With the objective of studying and understanding the reaction process within the core of the CTAB/SDS micelles, the catalyst concentration was doubled, while keeping all other synthetic parameters unchanged (see the SI for further details). The decision to increase the catalyst concentration was driven by previous studies that have demonstrated the pivotal role of increasing the catalyst concentration in achieving high yields and promoting crystallinity in the resulting COF powders. We observed that by doubling the catalyst concentration under identical synthetic conditions, a noticeable increase in turbidity was evident in the yellowish reaction mixture (Figure ). The Tyndall effect exhibited by this solution demonstrated an increased scattering phenomena after only four hours of reaction, suggesting the formation of larger aggregates (Figure , right). To explore the morphology of the distinct aggregates formed under the influence of the two catalyst concentrations, we conducted scanning electron microscopy (SEM) analysis on the flocculated and dried samples (see SI for further details of sample preparation). Surprisingly, at lower catalyst concentrations, SEM images revealed the formation of spherical-like particles with sizes below 40 nm (Figure ). In sharp contrast, higher catalyst concentrations exclusively led to the development of larger nanorod structures, characterized by widths below 70 nm and lengths below 1500 nm (Figure ). Accordingly, it is evident that the morphology of the resulting aggregates can be significantly influenced by the catalyst concentration when utilizing the micellar approach. Note that conventional bulk synthetic protocols, which lack the utilization of this micellar approach, do not offer the same level of control over the morphogenesis of the resulting products, even when attempting to increase the catalyst concentration. Nevertheless, it is important to highlight that in both cases, there was no discernible difference in yield employing either low or high catalyst concentrations in the micellar approach. Both conditions resulted in the successful generation of gram-scale yellow powders, as illustrated in Figure .