The Fe-N-C catalyst represents one of the most promising candidates for replacing platinum-based catalysts toward the oxygen reduction reaction. The pivotal factor in the successful integration of Fe-N-C catalysts within applications is the attainment of a large-scale production capability. Microwave-assisted pyrolysis offers various advantages, including enhanced energy and time efficiency, uniform heating, and high yield in single-batch processes. These characteristics render it exceptionally suitable for the mass production of catalysts. Through a synergistic approach involving machine learning techniques and microscopic characterization, we discerned performance trends and underlying mechanisms within batch-synthesized Fe-N-C catalysts under microwave-assisted preparation conditions. Machine learning analysis revealed that the precursor mass exerts the most substantial influence on product performance. Furthermore, microscopic characterization unveiled that these influencing factors impact catalyst performance by modulating the degree of agglomeration. Our research introduces an efficacious machine learning model for prognosticating performance and dissecting the influencing factors pertinent to Fe-N-C catalyst synthesis within a microwave system.