Sol-Gel Division, Central Glass and Ceramic Research Institute, Council of Scientific and Industrial Research, 196 Raja S. C. Mullick Road, Jadavpur, Kolkata 700032, India.
ACS Appl Mater Interfaces. 2009 Apr;1(4):833-40. doi: 10.1021/am800241x.
Nanocrystalline mesoporous gamma-Al2O3 film of high thickness has been developed and characterized. The films were prepared on ordinary glass substrates by a single dip-coating method using boehmite (AlOOH) sols derived from aluminum tri-sec-butoxide in presence of cetyltrimethylammonium bromide (CTAB) as structure-directing agent. The dried films were heat-treated at 500 degrees C in air to remove the organics and strengthen the network. The GIXRD of the heat-treated (500 degrees C) film shows a broad peak in the low-angle region supporting the formation of worm-hole-like disordered mesostructures. The high-angle GIXRD, FTIR, and TEM of the films confirm the formation of gamma-Al2O3. N2 adsorption-desorption analyses showed that the heat-treated (500 degrees C) film has a BET surface area of 171 m(2) g(-1) with a pore volume of 0.188 cm(3) g(-1) and mean pore diameter 4.3 nm. Pt nanoparticles (NPs) (approximately 2.7 mol % with respect to the equivalent AlO(1.5)) were generated inside the mesopores of the heat-treated films simply by soaking H2PtCl6 solutions into it, and followed by thermal decomposition at 500 degrees C. The surface area and pore volume of the Pt-incorporated film have been reduced to 101 m(2) g(-1) and 0.119 cm(3) g(-1) respectively, confirming the inclusion of Pt NPs inside the pores. FESEM and TEM studies revealed uniform distribution of Pt NPs (2-8.5 nm; average diameter 4.9 nm) in the films. Catalytic properties of the Pt-incorporated films were investigated in two model (one inorganic and other organic) systems: reduction of hexacyanoferrate(III) ions by thiosulfate to ferrocyanide, and p-nitrophenol to p-aminophenol. In both the cases, the catalyst showed excellent activities, and the reduction reactions followed smoothly, showing isosbestic points in the UV-visible spectra. The catalyst films can be separated easily after the reactions and reused several times.
已经开发和表征了具有高厚度的纳米晶介孔 γ-Al2O3 薄膜。通过使用正硅酸乙酯(TEOS)在十六烷基三甲基溴化铵(CTAB)存在下制备的水铝石(AlOOH)溶胶,通过单次浸涂法在普通玻璃基板上制备了薄膜。将干燥的薄膜在空气中于 500°C 下热处理以除去有机物并增强网络。热处理(500°C)后的薄膜的 GIXRD 在低角度区域显示出宽峰,支持蠕虫孔状无序介孔结构的形成。高角度 GIXRD、FTIR 和薄膜的 TEM 证实了 γ-Al2O3 的形成。N2 吸附-解吸分析表明,热处理(500°C)后的薄膜具有 171 m2g-1 的 BET 表面积,0.188 cm3g-1 的孔体积和 4.3nm 的平均孔径。通过简单地将 H2PtCl6 溶液浸泡在其中,然后在 500°C 下进行热分解,在热处理后的薄膜的介孔中生成了 Pt 纳米颗粒(NPs)(相对于 AlO1.5 约为 2.7mol%)。负载 Pt 的薄膜的表面积和孔体积分别减少到 101 m2g-1 和 0.119 cm3g-1,这证实了 Pt NPs 包含在孔内。FESEM 和 TEM 研究表明,Pt NPs(2-8.5nm;平均直径 4.9nm)在薄膜中均匀分布。在两个模型(一个无机和另一个有机)系统中研究了负载 Pt 的薄膜的催化性能:六氰合铁(III)离子通过硫代硫酸盐还原为亚铁氰化物,以及对硝基苯酚还原为对氨基酚。在这两种情况下,催化剂都表现出优异的活性,还原反应顺利进行,在紫外可见光谱中出现等色点。反应后可以很容易地分离催化剂薄膜并重复使用几次。