Copyright © 2014 American Scientific Publishers All rights reserved Printed in the United States of America Article Journal of Nanoscience and Nanotechnology Vol. 14, 7340–7344, 2014 www.aspbs.com/jnn A Novel Synthesis and Characterization of Ordered Meso/Macroporous Alumina with Hierarchical and Adjustable Pore Size Xiuhong Meng 1 2 , Linhai Duan 2 , Huibo Qin 2 , Xiaohua Xie 2 , Ahmad Umar 4 5 , Haiyan Wang 1 2 ∗ , and Qiang Wang 3 ∗ 1 College of Chemical Engineering, China University of Petroleum, Qingdao 266555, P. R. China 2 College of Chemistry, Chemical Engineering and Environmental Engineering, Liaoning Shihua University, Fushun 113001, P. R. China 3 College of Environmental Science and Engineering, Beijing Forestry University, Beijing 100083, P. R. China 4 Department of Chemistry, College of Science and Arts, Najran University, Najran-11001, Kingdom of Saudi Arabia 5 Promising Centre for Sensors and Electronic Devices (PCSED), Najran University, Najran-11001, Kingdom of Saudi Arabia The sub-micron polystyrene (PS) microspheres with adjustable size were firstly synthesized using emulsion polymerization method by adding only a small amount of emulsifier. Then, three dimen- sionally ordered macroporous alumina with mesoporous walls and adjustable macropore size was facilely prepared by the colloidal template method. The alumina and PS spheres were characterized by nanoparticle size analyzer, SEM, XRD and N 2 adsorption. The results show that the polystyrene microsphere has adjustable single-sized pore with diameter in the range of 100–350 nm and the yield is higher than that prepared by soap free emulsion polymerization. The alumina materials as prepared using the PS colloidal crystals as the template, had ordered meso-macroporous structures and adjustable apertures. The mesopores (about 3.6 nm) in  -alumina were formed by controlling the heat treatment of alumina precursor. BET surface area and pore volume of the hierarchical alumina as obtained can reach to 241.3 m 2 /g and 0.33 cm 3 /g, respectively. Keywords: Polystyrene, Macroporous Alumina, Colloidal Template Method, Meso-Macroporous Materials. 1. INTRODUCTION Hierarchical materials containing both interconnected macroporous and mesoporous structures have enhanced properties compared with single-sized pore materials due to its increased mass transport through the material and maintainance of a specific surface area on the level of fine pore systems. Incorporation of macropores in mesoporous materials combines benefits from both the mesoporous and macroporous structures. These novel meso-macroporous materials have attracted great research interest and have made a great impact in many applications, including separation, 1 catalysis, 2 fuel cell electrode materials, 3 ioma- terials engineering, 4 controlled drug delivery devices, 5 and membrane reactors. 6 Well-ordered mesoporous alumina ∗ Authors to whom correspondence should be addressed. materials with high surface area and a narrow pore size distribution were synthesized using a sol–gel technique, 7 anodization, 8 nanocasting process, 8 dip-coating method, 9 but the alumina possess monomodal pore channels which limits its application. For liquid phase catalysis, the use of mesoporous sup- ports is advanced to minimise diffusion limitation com- monly observed for microporous materials. Significant enhancements in in-pore accessibility can be achieved via the use of Three-Dimensionally (3D) interconnected mesopore architectures over 2D ones. 10 11 The incorpora- tion of macropores into mesoporous architectures offers an alternative strategy to minimise diffusion barriers, and potentially enhance the distribution of active sites during catalyst preparation. Consequently, compared to the hot studies of meso- porous alumina, the synthesis of the hierarchical and 7340 J. Nanosci. Nanotechnol. 2014, Vol. 14, No. 9 1533-4880/2014/14/7340/005 doi:10.1166/jnn.2014.9216