HR: 0800h
AN: V51A-0325 [Abstracts]
TI: Electron Microprobe Measurements of Nitrogen in SiC
AU: * Ross, K
EM: kentross@berkeley.edu
AF: Kent Ross, Earth and Planetary Science
University of California Berkeley, Berekeley, CA 94720-4767, United States
AB:
Methods have been developed for the measurement of low abundances of nitrogen in SiC films. These
techniques were developed for measurements of synthetic thin-film samples prepared by materials scientists but
the technique can also be applied to natural SiC grains in meteorites. One problem associated with measuring
nitrogen at low abundance levels is the low count rates due to strong absorption of the nitrogen signal in the
matrix material. In thin film samples, (SiC deposited on elemental Si) it is preferable to limit x-ray production and
emission to the overlayer. This eliminates the need for data reduction using thin-film methods. Thin film data
reduction is inevitably less accurate than bulk material data reduction methods. In order to limit x-ray emission to
the film layer, data has been collected at 5 kV and 3.5 kV accelerating voltage (depending on film thickness
estimates provided by scientists who prepared these samples). These low beam energies also promote
production of x-rays in the shallow region of the samples, and this minimizes strong absorption, leading to more
abundant nitrogen x-ray detection, which improves counting statistics and overall precision. The CASINO monte
carlo modeling program was used to model electron penetration and x-ray production as a function of beam
energy and depth in the sample in order to ensure that the excited volume is limited to the film. The beam was set
to 200 nA beam current. This high beam current also improves counting statistics by providing more abundant
count rates. One drawback of these beam conditions is the limited spatial resolution provided. In our Cameca
probe, a 5 kV, 200 nA beam is approximately 10 microns in diameter. SiC samples and standard were not carbon
coated (they are conducting). AlN was used as the nitrogen standard. These films contained 0.3 to 0.7 wt. per
cent nitrogen, with analytical uncertainties in the range of 10-20 per cent relative errors. The Si:C ratios were very
near 1:1 indicating that little if any Si signal originated in the substrate of the film.
DE: 8494 Instruments and techniques
SC: Volcanology, Geochemistry, Petrology [V]
MN: 2007 Fall Meeting