71Ga and 69Ga nuclear magnetic resonance study of beta-Ga2O3: resolution of four- and six-fold coordinated Ga sites in static conditions.

71Ga and 69Ga nuclear magnetic resonance (NMR) spectra have been obtained for beta-Ga2O3 at magnetic fields of 11.7 and 7.0 T with a combination of static and spinning samples and using echo techniques. Isotropic chemical shifts and well constrained electric field gradient (EFG) tensors were measured for the GaIV and GaVI sites in beta-Ga2O3 and are reported for the first time. Due to its high quadrupolar coupling constant the GaIV site in beta-Ga2O3 is only resolved in static conditions. Analysis of spectral discontinuities obtained for different isotopes and magnetic field strengths and a method of readily obtaining very broad spectra without point by point acquisition demonstrate an approach that should be very useful in constraining the chemical shifts and quadrupole parameters involved in solid-state gallium NMR spectra.

Two-dimensional magic-angle spinning isotropic reconstruction sequences for quadrupolar nuclei.

Two-dimensional magic-angle spinning (triple quantum, single quantum) correlation pulse sequences and phase cycles based on the technique of Frydman and Harwood for the reconstruction of the isotropic spectrum of half-integer spin quadrupolar nuclei broadened to second-order are described. These sequences provide pure absorption mode two-dimensional lineshapes and increased sensitivity. Experimental examples on spin I = 3/2 (87Rb in RbNO3) and I = 5/2 (27Al in NaSi3AlO8) are presented. The isotropic chemical shift and quadrupolar coupling parameters could be obtained from a simple analysis of the triple quantum filtered single quantum magic-angle spinning cross-sections.

71Ga NMR of reference GaIV, GaV, and GaVI compounds by MAS and QPASS, extension of gallium/aluminum NMR parameter correlation.

We report new measurements of NMR parameters for 71Ga in gallium bearing oxide reference compounds, ranging from perfectly ordered systems to disordered crystalline structures and their aluminate counterparts. Static, MAS, and QPASS spectra are obtained at magnetic fields ranging from 7.0 to 18.8 T. With these results we enhance the previously established correlation between isotropic chemical shifts of 71Ga and 27Al and propose a correlation between gallium and aluminum electric field gradients (EFG). This correlation shows that the EFG at 71Ga sites are generally three times greater than those at equivalent 27Al sites.