This project focuses on the microstructural evolution, phase stability, and grain boundary engineering in advanced Ni-based superalloys designed for high-temperature applications. Through a combination of thermo-mechanical processing, sub-solvus heat treatments, and multi-scale characterization techniques—including Atom Probe Tomography (APT), Transmission Electron Microscopy (TEM), Electron Backscatter Diffraction (EBSD), and in-situ X-ray diffraction—we investigate key phenomena such as γ/γ′ phase transformations, inverse precipitation, grain boundary engineering, and stress relaxation behavior. Particular emphasis is placed on solute segregation dynamics, the formation of heteroepitaxial interfaces, and the role of lattice misfit and crystallographic orientation relationships in influencing mechanical properties and long-term stability. These insights aim to support the design and optimization of next-generation superalloys with improved strength, corrosion resistance, and thermal stability for critical aerospace and energy applications.