奈米鉬金屬與氮化鉬之合成

Abstract

本論文中，成功地利用Si(SiMe3)4 和 (SiMe2)6 為還原劑，與高氧化價數化合物 MoO2Cl2(DME)， (NH4)2Mo2O7 和 MoO3 反應，製備出奈米鉬金屬。反應物經混合研磨在低壓下封管反應，加熱至 200 – 400 ℃，製備出黑色粉末產物，並經過 XPS、XRD、STEM、及元素重量百分比分析，鑑定為奈米尺寸的鉬金屬材料。 同樣以 Si(SiMe3)4 和 (SiMe2)6 為還原劑，當起始物為 [NMo(OSiMe3)3NH3]2 時，以甲苯為溶劑在氮氣下加熱迴流，成功地在溶液相製備出黑色固體粉末，熱處理至 350℃，經 XPS、STEM、及元素重量百分比分析，鑑定為奈米尺寸氮化鉬材料。

Molybdenum nanoparticles were successfully synthesized from high valent precursors, MoO2Cl2(DME), (NH4)2Mo2O7 and MoO3, by using Si(SiMe3)4 and (SiMe2)6 as the reductants. After heated at 200 - 400 ℃, black powders were produced from pulverized and mixed solids of reactants in tubes sealed under vacuum. The black product was examined by XPS, XRD, STEM, and elemental analysis as nano-sized molybdenum particles. Silane-reduction route were also applied in preparation of nano-sized molybdenum nitrides using [NMo(OSiMe3)3NH3]2 as precursor. When [NMo(OSiMe3)3NH3]2 was reacted with Si(SiMe3)4 or (SiMe2)6 in refluxing toluene under N2, a black powder precipitated. The black powder was heated to 350℃ and examined by XPS, STEM, and elemental analysis as molybdenum nitride nanoparticles.