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77Se solid-state NMR investigations on As(x)Se(1-x) glasses using CPMG acquisition under MAS
Authors:Deschamps M  Roiland C  Bureau B  Yang G  Le Pollès L  Massiot D
Institution:aCNRS-CEMHTI, UPR 3079, 1D Avenue de la Recherche Scientifique, 45071 Orléans cedex 2, France;bDépartement de Chimie, Université d’Orléans, Avenue du Parc Floral, BP 6749, 45067 Orléans cedex 2, France;cVerres et Céramiques, UMR-CNRS 6226 Sciences Chimique de Rennes, Université de Rennes 1, Campus de Beaulieu, 35042 Rennes cedex, France;dChimie du Solide et Matériaux, UMR-CNRS 6226 Sciences Chimique de Rennes, Université de Rennes 1, Campus de Beaulieu, 35042 Rennes cedex, France
Abstract:77Se (I=1/2) solid-state NMR is a very sensitive probe of the local structure of selenide glasses, which themselves are promising for optical applications. In this work, we show that although 77Se has a low natural abundance (7.58%) and a wide spectral range, the sensitivity can be dramatically increased using Carr–Purcell–Meiboom–Gill (CPMG) trains of rotor-synchronized π pulses during the detection of 77Se magnetization but may be affected by chemical shift anisotropy when the Magic Angle Spinning rate is not fast enough and by offset effects. The indirect dimension of the T2CPMG-resolved spectrum shows a strong influence of the J-couplings between naturally occurring 77Se pairs. The resulting spectra show that the structural model known as “chains crossing model” is not entirely suitable to describe the glassy network of the Se-rich compositions.
Keywords:Selenium  Glass  Arsenide  Selenide  CPMG  J-coupling
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