12.01.2013 Views

NNR IN RAPIDLY ROTATED METALS By - Nottingham eTheses ...

NNR IN RAPIDLY ROTATED METALS By - Nottingham eTheses ...

NNR IN RAPIDLY ROTATED METALS By - Nottingham eTheses ...

SHOW MORE
SHOW LESS

You also want an ePaper? Increase the reach of your titles

YUMPU automatically turns print PDFs into web optimized ePapers that Google loves.

- 95 -<br />

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

Hooray! Your file is uploaded and ready to be published.

Saved successfully!

Ooh no, something went wrong!