The present disclosure relates to a process for preparing the boron based nano-sheets. The process comprises a step-by-step chemical recipe that integrates the phenomenon of intercalation with ultrasonication. The chemical recipe includes a reaction of MgB2 crystals with aqueous H2SO4 which results in selective removal of Mg ions from parent crystals making it amenable for intercalation in presence tetramethylammonium hydroxide (TMAOH). The intercalation process leads to expansion of crystal by increase in the inter-layer gallery space from 3.5A� in parent MgB2 to 4.7A� in the expanded crystals. Subsequent ultrasonication of these expanded crystals exfoliates the crystals with higher yields, into few-layer-thick nanostructures which resemble morphology of accordions. For the first time, the present disclosure is reporting such accordion-like nano-sheets derived from MgB2.