The present work describes the influence of the parameters employed in the gas tungsten arc welding process (GTAW) when nickel powder is used as a filler metal in 2304/2507 duplex stainless-steel dissimilar joints. Multi-objective optimization was applied in order to maintain the austenite/ferrite percentage in the welded zone. A microstructural and phase quantification analysis was performed in each sample through optical and scanning electron microscopes. It was found that a nickel powder addition combined with low heat input increased the biphasic ratio across the different zones of the dissimilar welded samples. Although the austenite volume fraction increased in the 2304 heat-affected zone (HAZ) near to 25%, it was not sufficient according to international standards. The obtained results led to the maintenance of the 50/50 phase percentage in the 2507 HAZ welded joint side, as well as to the increment of the austenite percentage in the 2304 HAZ.Materials 2020, 13, 780 2 of 14 temperatures, another phenomenon is observed: ferrite decomposition occurs, causing the formation of harmful secondary phases, such as sigma (σ), chi (χ), carbides, and nitrides phases, which subsequently deteriorate the mechanical and corrosion-resistance properties of the DSS. Santos et al. conducted a study, based on the analysis of thermal history, which showed the temperature measured across the weld and its effect on the microstructural and mechanical behavior, and compared the results with the three-dimensional finite element model built. In addition, Sarlak, Atapour, and collaborators specifically studied the corrosion behavior across the welding in samples obtained by the welding process of a lean duplex stainless steel (LDSS) and its effect on the microstructure [9][10][11].Various joining techniques, such as plasma, laser, tungsten inert gas (TIG), and gas metal arc welding (GMAW) are being developed to meet the requirements demanded by these materials, avoiding distortion. However, ferritization is a problem with these processes. In addition, the effect generated by the entry of heat into these materials is a research topic. Plasma arc welding has beneficial results for DSS, which is situated at a controlled heat input and an acceptable ferrite ratio compared with other processes. Flux-cored arc welding (FCAW) has gradually attracted strong attention in welding DSS due to its higher welding efficiency compared with the gas tungsten arc welding process (GTAW) process. However, studies on the microstructure, mechanical properties, and corrosion resistance of the DSS FCAW joint are limited. Advanced laser hybrid welding has a great advantage for DSS, because it reduces heat input and distortion level compared with SAW and FCAW [12,13]. The GTAW is a welding procedure that has been employed efficiently in past years to weld materials such as stainless steels due to its facility to produce sound joints that meet specific requirements of industries, added to its facility to work when thin materials are required. However, it has be...