29Si NMR in solid state with CPMG acquisition under MAS

Abstract

A remarkable enhancement of sensitivity can be often achieved in 29Si solid-state NMR by applying the well-known Carr–Purcell–Meiboom–Gill (CPMG) train of rotor-synchronized π pulses during the detection of silicon magnetization. Here, several one- and two-dimensional (1D and 2D) techniques are used to demonstrate the capabilities of this approach. Examples include 1D 29Si{X} CPMAS spectra and 2D 29Si{X} HETCOR spectra of mesoporous silicas, zeolites and minerals, where X = 1H or 27Al. Data processing methods, experimental strategies and sensitivity limits are discussed and illustrated by experiments. The mechanisms of transverse dephasing of 29Si nuclei in solids are analyzed. Fast magic angle spinning, at rates between 25 and 40 kHz, is instrumental in achieving the highest sensitivity gain in some of these experiments. In the case of 29Si– 29Si double-quantum techniques, CPMG detection can be exploited to measure homonuclear J-couplings.