Electroless plating is widely utilized in engineering for the metallization of insulator substrates, including polymers, glass, and ceramics, without the need for the application of external potential. Homogeneous nucleation of metals requires the presence of Sn-Pd catalysts, which significantly reduce the activation energy of deposition. Therefore, rinsing conducted during Sn sensitization and Pd activation is a key variable for the formation of a uniform seed layer without the lack or excess of catalysts. Herein, we report the optimized rinsing process for the functionalization of Sn-Pd catalysts, which enables the uniform FeCo metallization of the glass fibers. Rinsing enables good deposition of the FeCo alloy because of the removal of excess catalysts from the glass fiber. Concurrently, excessive rinsing results in a complete removal of the Sn–Pd nucleus. Collectively, the comprehensive study of the proposed nanomaterial preparation and surface science show that the metallization of insulators is a promising technology for electronics, solar cells, catalysts, and mechanical parts.