As global demand for renewable energy grows, new avenues emerge to design cost-effective routes for enhancing energy storage and capture, such as high-capacity batteries and next-generation solar cells. This study focuses on characterizing the underlying dynamics of model energy storage and conversion materials in response to oscillating stimuli. The near-term goal is to develop a generalizable method of doing this that may be adapted to a wide array of different materials. The long-term goal is to apply this method to understand the fundamental chemical dynamics involved in the function of these materials, ultimately accelerating progress in improving ion storage media for batteries and enhancing photovoltaic efficiency. The first target is to selectively detect vibrational signatures associated with electron accumulation in response to an applied potential in semiconducting nanoparticles, with applications as anode materials for alkali metal ion-based batteries. I aim to do this by developing a phase-sensitive detection method using lock-in amplification, which allows measurement of small spectral signals that would otherwise be undetectable due to noise. To hit this target, a well-studied, reversible ferrocene/ferrocenium system was subjected to alternating current (AC) electrochemical modulation and probed using visible light. The electrical signals induced in these materials were analyzed at characteristic frequencies. By monitoring the spectral fingerprints of each ferrocene and ferrocenium, I will extend the application of these spectroelectrochemical methods to the model titanium(IV) oxide (TiO₂) electrode. Moving forward, this method to probe reaction dynamics may be applied to analyze the stabilizing effect of performance increasing modifications on anode materials within alkali metal-based batteries.