Electron Microprobe Measurements of Nitrogen in SiC

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.