真空融解法による二ケイ化モリブデン中の酸素の定量及びその存在状態

書誌事項

タイトル別名
  • Determination of oxygen in molybdenum disilicide using vacuum fusion analysis.
  • シンクウ ユウカイホウ ニ ヨル 2ケイカ モリブデンチュウ ノ サンソ ノ

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抄録

Determination of oxygen in molybdenum disilicide was studied by vacuum fusion analysis and inert gas fusion analysis. The chemical states of oxygen were also investigated by heating gas extraction analysis to assure the reliability of the method. Oxygen contents of molybdenum disilicides, which were analyzed under the conditions of platinum bath at 2100 °C, platinum-tin bath at 2100 °C, graphite capsule at 2000 °C, nickel bath in graphite capsule at 2000 °C and platinum bath in graphite capsule at 2000 °C using vacuum fusion analysis, were compared with those obtained at 2400, 2700 and 3000 °C and that with platinum bath at 2700 °C using inert gas fusion analysis. Oxygen content of molybdenum disilicide with platinum in graphite capsule at 2000 °C using vacuum fusion analysis agreed with that at 2700 °C using inert gas fusion analysis within their experimental errors. In the analysis of heating gas extraction curve, the following samples were heated at the rate of 25 ± 10 °C/min in the temperature range from 850 °C to 2000 °C: grain and powder of molybdenum disilicides; chemical polished molybdenum disilicide powder, molybdenum disilicide sintered at 1350°C for 5 h in hydrogen atmosphere; each of these powders added with powder of silicon dioxide, molybdenum(IV) oxide, molybdenum(VI) oxide, aluminium oxide, iron(III) oxide and chromium(III) oxide ; silicon and molybdenum powders in each graphite capsule. Extracted gases were measured in the differential values by a pirani gauge, and these results were examined against their extraction temperatures. Each component of gas for individual peak was identified. From the comparison of these curves, the chemical states of oxygen in molybdenum disilicide were suggested as adsorbed water and surface and bulk oxygen which was assumed as silicon dioxide.

収録刊行物

  • 分析化学

    分析化学 36 (8), 462-466, 1987

    公益社団法人 日本分析化学会

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