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Superconducting properties of the Fe(Se,Te) system are directly related to its microstructure. However, in the framework of a not well assessed phase diagram, a large spread of chemico-physical and functional properties is reported for compounds characterized by similar overall chemical compositions. This is in particular observed in materials produced by melting routes, where chemical inhomogeneities and multiple phases are commonly obtained. Both composition and morphology of these inhomogeneities seem to play a role in the behaviour of the superconducting phases, pointing out the need to assess the dependence of phase composition and therefore of the material performance on the sample thermal history. In this work, the effect of different post-synthesis annealing treatments is studied. A melting route has been adopted to synthesize polycrystalline samples, subsequently subjected to thermal treatments at different temperatures. Morphology and microstructure were characterized by means of x-ray diffraction and microscopy techniques. The superconducting properties have been evaluated by means of electrical and magnetic measurements. It is observed how microstructure, chemical composition and morphology of the obtained products strictly depend on the annealing temperature. Moreover, a crucial role of the cooling step is evidenced: in fact, a rapid cooling procedure from high temperature leads to the formation of high temperature (Tconset > 19 K) superconducting phases, but the overall bulk superconducting performance is negatively affected. Other annealing treatments can promote instead an enhancement in the critical current at high fields with respect to pristine sample, suggesting that a careful engineering of a post-synthesis thermal step can represent a useful tool to optimize the material properties.

The synthesis of hydroxylammonium lead iodide NH3OHPbI3 was accomplished by means of the reaction between water solutions of HI and NH2OH with PbI2 in sulfolane in conjunction with either crystallization by CH2Cl2 vapor diffusion or sulfolane extraction with toluene. The appropriate choice of the solvent was found to be crucial in order to attain the desired material. The synthesized compound was extensively characterized by single crystal and powder X-ray diffraction, UV-Vis diffuse reflectance spectroscopy, FT-IR spectroscopy, 1H-NMR spectroscopy, TG-DTA-QMS EGA (Evolved Gas Analysis), ESI-MS, and CHNS analysis. NH3OHPbI3 is an extremely reactive, deliquescent solid that easily oxidizes in air releasing iodine. Furthermore, it is the first reported perovskite to melt (m.p. around 80 °C) before decomposing exothermally at 103 °C. Such a chemical behavior, together with its optical absorption properties (i.e. yellow-colored perovskite), renders this material totally unsuitable for photovoltaic applications. The deliquescence of the material is to be ascribed to the strong hydrophilicity of hydroxylammonium ion. On the other hand, the relatively high Bronsted acidity of hydroxylammonium (pKa = 5.97) compared to other ammonium cations, promotes the reduction of atmospheric oxygen to water and the NH3OHPbI3 oxidation. The crystal structure, determined by single crystal X-ray diffraction with synchrotron radiation, is orthorhombic, but differs from the prototypal perovskite structure. Indeed it comprises infinite chains of face-sharing PbI6 octahedra along the c-axis direction with hydroxylammonium cations positioned between the columns, forming layers on the ac plane. The solvent intercalates easily between the layers. The crystal structure is apparently anomalous considering that the expected Goldschmidt's tolerance factor for the system (0.909) lies in the range of a stable prototypal perovskite structure. Therefore, the strong hydrogen bond forming tendency of hydroxylamine is likely to account for the apparent structural anomaly.

We report here the synthesis of the Z-3N(2-ethoxyphenyl)-2-N′(2-ethoxyphenyl)-imino-thiazolidin-4-one compound. The crystal structure is determined by X-ray diffraction. The compound crystallizes in the monoclinic system with the space group P21/n and cell parameters: a = 9.4094(10) A, b = 9.3066(10) A, c = 20.960(2) A, β = 99.0375(10)°, V = 1812.7(3) A3 and Z = 4. The structure is refined to final R = 0.05 for 2083 observed reflections. The molecule in the crystal exhibits the intermolecular hydrogen bonds of C–H…O, C–H…N, and C–H…S types. Ab initio calculations are also performed at Hartree–Fock (HF) and density functional theory (DFT) levels. The full HF and DFT geometry optimization is carried out using the 6-31G(d,p) basis set. The observed molecular structure is compared with that calculated by both HF and DFT methods. The optimized geometry of the titled compound is found to be consistent with the structure determined by X-ray diffraction.

X-ray powder diffraction was combined, for the first time, with Nuclear Magnetic Resonance spectroscopy and direct infusion mass spectrometry to characterise fresh and brined grape leaves. Covariance analysis of data generated by the three techniques was performed with the aim to correlate information deriving from the solid part with those obtained for soluble metabolites. The results obtained indicate that crystalline components can be correlated to the metabolites contained in the grape leaves, paving the way to the use of X-ray diffraction analysis for food fingerprinting purposes. Moreover it was ascertained that, differently from most of the metabolites present in the fresh vine leaves, linolenic acid (an omega-3-fatty acid) and quercetin-3-O-glucuronide (a polyphenol metabolite) do not undergo sensible degradation during the brining process, which is used as preservative method for the grape leaves. (C) 2013 Elsevier Ltd. All rights reserved.

C27H36ClN2O9PS, monoclinic, C12/c1 (no. 15), a = 36.495(3) A?, b = 8.5574(4) A?, c = 20.487(4) A?, b = 101.18(2)°, V = 6276.8 A?3, Z = 8, Rgt(F) = 0.052, wRref(F2) = 0.125, T = 295 K.

Nonstoichiometric REEAl(2.07)(B(4)O(10))O(0.60) (REE = (La, Ce); Ce; Nd) dimetaborates have been crystallized and analyzed by means of single crystal X-ray diffraction. The compounds resulted to be isostructural within hexagonal space group P (6) over bar 2m (n. 189), with the following unit cell parameters: a = 4.6060(6) angstrom, c = 9.3510(8) angstrom and V = 171.81(3) angstrom(3) (La, Ce); a = 4.5960(6) angstrom; c = 9.3170(10) angstrom and V = 170.44(4) angstrom(3) (Ce); a = 4.5830(7) angstrom, c = 9.2810(14) angstrom and V = 168.82(4) angstrom(3) (Nd). The REE cations are surrounded by six oxygen atoms, making up a trigonal prismatic coordination; Al cation is surrounded by five oxygen atoms, resembling a square pyramidal coordination, while the BO(4) group displays tetrahedral arrangement. The three-dimensional framework can be described as a mica-like structure packed down crystallographic axis c, with layers of six-membered rings of B tetrahedra alternated by inter-layers REE cations and layers of Al polyhedra. A complex network of REE center dot center dot center dot O and Al center dot center dot center dot O interactions concur to stabilize the framework.

In this work a treatment for surface preparation to improve mechanical resistance in adhesive bonding of plastic composites reinforced with fibres and metallic material, has been performed using an excimer laser. The following couplings have been selected to reproduce joints commonly used in the aerospace and automotive industry: CFC (carbon fibre composite) with CFC, CFC with Al 2024T3, Al 99% with Al 99%, GFC (glass fibre composite) with zinc-coated sheet in low carbon steel FeP01. The surfaces have been prepared using an excimer laser, adopting several values of laser parameters. The obtained surfaces have been examined by optical and scanning electron microscope: comparative measures of wetting and roughness have been performed to obtain an accurate characterisation and to select the proper finishes suitable to improve the mechanical resistance of the joints. The results obtained show that laser treatment always improves the final resistance of the joint; notable increases, and no significant surface damages have been highlighted. Better results have been obtained with the Al 99% with Al 99% joints which, with a low number of pulses treatment, have shown an increase of mechanical resistance up to the 70%.