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采用 MAS 下 CPMG 采集对 As(x)Se(1-x) 玻璃进行 77Se 固态 NMR 研究。

77Se solid-state NMR investigations on As(x)Se(1-x) glasses using CPMG acquisition under MAS.

机构信息

CNRS-CEMHTI, UPR 3079, Orléans, France.

出版信息

Solid State Nucl Magn Reson. 2011 Sep;40(2):72-7. doi: 10.1016/j.ssnmr.2011.06.001. Epub 2011 Jun 24.

Abstract

(77)Se (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 (77)Se 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 (77)Se 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 T(2)(CPMG)-resolved spectrum shows a strong influence of the J-couplings between naturally occurring (77)Se 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.

摘要

(77)硒的固态 NMR 是硒化物玻璃局部结构的非常灵敏的探针,而硒化物玻璃本身在光学应用方面很有前景。在这项工作中,我们表明,尽管(77)硒的天然丰度较低(7.58%)且光谱范围较宽,但通过在检测(77)硒磁化时使用转子同步 π 脉冲的 Carr-Purcell-Meiboom-Gill(CPMG)序列,可以显著提高灵敏度,但当魔角旋转速度不够快时,灵敏度可能会受到化学位移各向异性的影响,并且会受到偏移效应的影响。(77)硒 T(2)(CPMG)分辨谱的间接维度强烈影响天然存在的(77)硒对之间的 J 耦合。得到的光谱表明,被称为“链交叉模型”的结构模型并不完全适用于描述富硒成分的玻璃状网络。

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