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Implantation of Precursor on Synthesis of Monodispersed Alumina Hollow Microspheres and Other Inorganic Microspheres via Colloidal Templating
|關鍵字:||agglomeration;凝聚;agglomerates;alumina;porous;團聚;氧化鋁;多孔||出版社:||材料科學與工程學系所||引用:|| J.-F. Chen, H.-M. Ding, J.-X. Wang, L. Shao, “Preparation and characterization of porous hollow silica nanoparticles for drug delivery application,” Biomaterials, 25, 723-727, 2004.  L. Li, H. Song, X. Chen, “Hollow carbon microspheres prepared from polystyrene microbeads,” Carbon, 44, 587-610, 2006.  F. Caruso, “Nanoengineering of particle surfaces,” Adv. Mater. 13(1), 11-22, 2001.  N.J. Joseph, S. Lakshmi, A. Jayakrishnan, “A floating-type oral dosage form for piroxicam based on hollow polycarbonate microspheres: in vitro and in vivo evaluation in rabbits,” J. Control. Release. 79, 71-79, 2002.  J.-S. Yu, S. Kang, S. B. Yoon, G. Chai, “Fabrication of ordered uniform porous carbon networks and their application to a catalyst supporter,” J. Am. Chem. Soc. 124, 9382-9383, 2002.  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A facile and versatile route has been developed to synthesize non-agglomerating, “flowable” hollow alumina microspheres without addition of any surfactant. This novel method uses organic polymer microspheres as a sacrifice template, anhydrous aluminum chloride as a precursor for alumina, and tetrachloroethylene as a reactive solvent in a way that the metal chloride is implanted into surface of the organic cores to form a core-shell structure. Alumina microspheres with hollow interiors are formed after thermal pyrolysis to remove the organic template. From the depth profile of Auger analysis, the precursor used in this study facilitates the implantation of Al ions into the surface of the organic core. From SEM and DLS results, mono-dispersed alumina hollow spheres with a uniform size and a non-agglomerating character are obtained. Furthermore, both reaction and calcination temperatures have been changed to elucidate the mechanism, surface microstructure and pore-size distribution of the hollow alumina spheres by FTIR, NMR, FE-SEM, TEM, XRD, BET and DLS.
The evolution of surface microstructure, crystallization and specific surface area with temperature has been examined and is divided into three stages. First, from room temperature to 500oC, the shell structure is amorphous with crinkly and airtight character. The shell structure begins to change into γ-Al2O3 (major) and α-Al2O3 (minor) at 900oC. The surface of shells shows nano-sized pores at 900oC from SEM and BET analyses. When heated to 1000oC and 1100oC, the shell forms stable α-Al2O3 structure with smooth surface. Cracks often occur at the triple grain junctions. The specific surface area and the total pore volume of the hollow spheres increase with the calcination temperature. TEM results further reveal that the shell thickness is increased with the increasing reactive temperature, indicating that the thickness of shell can be tailored to a significant extent.
Furthermore, hollow metal oxides spheres and pure hollow metal spheres of various compositions, such as Al2O3, TiO2, ZnO, Fe3O4 and pure hollow Pt spheres can also be successfully fabricated by using this methodology, and are examined by SEM, EDS, TEM and SAD.
Finally, this research also demonstrated that the developed process route can be further extended to the synthesis of hollow Pt-Al2O3 composite microspheres by either one-step or two-step route, which implants AlCl3 and H2PtCl6 into the surface of the organic core to form a core-shell structure before the template core is thermally removed. Platinum-Alumina microspheres with hollow interiors are then synthesized with non-agglomerating and “flowable” character.
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