The present work is undertaken with a view to establishing the best practice (formulation/conditions ) for processing of new hybrid nanocomposite as a new colorant. Synthesis of the new colorants is based on the intercalation of Indigo Blue Vat dye with the silicate-layered nanocomposite (SLNC) which is a natural clay known as montmorillonite (MMT). The current study addresses the ultrafine nanoparticles formed under the effect of ultrasound technology on Indigo Blue vat dye in presence of the clay. The formation of Indigo Blue vat dye /clay hybrid nanocomposite under different formulations and conditions is studied in order to achieve the best practice for optimization of the synthesis of the new colorant based on Indigo Blue vat dye/clay hybrid nanocomposite. New colorants obtained by such are characterized, analyzed, and tested using state-of-the-art tools.