The study investigates the miscibility gap phenomenon in Zinc-Bismuth (Zn-Bi) alloys, a crucial aspect influencing the microstructure and properties of these alloys. The miscibility gap refers to the region in the phase diagram where two components of an alloy system are not fully soluble in each other, leading to the formation of distinct phases. Understanding the miscibility behavior is essential for tailoring the properties of Zn-Bi alloys for various industrial applications. This paper discusses the experimental methods employed to analyse the miscibility gap and discusses surface study of samples by using proper etchant on the Zn-Bi alloys