World Premier International (WPI) Research Center for Materials Nanoarchitectonics (MANA), National Institute for Materials Science (NIMS), 1-1 Namiki, Tsukuba, 305-0044, Japan.
Dalton Trans. 2011 Nov 7;40(41):10851-6. doi: 10.1039/c1dt10166h. Epub 2011 May 23.
Here we report the preparation of highly ordered mesoporous alumina films existing both as P6(3)/mmc and Fm-3m mesostructures by using triblock copolymer Pluronic P123 as the structure-directing agent. 2D grazing-incidence small-angle X-ray scattering (GI-SAXS) completely proves the existence of two different mesopore structures (i.e., [001]-oriented P6(3)/mmc and [111]-oriented Fm-3m symmetries). After calcination at 1000 °C, the amorphous alumina framework is successfully converted to γ-alumina crystals. During the crystallization process, large uniaxial shrinkage occurs along the direction perpendicular to the substrate with the retention of horizontal mesoscale periodicity, thereby resulting in formation of partially vertical mesoporosity in the film. Through detailed electron microscopic study, we discuss the formation mechanism for the vertical mesoporosity upon calcination. The obtained mesoporous γ-alumina film shows high thermal stability up to 1000 °C, which is highly useful in wide research areas such as catalyst supports and separators.
在这里,我们报告了使用三嵌段共聚物 Pluronic P123 作为结构导向剂,制备同时存在 P6(3)/mmc 和 Fm-3m 介孔结构的高度有序介孔氧化铝膜。二维掠入射小角 X 射线散射 (GI-SAXS) 完全证明了两种不同介孔结构的存在(即[001]取向的 P6(3)/mmc 和[111]取向的 Fm-3m 对称性)。在 1000°C 煅烧后,无定形氧化铝骨架成功转化为 γ-氧化铝晶体。在结晶过程中,沿着垂直于基底的方向发生大的单轴收缩,同时保留水平介观周期性,从而导致膜中形成部分垂直介孔。通过详细的电子显微镜研究,我们讨论了煅烧时形成垂直介孔的机理。所得介孔 γ-氧化铝膜在高达 1000°C 的温度下表现出高热稳定性,这在催化剂载体和分离器等广泛的研究领域非常有用。