A class F fly ash was subjected to high-energy ball milling-induced mechano-chemical activation aided by a surfactant. The resultant nanostructured fly ash was characterized by various techniques. X-ray fluorescence results showed that the amount of iron oxide was reduced from 4.39% to 2.75% after pre-treatment of fly ash by magnetic separation. Ethyl acetate as the milling medium, a ball to powder ratio of 12:1 and 2 wt% of surfactant reduced the average particle size of fly ash to 329 nm and led to a specific surface area of 8.73 m(2)/g. The decrease in crystallite size of mechano-chemically activated fly ash was confirmed from a reduction in peak intensity with a broadened amorphous phase by X-ray diffraction studies. X-ray photoelectron spectroscopic characterization illustrated that peak area of major elements (O, Si and Al) increased after milling. Morphological and FTIR studies revealed that the smooth and inert surface of the fly ash was converted to a rough and more reactive one after mechanochemical activation. The surface modification of fly ash with the surfactant was determined from FTIR spectroscopy. Also, a fractal approach was used to characterize the lacunarity of the agglomerates in the nanostructured fly ash. (C) 2014 Elsevier B.V. All rights reserved.