0000000000274045

AUTHOR

Maria Teresa Caldes

Intercalation chemistry of superconducting zirconium and hafnium nitride halides

Abstract Lithium intercalation in MNX (M=Zr, Hf; X=Cl, Br) may lead to superconducting compounds with critical temperatures up to 24 K. Electrochemical lithiation experiments agree with the results obtained with chemical methods, as samples with larger capacity on discharge are also those having larger lithium contents after chemical lithiation. Variations exist in the electrochemical profiles of different batches for these compounds indicating differences in the intercalation reaction pathway. High-resolution electron microscopy images confirm the structural model isotypic to SmSI for β-MNX phases. The major part of crystals from ZrNX as well as from the HfNCl samples showing a high lithiu…

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Lithium intercalation chemistry, microstructure and superconductivity in zirconium and hafnium nitride halides

Abstract Lithium intercalation in β-MNX (M=Zr, Hf; X=Cl, Br) leads to superconducting compounds with critical temperatures between 12 and 24 K. The lithium uptakes after treatment of the host materials with n-butyllithium/hexane solutions are ca. 0.2 atoms per formula for β-ZrNCl and β-ZrNBr, and between 0.07 and 0.67 for β-HfNCl. Electrochemical lithiation experiments agree with the results obtained with chemical methods, as samples with larger capacity on discharge are also those having larger lithium contents after chemical lithiation. Variations exist in the electrochemical profiles of different batches for the three compounds indicating differences in the intercalation reaction pathway…

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Ordered mesoporous materials: composition and topology control through chemistry

Abstract The atrane route constitutes a very versatile technique to obtain ordered mesoporous materials. A wide diversity of silica and silica-doped materials can be prepared by bringing into play fundamental synthesis parameters (like temperature, concentration and pH) which, in turn, allow modulation of the resulting material topology.

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Synthesis and crystal structure of the α polytype of HfNBr

Abstract α-HfNBr has been prepared at 760 °C in a sealed evacuated fused silica tube by reaction between NH4Br and Hf followed by purification through chemical vapour transport under a temperature gradient. The crystal structure of this compound at room temperature has been determined for the first time by Rietveld refinement of X-ray powder diffraction data, electron diffraction and high resolution electron microscopy. It crystallises in the orthorhombic space group Pmmn with the unit cell parameters a=4.1165(2), b=3.5609(2), c=8.6440(3) A. α-HfNBr is isotypic to FeOCl and is built from layers of composition BrHfNNHfBr stacked along c that are separated by a Van der Waals gap. The haf…

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