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Solid-State High-Resolution ¹H-NMR Study for Ammonia Borane of Hydrogen Storage Material

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In liquids NMR, 1H is the most widely observed nucleus, which is not the case in solids NMR. The reason is due to the strong homo-dipolar interactions between the hydrogen atoms which mask the useful chemical shift information. Therefore we must remove the strong homo-dipolar interactions in order to get structural information, which can be investigated by the isotropic chemical shift. There are two ways of obtaining it. One is the ultra-fast MAS of ca. 70 kHz spinning speed, which has become available only recently. The other way is devising a pulse sequence which can remove the strong homo-dipolar interaction. In the latter way, MAS with a moderate spinning rate of a few kHz, is enough to remove the chemical shift anisotropy. In this report, 1D-CRAMPS and 2D MAS-FSLG techniques are utilized and their results will be compared. This kind of high-resolution 1H NMR for solids, should become a valuable analytical tool in the understanding and the developing of a new class of hydrogen storage materials. Here ammonium borane -NH3BH3, whose hydrogen content is high, is used as a sample.

Abstract

In liquids NMR, 1H is the most widely observed nucleus, which is not the case in solids NMR. The reason is due to the strong homo-dipolar interactions between the hydrogen atoms which mask the useful chemical shift information. Therefore we must remove the strong homo-dipolar interactions in order to get structural information, which can be investigated by the isotropic chemical shift. There are two ways of obtaining it. One is the ultra-fast MAS of ca. 70 kHz spinning speed, which has become available only recently. The other way is devising a pulse sequence which can remove the strong homo-dipolar interaction. In the latter way, MAS with a moderate spinning rate of a few kHz, is enough to remove the chemical shift anisotropy. In this report, 1D-CRAMPS and 2D MAS-FSLG techniques are utilized and their results will be compared. This kind of high-resolution 1H NMR for solids, should become a valuable analytical tool in the understanding and the developing of a new class of hydrogen storage materials. Here ammonium borane -NH3BH3, whose hydrogen content is high, is used as a sample.

참고문헌 (11)

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