Intermetallic compounds (IMCs), which are very unique in terms of their well-defined stoichiometry, atomic arrangement and controlled crystal structure, represent a vibrant and exciting field of research converged at the forefront of catalysis, nanotechnology and materials. In contrast to the random atomic ordering in alloys, IMCs with specific geometric and electronic structures exhibit remarkably enhanced catalytic performance. In this review, we have summarized and highlighted the recent progresses on preparation methods of IMCs, including controlled colloidal synthesis, inorganic capsule synthesis, and layered double hydroxide synthetic method, with special emphasis on how to obtain tunable composition, stable particle size, and well-defined homogenous morphology. Then, we systematically introduce the advanced characterization techniques (e.g., ED, STEM, and XAFS) for the characterization of the crystalline and surface coordination structure of IMCs. A strong combination of experimental characterizations and theoretical calculations is the key to investigating the structure–property relationship. Moreover, we discuss the catalytic application of IMCs with focus on electrochemical catalytic reactions, oxidative dehydrogenation reactions, and selective hydrogenation reactions. Finally, the current issues and future prospects for development in this field are concretely discussed from the viewpoints of catalyst design, preparation methods and potential extension in industrial applications.