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In situ X-ray analysis of MoO3 reduction

机译:MoO3还原的原位X射线分析

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摘要

The reduction of MoO3 to MoO2 under hydrogen/argon atmosphere (5 vol. % H-2/95 vol. % Ar) in the temperature range 323 K...623 K was studied in situ by means of wide-angle X-ray scattering. It has been found that the starting material, MoO3, consists of two different orthorhombic MoO3 phases A and B with nearly the same structure parameters. The phase A (fraction of 37.1 wt%) describes the larger crystallites whereas the phase B (fraction of 62.9 wt.%) describes the smaller crystallites. Under the reduction to monoclinic MoO2 phase during the heating, the thermal evolution of the phase fractions is different. A conclusion is drawn that MoO2 is formed preferably in big crystallites. About 10 Wt % of MoO2 has been found to form at 623 K resulting in about 69 wt. % after cooling to room temperature followed by holding in Ar/H-2 atmosphere about 24 h. Additionally, about 4.4 wt. % of the Mo4O11 oxide probably formed in large crystallites was detected in the reduced powder after the cooling.
机译:利用广角X射线原位研究了在氢气/氩气气氛下(5体积%H-2 / 95体积%Ar)在323 K ... 623 K温度范围内将MoO3还原为MoO2的过程。散射。已经发现,起始原料MoO 3由具有几乎相同的结构参数的两种不同的正交MoO 3相A和B组成。 A相(37.1重量%的分数)描述了较大的微晶,而B相(62.9重量%的分数)描述了较小的微晶。在加热过程中还原成单斜MoO2相的过程中,相分数的热演化是不同的。得出的结论是,优选在大晶粒中形成MoO2。已发现在623 K时形成约10 Wt%的MoO2,导致约69 wt%。冷却到室温后,保持在Ar / H-2气氛中约24小时,然后将其以%计。另外,约4.4重量%。冷却后,在还原粉末中检测到可能在大晶粒中形成的Mo4O11氧化物的%。

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