This chapter describes how the aim of duplex surface engineering includes chronological application of two surface modification technologies for the production of a surface, with collective properties. Duplex treatment of nitriding and carbonitriding of austenitic stainless steel is of high technical importance owing to its capability to increase hardness, corrosion and wear resistance of treated surface. Duplex treatment has been utilized to enhance the surface mechanical properties of austenitic stainless steel (AISI 304). The microstructure of nitrided surface indicates the development of nitride phases, Fe4N, Fe2N, CrN, Cr2N and γN whereas, duplex treated films shows the formation of FeC, Fe3C, Fe7C3, Cr3C2, Cr7C3, along with nitride phases like Fe3N. Both nitrided and duplex treated samples show the formation of cauliflower like grains. Surface micro hardness of treated substrates has been dependent on the variation of crystallite size and increased by 1.26 times the hardness of nitrided sample and 4.60 times the hardness of the untreated substrates.