Understanding dynamic material evolution is essential for studying interfacial phenomena. This thesis explores two areas: electrochemical crystallization and in-situ atomic force microscopy (AFM). First, we introduce electrochemical crystallization to precipitate terephthalic acid (TPA) from alkaline solution, where the protons produced at the anode to protonate terephthalates into TPA crystals. This methodology allows us to control the addition rate of acid, enabling the crystallization process to be visualized by in-situ optical and atomic force microscopy. Fast acid generation (high electrochemical current) favors the nucleation regime, while slow acid generation (low current) favors growth, promoting larger crystal formation. Electrolyte and terephthalate concentrations were found to impact the morphology and structure of the TPA crystals, suggesting that TPA morphology depends on environmental factors beyond the proton addition rate. We show that controlling time, current density, and electrolyte concentration can afford tuning of TPA crystal morphology. Second, in-situ AFM is employed to study material evolution in micron/nanoscale under various conditions. The AFM imaging of highly oriented pyrolytic graphite (HOPG) surface confirms its stability in ambient air, water, acidic solution, and under constant potential within a short time frame. Additionally, dynamic behaviors and conformations of poly(2-vinylpyridine) (P2VP) in acidic environment are visualized by AFM, indicating that P2VP exists in the form of both chains and clusters in liquid. Together, these studies provide mechanistic insights into crystallization and interfacial dynamics, showing the power of combining electrochemistry with high-resolution, in-situ imaging.