The with various phases were prepared by simple ex-situ hydrolysis and spark plasma sintering (SPS) process of Al powder. The nano bayerite phase was derived by hydrolysis of commercial powder of Al with micrometer size, whereas the bohemite (AlO(OH)) phase was obtained by hydrolysis of nano Al powder synthesized by pulsed wire evaporation (PWE) method. Compaction as well as dehydration of both nano bayerite and bohemite was carried out simultaneously by SPS method, which is used to fabricate dense powder compacts with a rapid heating rate of per min. under the pressure of 50MPa. After compaction treatment in the temperature ranges from , the bayerite and bohemite phases change into various alumina phases depending on the compaction temperatures. The bayerite shows phase transition of sequences. On the other hand, the bohemite experiences the phase transition from AlO(OH) to It shows AlO(OH) sequences. The compacted at shows a high surface area .