IntroductionAlumina, Al 2 O 3 , is a ceramic metal oxide of great importance as building material, refractory material, electrical and heat insulator, attributed to its high strength, corrosion resistance, chemical stability, low thermal conductivity, and good electrical insulation. One phase of alumina, the -phase is widely used as catalyst, catalyst support and adsorbent because its high porosity and surface area. It is conventionally prepared by heating the hydrated trihydroxides, gibbsite and bayerite, to temperature of > 1000 o C to obtain the -alumina, corundum, a material with great hardness and low surface area. The trihydroxides, gibbsite, bayerite, both are Al(OH) 3. nH 2 O and the monohydroxyl oxide, boehmite, AlO(OH)·αH 2 O, have the monoclinic crystal structure with similar lattice parameters (a=0.866 nm, b=0.506 nm, c=0.983 nm, =94°34′ in boehmite, a=0.868 nm, b=0.507 nm, c=0.972 nm, =94°34′ in gibbsite, and a=0.867 nm, b=0.506 nm, c=0.942 nm, =90°26′ in bayerite [1,2]. In the process of heat treatment, the trihydroxide undergoes a series of transformations. It loses the water of hydration, then dehydroxalate at < 300 o C to form the monohydroxyl oxide boehmite, AlO(OH), which on further heating to increasingly higher temperatures, changes to the transition aluminas, including the -, -, -, and -phases, which then transform finally to the -form. These transition aluminas are crystalline solids with high porosity and surface areas as well as acidic and basic properties, which make them suitable as adsorbents, catalyst, catalyst support and fabricated into filtration membranes as well as used as fillers or components in polymer/ inorganic composite materials with enhanced mechanical properties. The conventional alumina as obtained are usually powder of particulates. These could be fabricated into alumina fibers by various method, through melt growth techniques including the internal crystallization method and extrusion, electrospraying [3] and electrospinning [4][5][6][7][8] have been developed for producing Al 2 O 3 fibers. The high surface areas of transition aluminas are due to the presence of pores. These pores are irregular in sizes and size distributions, and are mainly micropores of diameter less than 2 nm. Since the synthesis of mesoporous materials was first reported in the late 1980s , a number of methods for the synthesis of mesoporous alumina have been reported [8,9]. More recently, interest in nano-materials and nanotechnology has spurred a fury of investigations