An efficient and solvent-free approach for various substituted Bis-amides is described. The reaction was performed on the silica surface under microwave conditions. This Microwave Irradiation (MWI) reaction under solvent-free conditions resulted in a “green-chemistry” procedures, by which Bis-amides were synthesized. NiCuFe2O4 nanoparticle, an efficient and reusable catalyst was employed in the reaction between amide and aldehydes in presence of silica medium to achieve Bis-amides. This approach „synthesis of the titled compounds in the absence of co-catalyst/additives‟ is first of its kind. The recoverability and reusability of the catalyst used in the present method was studied. Further the synthesized Bis-amides were subjected for fluorescence studies.