Nano heterobimetallic catalysts are used for many industrial applications. Organic precursors are widely used to induce uniform distribution of metal atoms and enhance the porosity of catalysts. In this work, a novel chemical process was developed to enhance the catalyst porosity by distributing the Zn-Al metals in heterobimetallic cluster. 2, 2'-bipyridine was used as a ligand to interlink Zn-Al metal atoms in 2-propanol and dimethylformamide (DMF) environment Central Composite Design (CCD) method was employed to optimise the yield of monometallic and heterobimetallic clusters. The crystalline products were then characterised by FTIR, FESEM, EDX, TGA, DSC and XRD. The produced heterobimetallic complex and nano particles deposited by aerosol-assisted chemical vapour deposition (AACVD) on the stainless steel (SS) substrate have shown enhanced porosity and crystal morphology. The optimized experimental yield for Zn-complex, Al-complex and Zn-Al complex were 80%, 78% and 78.5%, which were in good agreement with the predicted yield by CCD. A systematic approach for the scale-up application of this material was also developed in this study. This study proved that the newly developed "Two-Step" process can be used for production of advanced heterometallic complexes, catalysts and composite materials with enhanced porosity and specific composition. (C) 2015 Elsevier B.V. All rights reserved.