Nitrogen-doped graphene (N-G) has gained considerable attention as a functional nanomaterial due to its tunable structural, chemical, and electronic properties derived from nitrogen incorporation into the graphene lattice. This chapter presents a comprehensive overview of the synthesis strategies and characterization techniques essential for the development of N-G materials. The discussion begins with an examination of the common precursor materials used in N-G synthesis, emphasizing the importance of selecting appropriate carbon sources such as graphene oxide (GO), reduced graphene oxide (rGO), graphite, or carbon nanotubes, along with nitrogen sources including ammonia, melamine, nitrogen gas, or plasma. The chapter then explores major synthesis techniques including chemical vapor deposition (CVD), thermal and gas annealing, plasma-assisted process, and mechanochemical methods such as dry and nanoscale high-energy wet (NHEW) ball milling and highlighting their respective mechanisms, benefits, and limitations. These synthesis pathways allow for precise control over nitrogen configurations and material morphology, thereby tailoring N-G’s performance for various applications. Subsequently, the chapter discusses a range of characterization methods categorized as physical, chemical, and electrochemical analyses. These include microstructural imaging, surface area and porosity assessments, crystallographic studies, elemental and functional group identification, and electrochemical performance testing. Together, these techniques provide a comprehensive understanding of the structure–property relationships governing N-G behaviour. By integrating knowledge of precursor chemistry, synthesis control, and advanced characterization, this chapter establishes a foundation for the rational design and scalable fabrication of N-G materials optimized for catalysis, energy storage, sensors, and other emerging technologies.