27Al nuclear magnetic resonance study of synthetic and natural corundum (alpha-Al2O3). Some experimental aspects of quantitative 27Al nuclear magnetic resonance spectroscopy.
The 27Al nuclear magnetic resonance (NMR) response of a series of natural and synthetic corundum (alpha-Al2O3) samples is studied quantitatively by short-pulse excitation and frequency-stepped adiabatic half-passage (FSAHP). Using on- and off-resonance nutation NMR, it was established that the quadrupole coupling parameters of visible Al is identical in all samples. Remarkably, the relaxation behavior for the aluminum is very different in the various samples and has a marked effect on the quantitative response. In natural corundum samples the 27Al spin-lattice relaxation is very efficient as these samples contain paramagnetic impurities. As a result, however, the full signal could not be recovered, which is attributed to relaxation broadening of spins in the vicinity of these impurities. In synthetic samples, containing no impurities, the full signal could be recovered, although the relaxation behaviour appeared to depend strongly on the preparation method. We observed differences in the spin-lattice relaxation by a factor 20; the longest T1 was observed in a crushed single crystal. This implies that alpha-Al2O3 can only be used as a standard in quantitative analyses if it has been characterized thoroughly. Furthermore, the effective relaxation behaviour for different types of excitation is studied. Finally, a method to measure the spin-lattice relaxation of half-integer quadrupole nuclei is introduced, using a frequency-stepped adiabatic passage (FSAP) to invert the spin system.
NSR Center for Molecular Structure, Design and Synthesis, National HF-NMR Facility, University of Nijmegen, Netherlands.
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Kentgens
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Bos
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Dirken
D000535:Aluminum; D000537:Aluminum Oxide / Q000138:chemical synthesis / Q000737:chemistry*; D009682:Magnetic Resonance Spectroscopy; D011868:Radioisotopes
D011868:Radioisotopes; D000535:Aluminum; D000537:Aluminum Oxide