蛍光X線分析法による窒化ケイ素中の酸素の定量

概要

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A possibility of quantitative analysis of oxygen by X-ray fluorescence spectroscopy was studied for silicon nitride powder. An X-ray spectrometer used was composed of a sealed rhodium target tube (3 kW), an analysing crystal of thallium acid phtalate (2 d=25.9 A) and a gasflow proportional counter as a detector for OK_a line with an 1 *m polypropylene film window with the operating condition of X-ray tube at large current under low potential (35 kV-80 mA), intensities of the OK_a peak (2θ=132.90°) and those of the background (2θ =128.00°) from the briquette samples were measured separately for 100 s and the net OK_a intensity was obtained by subtracting the background from the peak intensity. Typical counting rate of the OK_a line was 45 counts/s for the sample of 4.28% oxygen content. A calibration curve was constructed from silicon nitride powder samples of known oxygen contents that were obtained by the graphite capsule-nitrogen fusion method using tin as a bath metal. The result showed a favorable linearity over the oxygen concentration range of (0.1〜4.3)%. Ten kinds of samples were determined by use of the calibration curve. Analytical results agreed closely with that obtained by the fusion method, and the coefficient of variation was 2.3% for seven samples of 3.57% oxygen content.
社団法人日本分析化学会の論文
1982-05-05