Semiconductor nanoparticles have been a major focus in the investigation of functional materials, not only because of the drive towards the miniaturization of electronic components, but because of their extraordinary optical properties. Aluminium nitride (AlN) and its alloys play a central role in the manufacture of high-intensity ultraviolet light emitters, in addition to a very outstanding chemical and mechanical stability. Urea-glass route (UGR), a non-aqueous and surfactant free sol-gel based procedure, non-toxic and low priced, which uses urea as a nitrogen source, is used to prepare AlN nanoparticles. The products are analysed for different reaction conditions and variable urea:aluminum ratios with XRD, FTIR, SEM, TEM and TGA. β-AlN (cubic structure) is successfully synthesized, at 800C and low Aluminium:Urea ratio. Preparations with higher Al:U ratios successfully obtained a mixture of β-AlN and α-AlN at a higher temperature (900C). In a second research phase, the use of additives such as NH4Cl during the synthesis is examined with the purpose of lowering the temperature and the final properties of the particle. The addition of this supporting nitrogen allows the production of smaller particles, and significantly reducing the amount of Al2O3. Finally, the formation of bimetallic phases was examined by adding different metal transitions species. The analysis of the samples revealed the formation of AlN-M0 ternary compounds, with defined structures such as core-shell. Different strategies lead to different structure formations.