NNR IN RAPIDLY ROTATED METALS By - Nottingham eTheses ...
NNR IN RAPIDLY ROTATED METALS By - Nottingham eTheses ...
NNR IN RAPIDLY ROTATED METALS By - Nottingham eTheses ...
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annealed aluminium powder was placed in the standard Bruker probe<br />
system. The measurements were recorded at temperatures in the<br />
range 290-300 K using resonant frequencies of 15 and 16 MHz, but<br />
the results obtained were insensitive to these variations.<br />
Powders (a) and (b) were sieved so as to separate the specimen<br />
particle sizes so: 37 um, 37-44 um, and 44-76 pin. A few drops of<br />
pure acetone were added to the largest grain specimens in order to<br />
reduce distortion of the detected signals by mechanical vibrations<br />
set up in individual crystallites. The problem could not be cured<br />
by the powders being encapsulated in resin because the widths of<br />
the resonance spectra of the cured slugs were found to be increased<br />
by this treatment. (That this broadening was due to a quadrupole<br />
interaction rather than any stress induced distribution of Knight<br />
shifts was made evident by its partial removal upon rapid rotation<br />
of the specimens about the magic angle. ) Owing to the small skin<br />
depth (ti 20 um) the signal intensities obtained from the coarsest<br />
powders were less than those from the finer powders. However, with-<br />
in the limits of experimental error, the transformed lineshapes<br />
were found to be unaffected by particle size.<br />
The observed characteristic decay shapes from powder samples,<br />
(a) and (c), were quite distinguishable from each other. (Powder<br />
(c) was filtered to a particle size of less than 44 pm. ) Typical<br />
FIDs obtained from these two samples are shown in Figure 7.1 together<br />
with the corresponding lineshapes in the frequency domain. The<br />
FID and absorption spectrum of powder (b) were very similar in appear-<br />
ance to those obtained for (c), and are therefore not illustrated<br />
separately.<br />
The tails of nuclear spectra in the frequency domain are deter-<br />
mined largely by the supposition made about the behaviour of the FID