain, critical temperature (T_c), critical current density (J_c), irreversibility field (H_irr), upper critical field (H_c2), and resistivity (ρ) of 10 wt.% silicone oil doped MgB₂ bulk and wire samples are investigated in state of the art by this article. The a-lattice parameter of the silicone oil doped samples which were sintered at different temperatures was drastically reduced from 3.0864 Å to 3.0745 Å, compared to the un-doped samples, which indicates the substitution of the carbon (C) into the boron sites. It was found that sintered samples at the low temperature of 600 °C shows more lattice distortion by more C-substitution and higher strain, lower T_c, higher impurity scattering, and enhancement of both magnetic J_c and H_c2, compared to those sintered samples at high temperatures. The flux pinning mechanism has been analyzed based on the extended normalized pinning force density f_p = F_p/F_p,max scaled with b = B/B_max. Results show that surface pinning is the dominant pinning mechanism for the doped sample sintered at the low temperature of 600 °C, while point pinning is dominant for the un-doped sample. The powder in tube (PIT) MgB₂ wire was also fabricated by using of this liquid doping and found that both transport J_c and n-factor increased which proves this cheap and abundant silicone oil doping can be a good candidate for industrial application.     

Transport critical current density of Bi–Sr–Ca–Cu–O/Ag superconductor tapes with addition of magnetic nanopowder γ-Fe2O3

The effect of sintering temperature on the transport properties of Ag-sheathed-(Bi_1.6Pb_0.4)Sr₂Ca₂Cu₃O₁₀–(γ-Fe₂O₃)_0.01 superconductor tapes prepared by the powder-in-tube technique with sintering time fixed at 50 h has been investigated. The maximum transport critical current density, J_c of 6490 A/cm² at 77 K, was observed at sintering temperature of 845 °C. A further single intermediate rolling step increases J_c to 9560 A/cm². Sintering temperature from 830 to 845 °C increases the 2223 phase content and resulted in improved J_c. At 850 °C, the content of 2223 phase decreased resulting in a corresponding decrease in J_c. X-ray diffraction patterns suggest that the 2212 phase reacts with non-superconducting phase such as CaCuO₂, (SrCa)₂CuO₃, CaO, and CuO to form the 2223 phase. Samples without γ-Fe₂O₃ prepared under the same condition showed a lower J_c with maximum at 1560 A/cm². Our results show that nanomagnetic γ-Fe₂O₃ addition improved J_c which supports previous calculations on the possibility of frozen flux superconductor with nanomagnetic addition in this class of materials.     

Emission analysis of Sm3+:Ca4GdO(BO3)3 powder phosphor

This paper reports on the spectral analysis of reddish orange color luminescent Sm³⁺:Ca₄GdO(BO₃)₃ powder phosphor. This phosphor powder has been synthesized by a solid state reaction method. Emission spectrum of it has shown four emission transitions of ⁴G_5/2 → ⁶H_J (J = 5/2, 7/2, 9/2, 11/2) and among them, the transition ⁴G_5/2 → ⁶H_7/2 displays the reddish orange (605 nm) color. Lifetimes of three emissions (⁴G_5/2 → ⁶H_{J=5/2, 7/2 & 9/2}) have been computed based on the measured decay curves. Besides the measurement of emission spectrum of this material, its nature and structural details have also been investigated from XRD, SEM and FTIR studies.     

Temperature-dependent multi-k magnetic structure in multiferroic Co3TeO6

A complex magnetic order of the multiferroic compound Co₃TeO₆ has been revealed by neutron powder diffraction studies on ceramics and crushed single crystals. The compound adopts a monoclinic structure (s.g. C2/c) in the studied temperature range 2–300 K but exhibits successive antiferromagnetic transitions at low temperature. Incommensurate antiferromagnetic order with the propagation vector k₁ = (0, 0.485, 0.055) sets in at 26 K. A transition to a second antiferromagnetic structure with k₂ = (0, 0, 0) takes place at 21.1 K. Moreover, a transition to a commensurate antiferromagnetic structure with k₃ = (0, 0.5, 0.25) occurs at 17.4 K. The magnetic structures have been determined by neutron powder diffraction using group theory analysis as a preliminary tool. Different coordinations of the Co²⁺ ions involved in the low-symmetry C2/c structure of Co₃TeO₆ render the exchange-interaction network very complex by itself. The observed magnetic phase transformations are interpreted as an evidence of competing magnetic interactions. The temperature dependent changes in the magnetic structure, derived from refinements of high-resolution neutron data, are discussed and possible mechanisms connected with the spin reorientations are described.     

X-ray powder diffraction,vibration and thermal studies of [A0.92(NH4)0.08]2TeCl4Br2 with A = Cs,Rb: Influence of mixed cationic and anionic substitutions

The crystal structures of [A_0.92(NH₄)_0.08]₂TeCl₄Br₂ with A = Cs, Rb have been determined using X-ray powder diffraction techniques. The two compounds crystallize in the tetragonal space group P4/mnc, with the unit cell parameters: a = 7.452(1) Å, c = 10.544(3) Å, Z = 2 and a = 7.315(2) Å, c = 10.354(4) Å, Z = 2 in the presence of Cs and Rb, respectively. These two compounds have an antifluorite-type arrangement of NH₄⁺/Rb⁺/Cs⁺ and octahedral TeCl₄Br₂^2? anions. The stability of these structure is by ionic and hydrogen bonding contacts: A?Cl, A?Br and N–H?Cl, N–H?Br. The different vibrational modes of these powders were analysed by FTIR and Raman spectroscopic studies. A DTA/TGA experiment reveals one endothermic peak at 780 K implicating the decomposition of the sample. At low temperature, one endothermic peak in thermal behavior is detected at around 213 K by DSC experiment. This transition was confirmed by dielectric measurements.     

Effects of grain boundaries on electrical and magnetic properties of melt-processed SmBa2Cu3Ox superconductors

In the present study, we examine the energy dissipation mechanisms and grain boundary effects on the superconducting properties of high-T_c SmBa₂Cu₃O_7?x samples. Sm-123 was synthesized with the top-seeded-melt-growth technique. Grain sizes, as determined by optical microscopy, ranged between 0.5 mm and 1.5 mm. Thus, each specimen, on which the electrical and magnetic measurements were carried out, contained several grains. Some of our findings are as follows: (1) the intragrain T_c is 93.5 K and the intergrain T_c is 87.5 K. Superconducting transition width is narrow and is not affected much by the magnetic field. (2) The intragrain J_c is 110,000 A cm^?2 while the intergrain J_c is 210 A cm^?2 at 10 K. (3) The intergrain J_c shows a secondary peak with the increase in temperature from 10 K to 30 K. The main reasons behind these observations are discussed in detail.     

Hybrid tandem photovoltaic devices with a transparent conductive interconnecting recombination layer

We demonstrate hybrid tandem photovoltaic devices with a transparent conductive interconnecting recombination layer. The series-connected hybrid tandem photovoltaic devices were developed by combining hydrogenated amorphous silicon (a-Si:H) and polymer-based organic photovoltaics (OPVs). In order to enhance the interfacial connection between the subcells, we employed highly transparent and conductive indium tin oxide (ITO) thin layer. By using the ITO interconnecting layer, the power conversion efficiency of the hybrid tandem solar cell was enhanced from 1.0% (V_OC = 1.041 V, J_SC = 2.97 mA/cm², FF = 32.3%) to 2.6% (V_OC = 1.336 V, J_SC = 4.65 mA/cm², FF = 41.98%) due to the eliminated interfacial series resistance.     

Synthesis,crystal structure and properties of a new lead fluoride borate,Pb3OBO3F

A new compound, Pb₃OBO₃F, has been grown by the high temperature solution method from the PbO–PbF₂–B₂O₃ system. It crystallizes in the orthorhombic system, space group Pbcm with unit-cell parameters a = 7.6313(14) Å, b = 6.5229(12) Å, c = 11.906(2) Å, Z = 4, volume = 592.66(19) Å³. The structure of the compound is solved by the direct methods and refined to R₁ = 0.0528 and wR₂ = 0.1400. Pb₃OBO₃F consists of Pb(1)O₃F tetrahedra, Pb(2)O₄ tetrahedra and BO₃ triangles which build up the symmetrical chains extended along the c-axis. The powder X-ray diffraction pattern of the Pb₃OBO₃F has been measured. Functional groups presented in the sample were identified by Fourier transform infrared spectrum.     

Critical current density and stability of Tube Type Nb3Sn conductors

The critical current densities (J_c) and stabilities of Tube Type Nb₃Sn conductors have been measured. The strands had superconducting subelement counts ranging from 192 to 744, and flat-to-flat filament sizes (for 0.7 mm OD wire) of from 35 μm down to 15 μm. These Tube Type conductors had a very simple structure: prior to heat treatment the filaments consist of a Sn core surrounded by a thin Cu tube, itself surrounded by a Nb or Nb alloy tube. Eight different strand types were investigated using various techniques including SEM, residual resistance ratio (RRR), transport J_c, and stability measurement. Most strands were studied at 0.7 mm OD, with one representative at 0.42 mm. The transport measurements were made at 4.2 K in fields up to 14 T. Numerous heat treatment schedules were investigated, with reaction temperatures ranging from 615 °C to 650 °C, and times ranging from 36–500 h. The highest J_cs were seen for the lowest reaction temperatures, with 12 T transport J_c values as high as 2450 A/mm² observed. The RRRs were lower for longer time and higher temperature reactions and ranged from 4 to 180. Strand stability was a strong function of the effective filament diameter, d_eff, and RRR. The most stable strands showed stability currents, J_s, of 8700 A/mm² and 15,300 A/mm² for 0.7 mm OD and 0.42 mm OD conductors, respectively.     

Anisotropic thermal expansion behavior in tetragonal Sr2MgWO6

The colorless sample of Sr₂MgWO₆ was prepared by conventional solid-state reaction of stoichiometric amounts of SrCO₃, WO₃ and MgO and characterized by powder X-ray diffraction (XRD) studies. In the temperature range of 300–15 K, detailed structural studies on Sr₂MgWO₆ were carried out by Rietveld refinements of the observed powder neutron diffraction (ND) data. At ambient temperature Sr₂MgWO₆ crystallizes in tetragonal (space group I4/m) lattice with unit cell parameters: a = 5.5882(2) and c = 7.9452(7) Å, V = 248.11(3) Å³, Z = 2. This tetragonal (I4/m) structure is retained down to 15 K. The structural analysis of the sample at different temperatures indicates no appreciable change in the MgO and WO bond lengths. However, a decrease in the tilt angle is observed with increasing temperature. The negative thermal expansion of the c-axis is attributed to increasing transverse displacement amplitude of the bridging oxygen atoms along this axis.     

Microwave direct synthesis of MgB2 superconductor

Intermetallic compound superconductor MgB₂ was synthesized from spherical magnesium powder and lower purity amorphous boron powder by microwave direct heating. Powder X-ray diffraction (XRD) analysis indicates that the phases of the synthesis sample are MgB₂ (major phase) and a small amount of MgO. Scanning electron microscope (SEM) observation shows that the MgB₂ grain size is homogeneous and the particle size is about several hundreds of nanometers. The onset superconducting transition temperature of the MgB₂ sample measured by the temperature dependence of magnetization measurement is about 37.6 K. The critical current density J_c calculated according to the Bean model are about 2.0 × 10⁵ A/cm² at 20 K in self-field and 1.0 × 10⁵ A/cm² at 20 K in 1 T applied field.     

Synthesis and structure determination of new open-framework chromium carboxylate MIL-105 or CrIII(OH)·{O2C–C6(CH3)4–CO2}·nH2O

Two new three-dimensional chromium(III) dicarboxylate, MIL-105 or Cr^III(OH)·{O₂C-C₆(CH₃)₄-CO₂}·nH₂O, have been obtained under hydrothermal conditions, and their structures solved using X-ray powder diffraction data. Both solids are structural analogs of the known Cr benzenedicarboxylate compound (MIL-53). Both contain trans corner-sharing CrO₄(OH)₂ octahedral chains connected by tetramethylterephthalate di-anions. Each chain is linked by the ligands to four other chains to form a three-dimensional framework with an array of 1D pores channels. The pores of the high temperature form of the solid, MIL-105ht, are empty. However, MIL-105ht re-hydrates at room temperature to finally give MIL-105lt with pores channels filled with free water molecules (lt: low temperature form; ht: high temperature form). The thermal behaviour of the two solids has been investigated using TGA. Crystal data for MIL-105ht: monoclinic space group C2/c with a = 19.653(1) Å, b = 9.984(1) Å, c = 6.970(1) Å, β = 110.67(1)° and Z = 4. Crystal data for MIL-105lt: orthorhombic space group Pnam with a = 17.892(1) Å, b = 11.165(1) Å, c = 6.916(1) Å and Z = 4.     

Synthesis,structure, growth and characterization of a novel organic NLO single crystal: Morpholin-4-ium p-aminobenzoate

The title compound, morpholin-4-ium p-aminobenzoate (MPABA)(C₄H₁₀NO⁺,C₇H₆NO₂^?), has been synthesized for the first time by the addition of morpholine with 4-aminobenzoic acid in equi-molar ratio and good quality single crystals have been grown by solution growth technique using methanol as a solvent. The molecular structure of the compound was solved and refined by Direct Methods using SHELXS97 and full-matrix least-squares technique using SHELXL97, respectively. MPABA crystallizes in a monoclinic system with unit cell parameters, a = 5.948(5) Å, b = 18.033(4) Å, c = 10.577(5) Å, β = 90.40(1)° and non-centrosymmetric space group Cc. The experimentally measured density and chemical compositions were found to be in good agreement with the theoretical values. The phases and functional groups of MPABA have been identified and confirmed through powder X-ray diffraction and Fourier transform infrared (FTIR) studies, respectively. The thermal stability and decomposition details were studied through TG/DTA thermograms. The UV–visible transmission spectra were recorded for the grown crystal and its NLO characteristic was explored by powder second harmonic generation (SHG) studies.     

Preparation,magnetic and optical properties of layered oxychalcogenides SmCuOCh (Ch = S or Se)

This paper reports on the synthesis and the electrical, magnetic and optical properties of SmCuOS and SmCuOSe. The magnetic properties reveal that Sm is in its 3+ oxidation state (μ^theo = g√J(J + 1) = 0.85 μ_B; g = 2/7) with a large Van Vleck contribution, and exclude the possibility of a divalent oxidation state for samarium (Sm²⁺; ⁷F₀ state, g = J = 0, μ_eff = 0).Optical properties were studied by means of diffuse reflectance and photoluminescence spectra in the UV–vis range. The electrical measurements show that the two samarium copper oxychalcogenides, SmCuOSe and SmCuOS are semiconductors with optical band gap (E_g) values of 2.60 and 2.90 eV, respectively.     

Structure and magnetism in Pr3RuO7

The crystal structure of the ordered fluorite, Pr₃RuO₇, was refined from powder neutron diffraction data in Cmcm. An interesting structural feature is the presence of relatively well separated zig-zag chains of corner sharing RuO₆ octahedra, Ru–Ru interchain distance 6.61 Å vs. Ru–Ru intrachain distance of 3.76 Å. Magnetic susceptibility data show a Curie–Weiss behavior for T>225 K with C=5.96(4) emu K mol⁻¹ and θ_c=+11(2) K. In an attempt to separate the contributions of Pr(3+) and Ru(5+), the properties of isostructural Pr₃TaO₇ were also measured, yielding C=4.63(3) emu K mol⁻¹. Thus, the contribution of Ru(5+), 4d³, S=3/2, to the measured Curie constant is estimated to be 1.33 emu K mol⁻¹, not far from the spin-only value of 1.87 emu K mol⁻¹. This supports the view that the Ru 4d electrons are localized and magnetic, not itinerant. A susceptibility maximum at about 50 K is attributed to long-range magnetic order and this is substantiated by neutron diffraction data. There is little evidence for one-dimensional antiferromagnetic correlations in this material but behavior characteristic of short-range ferromagnetic correlations attributed to Pr–Ru exchange interactions are found in the temperature range 50–200 K, consistent with the positive θ_c.     

Two 2-D 36 tessellated metal–organic frameworks constructed from trimetallic clusters and dicarboxylate ditopic links

Two metal–organic framework compounds, [Zn₃(1,4-BDC)₃(Py)₂]·2(1,4-dioxane) (MOF-CJ6) and [Cd₃(bpdc)₃(H₂O)₂] (MOF-CJ7), have been solvothermally synthesized and characterized by single crystal X-ray diffraction, X-ray powder diffraction, ICP, IR and photoluminescence spectroscopy analyses, respectively. MOF-CJ6 crystallizes in monoclinic, space group P2(1)/n (no. 14) with a = 14.6886(14) Å, b = 9.6194(6) Å, c = 15.9161(16) Å and β = 105.687(6)°. Its framework can be described as a 2-D 3⁶ tessellated net based on the assembly of trimeric Zn₃(CO₂)₆ clusters and 1,4-benzenedicarboxylates ditopic links. The 2-D nets can be further linked into a novel 3-D supramolecular hexagonal lattice (hex) network through π–π packing interaction. MOF-CJ7 crystallizes in trigonal, space group R-3 (no. 148) with a = 14.1129(8) Å, b = 14.1129(8) Å, c = 20.1168(13) Å and γ = 120°. MOF-CJ7 exhibits analogous framework topology with that of MOF-CJ6, consisting of trimeric Cd₃(CO₂)₆ clusters and 4,4′-biphenyldicarboxylate links.     

A facile one-step route to nanocrystalline TiB2 powders

Nanocrystalline titanium diboride (TiB₂) has been prepared by the reaction of TiCl₄ with NaBH₄ in the temperature range of 500–700 °C in an autoclave. X-ray powder diffraction (XRD) patterns can be indexed as hexagonal TiB₂ with the lattice constants of a=3.032 and c=3.229 Å. Transmission electron microscopy (TEM) image shows particle morphology, with average size of 15 nm for the powder obtained at 600 °C. Selected area electron diffraction (SAED) pattern confirms the prepared hexagonal TiB₂. The oxidation behavior of TiB₂ is studied by thermogravimetric analysis (TGA) and differential thermal analysis (DTA).     

Fluorescence properties and relaxation processes of Tb3+ ions in ZnCl2-based glasses

60ZnCl₂–20KCl–20BaCl₂–xTbCl₃ glasses (x = 0.10, 0.25, 0.50, 0.75, 1.00, and 1.25) were prepared by melt-quenching method, and Tb³⁺ fluorescence properties were investigated under 355 nm excitation. Regardless of x values, the electrons that were relaxed from the ⁵D₃ to ⁵D₄ level of Tb³⁺ ions by the multiphonon relaxation, were repressed to 28% of all the excited electrons because the ZnCl₂-based glass had much lower phonon energy than oxide glasses. For 0 < x ≤ 0.34, the cross relaxation, (⁵D₃ → ⁵D₄) → (⁷F₀ ← ⁷F₆), was repressed, and consequently 72% and 28% of all the excited electrons were radiatively relaxed by the ⁵D₃ → ⁷F_J (J = 6, 5, 4, 3, and 2) and ⁵D₄ → ⁷F_J (J = 6, 5, 4, and 3) transitions, respectively. The lifetimes of the ⁵D₃ and ⁵D₄ initial levels were obtained to be 1.1 and 2.1 ms, respectively.     

Preparation,crystal structure and characterization of α-NaSbP2S6 and β-NaSbP2S6 phases

The new phases α-NaSbP₂S₆ and β-NaSbP₂S₆ were synthesized by ceramic and reactive flux methods at 773 K. The structures of α-NaSbP₂S₆ and β-NaSbP₂S₆ were determined by the single-crystal X-ray diffraction technique. α-NaSbP₂S₆ crystallizes in the monoclinic space group P2₁/c with a = 11.231(2) Å, b = 7.2807(15) Å, c = 11.640(2) Å, β = 108.99(3)°, V = 900.0(3) Å³ and z = 4. β-NaSbP₂S₆ crystallizes in the monoclinic space group P2₁ with a = 6.6167(13) Å, b = 7.3993(15) Å, c = 9.895(2) Å, β = 92.12(3) °, V = 484.10(17) Å³ and z = 2.The α- and β-phases of NaSbP₂S₆ are closely related, the main difference lies in the stacking of the [Sb[P₂S₆]]_nⁿ⁻ layers. The structure of α-NaSbP₂S₆ consists of two condensed layers (MPS₃ type) to give an ABAB… sequence with Na⁺ cations located in the interlayer space. The packing of β-NaSbP₂S₆ is formed by monolayers of [Sb[P₂S₆]]_nⁿ⁻ stacked in an AA… fashion separated by a layer of Na⁺ cations. Both phases are derivates of the M¹⁺M³⁺P₂Q₆ family.The optical band gaps of α-NaSbP₂S₆ and β-NaSbP₂S₆ were determined by UV–vis diffuse reflectance measurements to be 2.17 and 2.25 eV, respectively.