This chapter explores advanced nano-characterization techniques for cementitious materials, focusing on their applications in understanding microstructure, micromechanical properties, and chemical composition. Key techniques discussed include nanoindentation, modulus mapping, PeakForce Quantitative Nanomechanical Mapping (PeakForce QNM), and nanoscratch. Nanoindentation is widely used for measuring elastic modulus and hardness at micro/nano scales, while modulus mapping and PeakForce QNM offer high-resolution, non-destructive mapping of nanomechanical properties. Nanoscratch is employed for adhesion, hardness, and wear resistance studies. Each technique has unique advantages, such as high-speed testing, spatial resolution, and the ability to analyze small-scale interfacial transition zones (ITZs). The chapter highlights the importance of these techniques in advancing the development of low-carbon, high-performance cementitious materials and their potential for future research and applications.