Phase structure and micromorphology of gibbsite after hydrothermal treated in different solvents were studied. Results showed that there was a relationship between micromorphology and phase structure of as-synthesized product. The cubic slice-like boehmite microstructure can be obtained in water. The 3D flowerlike boehmite microstructure can be obtained in isopropanol or sodium carbonate solution. The global ammonium aluminum carbonate hydroxide (AACH) architectures assembled by the lathes can be obtained in urea solvent. Gibbsite can transform to boehmite after 12h hydrothermal treatment in water. In isopropanol or sodium carbonate solution, this time decreased to 6h. In urea solution, Aluminum hydroxide turned from gibbsite to the mixture of boehmite, gibbsite and AACH. Finally, AACH is synthesized. This procedure needs 24h.