Alumina (Al2O3) is one of the most widely used engineering ceramic. It can be used in a wide range of applications like electrical/thermal insulation, wear resistance, structural refractories, cutting tools, abrasives, catalyst carriers and coatings. A traditional ceramic process has several steps (i.e. powder synthesis and processing, shape forming, drying, organic burnout and densification). Accessing powders with sizes in the range of a couple of micrometers down to several tens of nanometers is considered critical in attaining higher densities in the final ceramic bodies. Besides since significant shrinkage can be observed in the thermal treatment steps due to the excessive use of additives (e.g. binders, solvents and plasticizers) in the powder processing and forming steps, it is important to take remedies that would increase the solids loading in the initial mixtures. In addition, most of the conventional additives and solvents used in these steps are toxic and it is necessary to replace them with the environmentally benign aqueous-based alternatives. Alumoxanes could be used as a benign aqueous-based alternative to be used as a ceramic precursor or an agent. They are a group of compounds that have nano sized boehmite cores encapsulated with the organic groups used in its production steps. In this research work, alumoxane nano particles which can be used as precursors for nano-alumina were developed starting from aluminum trihydroxide. As a preconditioning step, grinding was applied to decrease the aluminum hydroxide particle size (&amp / #8804 / 60 &amp / #956 / m) to submicron sizes. This process was followed by the glycothermal ageing step, and organic derivative of boehmite was obtained. The amorphous particles thus obtained were further treated mechanochemically in a high energy ball mill with organic chemicals like acetic acid, methoxy acetic acid, stearic acid and L-lysine. After this step the observed sizes of the particles were as low as 10-100 nm. The effects of organic molecules used in each step were studied by FTIR spectroscopy and their effectiveness in exfoliation of hydroxide layers were identified with dynamic light scattering from processing solutions dispersed in aqueous medium. Moreover, in each step, structural analyses were carried out by XRD.