A three-step preparation of macro-mesostrucred gamma-Al2O3 nanofibres with a large pore volume of 4.21 cm g(-1) and a high specific surface area of 396.3 m(2) g(-1) has been reported by H2O2-precipitated boehmite from sodium aluminate solution, followed with azeotropic distillation and calcination. The boehmite nanofibres of crumpled sheet-like morphology about 5-10 nm thick and over 100 nm long were preserved after calcination. A mechanism of n-butanol-induced crumpled sheet-like boehinite nanofibres formation was proposed. This interaction between butoxy groups (CH3(CH2)(3)O-) and the surface of boehmite crystallites through hydrogen bonds induces profound changes in the morphology of boehmite particles and their growth. (c) 2005 Elsevier B.V. All rights reserved.