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Structural studies of silica- and alumina-pinned nanocrystalline SnO_2

机译:二氧化硅和氧化铝固定的纳米晶SnO_2的结构研究

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摘要

Sol-gel-prepared nanocrystalline tin (IV) oxide has been characterized by magic angle spinning nuclear magnetic resonance (MAS NMR) in a pure form and also with silica and alumina pinning phases present. The u9Sn MAS NMR lineshape was observed to broaden as the SnO_2 nanocrystal sizes decreased, a reflection of the increasingly important contribution of the more disordered surface region. A second local Sn environment other than the cassiterite phase was observed, probably an orthorhombic phase that has previously been observed in nanoparticles of SnO_2. The silica and alumina pinning particles were characterized by 29Si and 27 Al MAS NMR. The silica pinning particles retained a high degree of disorder over the range of annealing temperatures, whereas alumina crystallized at ~1000 deg C. A possible explanation for this difference is that since the alumina pinning particles are less successful at restricting nanocrystal growth than the silica particles, they may aggregate together and combine, hence they are larger, less constrained particles.
机译:溶胶-凝胶制备的纳米晶锡(IV)氧化物的特征在于,其具有纯净的魔角旋转核磁共振(MAS NMR)以及存在的二氧化硅和氧化铝固定相。随着SnO_2纳米晶体尺寸的减小,u9Sn MAS NMR线形变宽,这反映了无序表面区域的日益重要的贡献。观察到除了锡石相以外的第二局部Sn环境,可能是先前在SnO_2的纳米颗粒中观察到的正交晶相。二氧化硅和氧化铝钉扎颗粒通过29Si和27 Al MAS NMR表征。二氧化硅钉扎颗粒在退火温度范围内保持高度的无序度,而氧化铝在〜1000℃时结晶。对此差异的可能解释是,由于氧化铝钉扎颗粒在限制纳米晶体生长方面不如二氧化硅颗粒成功,它们可能会聚集在一起并结合在一起,因此它们是较大的,受约束较小的颗粒。

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