화학공학소재연구정보센터
Journal of Chemical Physics, Vol.117, No.7, 3327-3339, 2002
Determination of distances between aluminum and spin-1/2 nuclei using cross polarization with very weak radio-frequency fields
In this work the possibility of using cross-polarization (CP) experiment for the determination of distances between spin-5/2 and spin-1/2 nuclei in polycrystalline and amorphous materials was investigated. The properties of the method were experimentally studied in an isolated Al2H spin system within the as-synthesized AlPO4-31 and in "infinite" aluminophosphate networks within the calcined AlPO4-31 and the hydrated VPI-5. In all three cases time-dependent oscillations due to coherent polarization transfer between aluminum and spin-1/2 nuclei were detected. The crucial parameters that influenced the visibility of dipolar oscillations were rotating-frame spin-lattice relaxation times of both nuclear species involved in a CP process and the homogeneity of rf fields. For a successful measurement the relaxation times, which varied remarkably with amplitudes of applied rf fields, had to be comparable to or larger than the period of time-domain oscillations. Radio-frequency field inhomogeneity was minimized when amplitudes of rf fields were adjusted to the Hartmann-Hahn sideband matching condition 3nu(1I)+nu(1S)=nu(R), the nutation frequency of spin-5/2 nuclei was limited to nu(R)/2<3nu(1I)